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HEXAMINE 2013-2014

SHRI.K.J.POLYTECHNIC,BHARUCH

HEXAMINE
2013-2014

Project Report

2013-2014

This project of hexamine consist of productino of HEXAMINE,with the best suiteable


process which is used in now days in the industry,it also consist of designing of the
selected process,economic evalution.

shri k.j polytechnic,bharuch


HEXAMINE 2013-2014

SHRI K. J. POLYTECHNIC, BHARUCH

CHEMICAL ENGINEERING DEPARTMENT

A
PROJECT REPORT
ON
HEXAMINE

PREPARED BY :-

Sr. No. Enroll No. Name

1. 116450305053 DIVYESH DHRUV

2. 116450305054 JAYVEERSINH

3. 116450305057 KETAN PATEL

4. 116450305058 MEHUAL CHAUHAN

5. 116450305060 MANORANJAN SINGH

GUIDED BY:-
Mr.R.I.RATWANI
( H.O.D)

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Gujarat technological university is one of the biggest university which offers the
various types of courses likes masters,bachelors,diploma,post
graduate,medical,pharmacy,etc..

This project is given by GTU to the partial fullfillment of the diploma in chemical engg.
To undeerstand and analysed the various project done in the industry through project
surveys and visiting of the industry . GTU also describe the meaning of giving the project
to the enigneer in the 6th semister for well learning of the manufacturing of the chemicals
and their detail study including the project management, production, properties of the
chemical,economic evalution as per company capacity and dail production rate, it also
include the site selection parameters which gives engineers the study of the plant site setup
and the layout of the plant .

The reason of giving project to the engineers is to develop the leadership ,project
management ,surveys and detail study.

Thanks to GTU,

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HEXAMINE 2013-2014

SHRI K.J POLYTECHNIC

BHARUCH-392001

(Affiliated to Gujarat Technological University)

This is to certify that the project HEXAMINE MANUFACTURING


Submitted by towards fulfilment of diploma 6th semester in chemical
Engineering for the exam may 2013 conducted by Gujarat technological
University, Ahmedabad is a record of Bonafide work done by him under my
supervision.

Date: / /2014

----------------------------- ------------------------------

(GUIDED BY) ( H.O.D)

Mr.R.I.Ratwani Mr.R.I.Ratwani

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Preface
Teaching is the important knowledge, but training develops habits. It assures that
Technical skills cannot be perfect without practical training Hence, the practical
training is grate valuable for Engineering Student the Actual aim of in Plant
training is to get all Operation and Process which are Carried Out in the Industries
and More about the Chemical Equipment..

Practice makes a man perfect in practical training a person Deals with Many technical
Problems. In real Operation and Process another Aim of in Plant training is to learn
Industrial Management and Discipline.

This project report describes the manufacture of hexamine is prepared in partial


fulfillment in chemical engineering. It is purely academic in nature though attempts
have been made to incorporate faculty data available from journals, books and
other sources. Reasonable assumptions have been made for data those were not
available.

This report includes the information based on theoretical backgrounds. so this


report cannot application to industrial scale to tally. But for actual setting up of a
new chemical plant and expansion or revision of existing one requires the use of
design report as a preliminary estimate

The report provides preliminary information and gives an idea and in sigh into the
process design aspects.

The report also includes safety consideration, instrumentation and process control,
cost analysis. The reference section at the end lists the source of information. A
detailed market surveys and plant set up design factor has to be studied before
setting up a plant end. A number of pilot plant trials should be conducted before
starting. No such trials were conducted.

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HEXAMINE 2013-2014

ACKNOWLEDGEMENT

I extend my sincere gratitude to my guide, Mr.R.I.RATWNI lecture and our head


of department in chemical engineering dept. Shri .K.J.Polytechnic,Bharuch for sharing his
vast knowledge and resources and also for his availability
Round a clock,

I am also thankful to prof Mr.R.I.Ratwani in lecture and our project group adviser in
chemical engineering department Shri.K.J.polytechnic,Bharuch. For extending their help in
the course, I am also in dept. to all the authors and editors of various reference books,
research paper that helped me through this report

Thanking you sir..

D.Chemical Engineering

(3rd year)

INDEX

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PAGE
SR.NO SUBJECT
NO.
1 INTRODUCTION AND HISTORY OF PRODUCT 8

2 PRESENT STATUS INCLUDING LIST OF INDUSTRIES 12

3 PROPERTIES AND APPLICATION OF PRODUCT 14

4 PROPERTIES OF RAW MATERIAL 22

5 VARIOUS PROCESSES OF MANUFACTURING 24

6 MOST SUITABLE PROCESS IN DESCRIPTION WITH FLOW SHEET 27

7 MAJOR EQUIPMENT REQUIRED 32

8 MAJOR INSTRUMENTS REQUIRED 36

9 UTILITIES REQUIRED 43

10 LAYOUT AND LOCATION OF PLANT 46

11 SITE SELECTION PARAMETERS 52

12 ECONOMIC EVALUTION 57

13 IMPORTANT ASPECTS OF SAFETY 64

14 EFFLUENT TREATMENT RELATED TO PRODUCT 81

15 CONCLUSION 85

16 REFERENCE 86

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CHAPTER -1
INTRODUCTION AND
HISTORY OF PRODUCT

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INTRODUCTION AND HISTORY OF PRODUCT

A detail process study was done on the Hexamine production plant in Semester VII. All
the available processes were studied and the best suitable and feasible process was
selected. In this semester, Energy Balance, cost estimation etc. of the selected process was
done on the basis of the future trend of demand and purity required. All the utilities and the
supporting infrastructure required were determined.

This project report also consists of the designing of the selected process. The designing
consists of sizing of the all the major equipments present in the process. A detailed
mechanical design of the main Reactor was also done.

Rough plant layout is also prepared to get an idea of required plot area. A detailed financial
study comprising Project cost estimate, Cost of production and financial analysis was also
carried out. The project was found to be financially sound with an attractive pay out
period.

Altogether this report consists of all the engineering and financial aspects required for
setting up a Hexamine manufacturing facility.

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HEXAMINE 2013-2014

HISTORY OF HEXAMINE

The synonyms or other names of Hexamine are 1,3,5,7- Tetraazaadamantane;


Ammonioformaldehyde,Aceto HMT; Aminoform; Ammoform; Cystamin; Cystogen;
Formamine; Formin; Hexaform; Hexamethylenamine; Urotropin; Hexamethylentetramine;
Hexilmethylenamine; HMT; Methamin; Methenamine; Resotropin; Uritone; Urotropine;
Esametilentetramina; 1,3,5,7-Tetraazatricyclodecane.

Hexamine was firstly prepared by a Russian chemist in 1859. Hexamine is a colourless


substantially crystalline compound with a sweet metallic taste. Particle size ranges from
80-800 micrometers. It can be readily ignited and burns with a bluish yellow flame.

The chemical structure of Hexamine is known in great detail. The carbon and nitrogen
atoms are all equivalent. In the three dimensional structure, the nitrogen atoms occupy the
summits of an octahedron. It crystallizes as rhombic dodecahedron. On heating it sublimes
with decomposition at temperature above 200 oC but does not melt. Products of thermal
decomposition include ammonia, hydrogen cyanide, methane, hydrogen, nitrogen and
resinous oil. Charring becomes apparent at about 280 oC when it is heated in sealed tube.

Its heat of combustion (adjusted to 25 oC) is approx 1003.0 k cal per g mole (10). thermo
dynamic properties as reported by change western per g mole at 25 oC are heat of
formation 28.8 k cal , free energy 102.7 k cal heat capacity 36.4 cal/ oC and entropy
36.048cal/ oC . It is soluble in water and can be crystallized as a hydrate (CH2)6N4.6H2O
which is stable at temperature below 14 C. Hexamethylene tetra amine forms a saturated
aqueous solution containing 46.5% by weight at 25 oC. Its solubility decreases with
increase in temperature; the solubility also reduced by dissolving ammonia.
Hexamethylene tetra amine is soluble in chloroform (13.4g /100 ml at RT) and ethyl
alcohol (2.9 g /100 ml at RT) and methanol (7.3 g /100 ml at RT). It is slightly soluble
(less than approx 1%) in carbon tetra chloride, acetone, benzene and ether and it is

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HEXAMINE 2013-2014

completely insoluble in petroleum ether. It behaves like a weak monobase and aqueous
solution shows pH values in range of 8-9.

Solutions are comparatively stable, showing little hydrolysis in absence of acid. Hexamine
is easily hydrolyzed in presence of acids to formaldehyde & ammonia. Its primary reaction
with acids leads to the formation of salts such as (CH2)6N4HCl but these are relatively
unstable and cannot be easily isolated.
With hydrogen peroxide in acid solution, Hexamethylene tetra amine forms explosive
peroxide Hexamethylene tri peroxide Diamine.

Hexamine is reduced with zinc and acetic acid or by electrolytic means to give methyl
amines. It forms addition compounds with chlorine, bromine and iodine. Its tendency to
form addition complexes is highly marked in case of in case of metallic salts which may be
illustrated by silver nitrate and mercuric chloride derivatives.
Hexamine is analyzed by boiling a weighed sample (approx.) with 40ml 1N sulfuric acid
until all formaldehyde is vaporized, and titrating the excess acid. Each ml of 1N acid
consumed is equal to 0.03504g of hexamine.

Hexamine is not poisonous but some human beings are sensitive to it and are subjected t
skin rash when they come in contact with it t its vapours. If toxic symptoms are observed
then a physician may be consulted.

Annual US production of technical hexamine rose from 16 million lb in 1950 to 41 million


lb in 1963. The price has remained relatively constant at about 23-24 million lb.

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HEXAMINE 2013-2014

CHAPTER-2
PRESENT STATUS
INCLUDING LIST OF
INDUSTRIES

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The following are the other manufacturers in India

1. Indian Switchgears & Consultants Company Limited, Vadodara


2. Simalin Chemical Industries Limited, Mumbai
3. Jai Ambey Ganga Chemicals Private Limited, Hanumangadh, phase -1
4. Taru Vikas Private Limited, Mumbai
5. Nuchem Limited, Faridabad
6. Aldehydes India,Faridabad
7. Kakar Trading Co., New Delhi
8. Solar Surgical and Pharmaceuticals,mumbai

World Wide Producers Of Hexamine

1. BEIJING SUNNY-RICH COMPAY [China]


2. Jinan xinxing blowing agent co.ltd. [China
3. Wuyi beiqi commodity factory
4. Yantai huawei industry and trading co,ltd [China]
5. Jinan Shenyu International Trade Co., Ltd. [China]

6. Henan Harvest Chemicals Import & Export Co. Limited, china


7. Chemanol,dammam,Saudi , Arabia
8. Jinan Licheng District Xinxing Auxiliary Agent Factory, china
9. Quzhou Chemical City Trade Co. Limited, Quzhou, China
10. Lee Chang Yung Chemical Industry Corporation, Taipei, Taiwan
11. Cioma SA, Medelln - Na, Colombia
12. Blagden Chemicals Limited, Croydon - CR9 3QU, United Kingdom
13. Shandong Jiasheng Industry Co. Limited, Taian - 271 000, China
14. Yantai Huawei Industry And Trading Co. Limited, Yantai - 264 100, China
15. Heliopolis Chemical Industries, Cairo - Na, Egypt

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CHAPETER : 3

PROPERTIES AND

APPLICATION OF PRODUCT

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PROPERTIES AND APPLICATION OF PRODUCT


3.1 Physical Properties

Table 3.1 Physical Properties of Hexamine


Contents 99.55%
Molecular Weight 140.19
Melting Point Sublimes at 280 C
Ph-Value (10% Solution) 7.5-9.0
Density (20C) 1.33g/cm3
Solubility (in water) At 20C 89.5g/100g
At 40C 87.4g/100g
At 60C 84.4 g/100g

Ignition temperature 390 C


Bulk density Crystalline form 700-800 kg/m3

Ground form 300-400 kg/m3

Hexamine does not melt and sublimates almost under composed in a vacuum at 230-
270C.Decomposition begins at temperatures above 270C. Hexamine is highly soluble
In water. Solubility decreases slightly as temperature rises.
The solutions are slightly alkaline, with pH values usually between 8 and 9. In organic
Solvents, Hexamine is barely soluble.

The following table shows the solubility of the pure product in a number of important
Solvents

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Table 3.2 Solubility Data of Hexamine


SOLVENT Kg hexamine in 100 cm3
Solvent
Chloroform 13.4
Methanol 7.2
Ethanol 2.9
Amyl alcohol 1.8
Acetone 0.6
Petroleum 0.2
Xylene 0.1
Trichloroethylene 0.1

3.2 Chemical Properties


Hexamine reactions can be divided into three groups.
3.2.1 Resembling a tertiary amine
With many inorganic and organic acids, salts are formed as primary products.

3.2.2 Resembling formaldehyde


Hexamine hydrolyzes under the influence of heat, causing formaldehyde to split off
ammonium salts to form. In many cases, it is advantageous that reaction is slower with
Hexamine, than when using formaldehyde.

3.2.3 Other reaction


Hexamine forms additive or complex compounds with metal salt. Nitration produces
cyclotrimethylene trinitramine, which is known by the names Hexogen, Cyclonite and RDX
and uses as an explosive.Various amines are produces by reduction, such as
monomethylamine and trimethylamine.

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3.3 Storage Behavior & Flow Properties


Hexamine is not hygroscopic. However, it is sensitive to humidity and absorbs moisture at a
relative humidity above 65%, causing binding or clogging.
Pressure and warmth increase the likelihood of the product forming lumps. This effect is
more pronounced with fine grained products.
Above all, this has a negative effect on the flow properties of the ground product. The
product should therefore be best stored in a room with a constant temperature and a relative
humidity below 60%. Likewise, there should be as little pressure on the product as possible
(i.e. do not stack pallets on top of each other).

Fig 3.1 Behavior of Hexamine

Apart from its tendency to stick, Hexamine is not subject to changes during storage and can

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be used even after several months. To improve the flow properties, particularly for the
grades marked free flowing, special highly dispersed silica are added.
These additives are chemically neutral for those areas in which these grades are used. They
are essential to enable the product to be used effectively. When conducting a test analysis of
these grades, it should be remembered that the ash content is higher and the Hexamine
content lower.
When working with finely ground grades, precautionary measures must be taken against
explosive dust/ air mixtures. Explosion pressure can reach 12.7 bars, with a maximum
pressure build-up speed of 370 bar/sec.

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USES AND APPLICATION

Hexamethylenetetramine, which is used as a urinary antiseptic. Nitration of Hexamine gives


the explosive cyclonite, or RDX. Formaldehyde and acetaldehyde react with Hexamine in
the presence of calcium hydroxide to give pentaerythritol, the tetranitrate of which is the
explosive. Hexamine is also useful in adhesives, coatings, and sealing compounds. In
medicine, it is an antibacterial agent. It is used as a dye fixative and in the preservation of
hides. It is used in vulcanizing rubber and as an anti-corrosive agent in steel. It is used in the
detection of metals and in the absorption of poisonous gases. It stabilizes lubricating and
insulating oils. It is sometimes burned in camping stoves.

Reagent in organic chemistry:

Hexamine is a reagent in organic chemistry. It is used in the Duff reaction (formylation of


arenes), the Sommelet reaction (converting benzyl halides to aldehydes) and in the Delepine
reaction (synthesis of amines from alkyl halides).

Medicinal and food uses:

Methenamine hippurate is mainly used for the prophylaxis (prevention) of urinary tract
infections, where it is hydrolyzed in the acidic pH of the urine to form formaldehyde.
Formaldehyde is an effective antiseptic against bacteria and fungi in vitro, but may not be
effective in vivo - it has not been shown to be effective for the treatment of urinary tract
infections. Furthermore, certain bacteria increase urinary pH, rendering Methenamine
ineffective. Methenamine can also be used to treat hyperhidrosis when applied topically .In
China, a 10% solution is used as a deodorant. As a food additive, hexamine is used as a
preservative in cheeses. In some countries, such as Russia, it is banned for this use.
Hexamine can be absorbed through the skin, and some people are allergic to it

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Industrial and commercial uses:

Hexamine is used as a component with 1,3,5-trioxane in hexamine fuel tablets (often called
Esbit). This solid fuel in tablet form is used by campers, hobbyists, the military and relief
organizations for heating camping food or military rations. It burns smokelessly, has a high
energy density, does not liquefy while burning and leaves no ashes.

Another important area for use of hexamine is in the production of powdery or liquid
preparations of phenolic resins and phenolic resin moulding compounds, where hexamine is
added as a hardening component. These products are used as binders, e.g. in brake and
clutch linings, abrasive products, non-woven textiles, formed parts produced by moulding
processes, and fireproof materials.

It is used in rubber and textile adhesives, in paints and lacquers, in the photographic
industry, in the production of explosives such as RDX, as a corrosion inhibitor, as a protein
modifier, as a reagent in chemical analysis, and in the production of deodorants and hair
fixers, among many other uses.

A hexamine fuel tablet is a very useful form of hexamine used as solid fuel in tablet form.
The tablets burn smokelessly, have a high energy density, do not liquify while burning and
leave no ashes. Invented in Murrhardt, Germany in 1932, the main component is hexamine.

The tablets are used for cooking by campers, the military and relief organizations. The
tablets are often used with disposable metal stoves that are included with Combat ration
packs. Backpackers concerned with ultra light gear, tend to buy or make their own much
lighter stove. An Esbit stove can be made by cutting off the bottom of an aluminum pop can,
and turning it upside down to support the fuel tab; a pot can be supported above this with a
circle of mesh chicken wire or tent pegs. Although not ideal, fuel tab can be placed on a rock
or on the dirt, with a pot supported above by rocks. Another common use is to provide a safe
heat source for model steam engines.

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Advantages and disadvantages:

Fuel tablets are ultra light weight compared to other stove options.Compact; entire stove
system and fuel can be stored inside cooking pot; use plastic bags inside and out due to
burned residue. They are simple.

However, they have several disadvantages:

Boils water, but not ideal for any cooking requiring simmering. Expensive fuel and less
widely available, compared to alternatives such as alcohol or petrol stove fuels.

Hexamine tablets give off noxious fumes, requiring foods being cooked to be contained in a
receptacle such as a pot or pan. Burned tabs will leave a sticky dark residue on the bottom of
pots, although this can be easily removed by rubbing the pot on grass.

Major Application Areas:


Rubber industry: Vulcanizing agent and rubber blowing agent
Explosives industry: Slurry, explosives, RDX (hexogen), HMX (octogen), HMTA
(hexamethyline triperoxide Amine)
Fuel industry: HMT fuel tablets, smokeless pellets, friction dust manufacturing
Synthetic resin industry: Liquid resin stabilizer, Hardening of Novolak resins, Aniline
shellac resins
Pharmaceuticals industry: As a Disinfectant.
Photographic industry: As a Stabilizer for developers.
Organic synthesis industry: Additives in deodorizing powder, absorption of phosgene gas,
preservation of fresh products.
Metal industry: Inhibitor against acids and hydrogen sulphide
Leather industry: Conservation of furs and skins
Paper / cellulose industry: Surface treatment during manufacture of water repellent papers
and cardboards.
Lubricant industry: Stabilizer for greases and oils
Fertilizer industry: Anticaking agent for prilled urea\

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CHAPTER-4
PROPERTIES OF
RAW MATERIALS

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FORMALDEHYDE

Physical and Chemical Properties:


Chemical Formula: HCHO
Molecular Weight: 30.03
Appearance: Clear, colorless liquid.
Odor: Pungent odor.
Solubility: Infinitely soluble.
Specific Gravity: 1.27
pH: 2.8 (31% solution)
% Volatiles by volume @ 21C (70F): 100
Boiling Point: 96C (205F)
Melting Point: -15C (5F)
Vapor Density (Air=1): 1.04
Vapor Pressure (mm Hg): 1.3 @ 20C (68F)

AMMONIA

Physical and Chemical Properties:


Chemical Formula: NH3
Molecular Weight: 17.03
Appearance: colorless gas
Odor: Pungent odor.
Solubility in water: 89.9 g/100cc at 0C
Specific Gravity: 0.9 at 25 C
pH: 8.4
% Volatile: 100
Boiling Point: -33 C
Freezing Point: -77C
Vapor Density (Air=1): 0.596 at 0 C
Vapor Pressure (mm Hg): 10 atm at 25.7 C

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CHAPTER-5
VARIOUS PROCESSES OF
MANUFACTUING

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PROCESSES FOR HEXAMINE MANUFACTURE

Earlier Hexamine Production Method:


Hexamine was formed by the reaction of aqueous ammonia with aqueous formaldehyde
according to the following reaction:

6CH 2 O 4 NH 3 C6 H 12 N 4 6H 2 O

The reaction is strongly exothermic. The normally expected temperature rise should not,
take place, since at, too high a temperature there is the danger of producing by-products.
The first plants for production of hexamine operated at, a reaction temperature of about
20 oC, and used aqueous solutions of formaldehyde and ammonia as raw materials in
the batch process. In some cases a part of the ammonia was gaseous. The reaction
temperature and the relatively great, heat of reaction has always been difficult to control.
To provide the cooling surfaces, large units of correspondingly large volumes were
necessary. The procedure was batch wise and required as much as 36 hours per charge.
The hexamine obtained in solution (10 to 20% depending on the consent, ratio of the raw
materials) was concentrated in vacuum (about 40 mm. Hg.) until hexamine was
crystallized during a continuous addition of ammonia. After this operation, requiring 24
hours, the product obtained was re crystallized to hexamine.

2. Continuous production of Hexamine:

A continuous process for Hexamethylene tetramine production allows the direct addition
of the formaldehyde and the ammonia in the gaseous phase to the reactor. The
formaldehyde may come directly in unpurified form from an efficient and specially
devised oxidation unit fed with methanol and integrally a part of the production unit. The
heats of hydration of the two gases and the heat of the reaction accomplished in an aqueous
phase are removed by vaporization of water from the reactor, which is actually a specially

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fitted still pot. In order to prevent losses of ammonia or formaldehyde gas, their effective
concentrations in the reactor must be very low, or they would pass off with the vapors and
be lost to the reaction. The optimum temperature of the reaction may be controlled by
varying the total pressure at which the reaction mixture is allowed to boil or by controlling
the partial pressure by the presence of noncondensable gases. The reaction under these
desirable conditions is extremely fast. The solid hexamine is removed continuously from
the reactor either as fine white crystals or as a solution of any desired concentration. The
heat of the reaction and of the hydration of the starting gases performs the entire water
removal and eliminates the need of additional evaporative equipment and heat.

3. Hexamine manufacture:

As we know the lower aldehydes react very rapidly with ammonia without any need of
catalysts and also at low temperature. This phenomenon is used for the production of
Hexamine. Aqueous phase reaction of ammonia and formaldehyde is carried out in a
semibatch manner. In such plant reactors it is from 1 to 2 metric tons per day for a reactor
of relatively small size with a yield on a one-pass basis of above 99% for both ammonia
and formaldehyde.

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CHAPTER-6
MOST SUITABLE PROCESS
IN DETAIL(DESCRIPTION)
WITH FLOW SHEET

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MOST SUITABLE PROCESS IN DETAIL(DESCRIPTION)


WITH FLOW SHEET

From the above described processes we select the third process of Hexamine manufacture.
The description the first process itself tells that how disadvantageous the process is. The
reaction is strongly exothermic and hence it is difficult to control the heat evolved and this
high temperature may lead to formation of byproducts that may be harmful. Due to high
temperature evolution large cooling surfaces are needed to be provided leading to increase
in the cost of manufacture. The earlier method of Hexamine production used batch process
hence the process is very much time consuming as compared to our selected process. The
labor cost is also added as the process is a batch one.

In the second given process both the reactants react in gaseous form and hence it is very
difficult reaction. This is because ammonia in the gaseous form may prove very dangerous.
Moreover the concentrations of ammonia and formaldehyde must be kept low. Otherwise
there will be loss of the gases (due to passing off with vapours) and ultimately cause loss to
the reaction.

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PROCESS DESCRIPTION

The feed of aqueous formaldehyde from the storage tank is charged in an agitated and
refrigerated steel reactor. Ammonia and formaldehyde both are stored in storage tanks.
Ammonia is then introduced in the formaldehyde solution. Ammonia added is kept slightly
in excess to prevent side reactions to occur. The reaction is continued and the pH is
maintained to about 8. The formaldehyde for the reaction may be produced from methanol.
The reaction mixture is kept for 9 hours. At this time the product should be alkaline to
phenolphthalein. As the stoichiometry shows water formation takes place due to the
reaction. The mixture of Hexamine and water is then removed from the agitated steel
reactor.

The liquid product in the outlet is then sent for several unit operations for achieving pure
Hexamine. Activated charcoal is added for filtration of the liquid product (Hexamine) and
then the liquid is filtered through canvas in the filter press. The liquid is evaporated at a
maximum temperature of 30 oC and the pressure is kept about 20-30 mmHg. Aqueous
ammonia is again added at a rate of 7 ml/min for stability. The remaining mass comprising
of solids is washed and centrifuged with 1 Kg 25% of ammonia. The product is dried in the
drier at 30 oC. By processing the mother liquor the yield may be increased to 96-100%.

The hexamine waste water is sent for purification to waste water treatment or the effluent
treatment plant and cation exchange processes.

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Major engineering problems:

The effective treatment of hexamine waste water is one of the major problems or the
producers of Hexamine. The waste water generally contains residual amounts of reactants
i.e. formaldehyde and ammonia. As well as residual amounts of Hexamine. It is very
essential for removal of these impurities from water. There is no general process or
hexamine water treatment.

Firstly the waste water is sent for distillation to remove all the volatile impurities. The
waste water is sent through cation resins to remove cations. The cation resin is used such
that it can be regenerated. Then they are passed through exposure to ultra violet rays or
bacteria culture (bacteriological treatment) or removal of formaldehyde.

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Chapter-7
MAJOR EQUIPMENT
REQUIRED

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MAJOR EQUIPMENT REQUIRED


Fomaldhyde storage.
Condition in the tank.
Temp = 250o C
Pressure = 1 atm
Capacity = 2275x 10 = 22750 kg (for 10 days supply)
22750
Total volume of storage required
1071kg / m3
= 21.24 m3
Gross volume = 1.5 x 21.24
= 451139 m3
L
Taking =2
D
D =3m
L =6m
Material of construction = mild steel
Thickness = 6mm

Agitator reactor.
Capacity = 19500 kg
Volume of NaOH = 18.829 m3
Gross volume = 19.24 m3
Diameter = 2.3 m
Height = 4.6 m
T = 25o C
P = 1 atm
Thickness = 6 mm
Material = mild steel

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Ammonia storage tank


Capacity = 13200 kg

Volume = 1221.8 m3
Taking 3 equal size tank of
Diameter = 6.8 m
Length = 13.6 m
P = 6 atm
Thickness = 6 mm
Material = s.s 316

Filter press :

Substance volume
Fomaldhyde (2275 kg) 2.1292
50% NaOH (1950kg) 1.283
3.41 m3

Gross Volume = 1.5 x 3.41


= 5.1106 m3
Diameter = 1.5 m
Length =3m
Agitator (no. 1) = turbine type

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Centrifuge washer:
Substance volume
ammonia (3933.3 kg) 2.55 m 3
Water (3700 kg) 3.7 m 3
Gross volume = 1.5 x 6.25 = 9.375m 3
Diameter = 1.82 m
Length = 3.64 m
Thickness = 6 mm
Material = s.s
Ambient pressure and temperature.

Evaporator :

Duty: 1. evaporator 1410.6 kg of water from 28072.2 kg Na Phenate solution and convert
it to dry powder(130o C, 1 atm )
2. 2807.2 kg solid Na Phenate is reacted with 1320 kg CO2 gas at 6 atm and 140oC .

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Chapter-8
MAJOR
INSTRUMENTATION
REQUIRED

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MAJOR INSTRUMENTATION REQUIRED

Pressure Measurement:

Pressure Gauge:

The bourdon tube is most frequently used in the pressure gauge. A bourdon tube consist of
a long think walled cylinder of non circular cross section sealed at the end, made from
materials such as phosphor bronze, steel & beryllium copper, and attached by a light line
work to the mechanism which operates the pointer. The other and of tube is fixed and is
open for the application of the pressure which is to be measured.

The tube is soldered or wended to a socket at the based, through which pressure connection
is made. Bourdon tube is available in many shapes like, c type, spiral, & helical.

Advantages:-
1. Cost is low
2. Construction is simple
3. Life is long
4. Efficiency is high
5. Tubes are in different range

Disadvantages:-
1. Spring gradient is low (50psig)
2. Shock and vibration effect

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Temperature Measurement:

Temperature has been defined in a variety of ways. One example defines temperature as
the measure of heat associated with the movement of the molecules of a substance. This
definition is based on the fact that the molecules of all matter are in continuous motion that
is sensed as heat.

Another definition is based on the concept of thermodynamics. Thermal energy always


flows from a warmer body to a cooler body. In this case, temperature is defined as an
intrinsic property of matter that quantifies the ability of the one body to transfer thermal
energy to another body. If two bodies are in thermal equilibrium and no energy is
exchanged, the bodies are at the same temperature.
In simplest terms, the temperature is the measurement of the hotness or coldness of the
body.

Temperature Measuring Devices:

Consistent measurement of the temperature is an important part of the process control.


Therefore, it is essential that the temperature measuring device must be reliable.

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While there are many types of temperature sensing devices, they can be classified into two
major groups temperature sensors and absolute thermometer. Three of the most common
types of the temperature sensors are thermocouples, resistance temperature devices, and
filled systems.

Temperature depends on the properties of some of the particular material, such as a gas,
liquid, metal and alloy for their temperature indications. Typically, temperature indications
are based on the material properties such as the coefficient of expansion, temperature
dependence of electrical resistance, thermoelectric power and velocity of sound.

Flow Measurement:

Flow is one of the most difficult process variables to measure accurately. One of the
simplest methods for determining the flow rate is the fluid per unit time method, which
assumes a basic premise of the fluid mechanics that mass is a conserved quantity. The
mass entering a system is equal to the mass leaving the system and both are measured over
the same time interval.
This method for accurate flow measurement takes into consideration two basic properties
of fluid, which are density and viscosity and their effect on the accuracy of flow
measurement. The instruments used are Differential pressure meter and orifice plates

Level Measurement:

Level is measured at the position of the interface between phases, where the phases are
liquid/gas, solid/gas, or immiscible liquid/liquid. Level is simply a measure of height

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defining the position of the interface that is the surface where the two phases meet with
respect to a reference point. This measurement is often converted to a volumetric or
gravimetric quantity. So level may be measured directly by defining the position of the
interface or indirectly by measuring another quantity, such as volume and interfacing the
level measurement by converting the quantity to a level measurement.

Level is a vertical measurement taken from the surface or interface to a fixed point.
Normally the reference point is the bottom of the vessel holding the substance. As with
most process variables, level can be measured by both direct and indirect methods.
The level measurement is done by Level Gauge, Differential pressure level detector,
Displacer Level detector, Ultrasonic Level detector.

Ph Meter:

In our required process we need to maintain pH of 8.0. Because of this we use the
following specifications.

Make: BELTA INSTRUMENTS


Model series: 671 P
While measuring pH:

Match the filling solution of the reference electrode to the sample, to minimize
junction potential problems.
Select a pH electrode with lower resistance glass rinsing the electrode with
appropriate solvents, and then soaking in pH buffer.
Add a quaternary ammonium salt to the sample to improve conductivity, or select
an electrode with lower resistance.

Pure water pH measurement kit:

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HEXAMINE 2013-2014

Method have been developed which minimizes the problems encountered when measuring
Ph in pure waters. The method uses a quality glass pH electrode and special set of a pure
water pH additive & a special se of diluted buffers containing the same background of
pure water pH additive.

Adding the pure water pH additive to the samples increases the ionic strength thus
reducing the noise and improving time. The shift in pH caused by the addition of the pure
water pH additive is minimal, between 0.005 & 0.01 pH units, since the same amount of
pure water pH additive is added to the buffers and samples the net effect on the pH is
negligible.

Control Valves:

Valve Sizing:-

Correct valve sizing is absolutely necessary for efficient and economical process control
installation. Selection of suitable flow data for sizing calculation should proceed with great
care. Realistic valves for minimum flow conditions are the most frequent reasons for
incorrect sizing.

Since the control valve is an adjustable orifice its area is automatically changed by the
controlling instrument to produce rate of flow under varying pressure drop condition.
Therefore available operating range is sacrifice when pressure drops are specified too low,
and when safety factors are unnecessarily high.
The amount of the operational pressure drop require for good control is a function of the
pressure differential across the valve with respect to the drop through the entire system.
The operational pressure drop should be at least 1/3 or of the total system pressure drop.

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Types of Control Valves :-

In the process industries there are various types of the control elements in which control
valve is one and is the final control element in any of the process loop. Control valve has a
vast classification according to its various parameters, mechanisms and many other factors.
Depending upon that all here following valves are described in brief with their features and
applications:

1) Globe valves
2) Bellow sealed valves
3) Butterfly valves
4) Ball valves
5) Diaphragm valves
6) Pressure Reducing valves

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HEXAMINE 2013-2014

Chapter-9
Utilities required

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Utilities required

Utilities of plant are as follows:

Steam
Cooling water
Raw water
DM water
Instrument air
Air

STEAM:

Steam is the important utility for heating purposes


Steam of 5 kg/cm2 is produced in boiler
Water is heated in a boiler
Steam generates in boiler is medium pressure steam
From boiler ,steam is supplied to the plant through pipelines

COOLING WATER:

In Lactic acid plant cooling water is required for cooling process.


Cooling water is used in every chemical process industry.
PH of water is 7-7.5.
Total hardness is maximum 600 ppm.
Total dissolved solid is maximum 800 ppm.
Cooling water is produced in cooling towers.
Color code for cooling water pipelines is green.

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RAW WATER:

It is the basic requirement of all industries.


Raw water is used for making slurries, solutions etc.
It is also used for domestic purposes.
Every chemical industry has its own raw water sump.
Color code for raw water is blue.

DM WATER:

DM WATER passes through de-aerator where Oxygen is removed and then it is


used as Boiler Feed Water for Steam generation.
De mineralized water is used in many places such as,
Cooling water plant, Boiler feed & for process solvent.
INSTRUMENT AIR:
Instrument air is normally supplied from the dry air stream for regulating
controllers, valves and auto controlling instruments.
Dew point of instrument air -35 deg C.
AIR:
Air should be dust free and moisture free.
Plant air can also be used for flushing the vessel purpose.
Temperature of air is atmospheric temperature.

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Chapter-10
Layout and location of plant

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HEXAMINE 2013-2014

Layout and location of plant

The geographical location of the final plant can have strong influence on the success of the
industrial venture. Considerable care must be exercised in selecting the plant site, and
many different factors must be considered. Primarily the plant must be located where the
minimum cost of production and distribution can be obtained but, other factors such as
room for expansion and safe giving conditions for plant operation as well as the
surrounding community are also important. The location of the plant can also have a
crucial effect on the profitability of a project.

The choice of the rural site should first of all based on a complete survey of the advantages
and disadvantages of various geographical areas and ultimately, oil the advantages and
disadvantages of the available real estate. The various principal factors that must be
considered while selecting a suitable plant site are briefly discussed in this section. Tile
factors to be considered are:

1. raw material availability


2. location (with respect to the marketing area)
3. availability of suitable land
4. transport facilities
5. availability of labors
6. availability of utilities (water, electricity)
7. environmental impact and effluent disposal
8. local community considerations
9. climate
10. political strategic considerations
11. taxations and legal restrictions

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Raw material availability:

The source of raw materials is one of the most important factors influence site selection of
a plant site. This is particularly true for the sulfuric acid plant because large volumes of
sulfur are consumed in the process which will result the reduction of the transportation and
the storage charges. Attention should be given to the purchased price of the raw materials,
distance from the source of supply, freight and transportation expenses, availability and
reliability of supply, purity of raw materials and storage requirements.

Location:

The location of markets or intermediate distribution centers affects tile cost of product
distribution and time required for shipping. Proximity to the major markets is an important
consideration in the selection of the plant site, because the buyer usually finds
advantageous to purchase from near by sources. In case of sulfuric acid plant, the major
consumers are fertilizer industries and hence the plant should be erected in close proximity
to those units.

Availability of suitable land:

The characteristics of the land at the proposed plant site should be examined carefully. The
topography of the tract of land structure must be considered; since either of both may have
a pronounced effect on the construction costs. The cost of the land is important, as well as
local building cost sand living conditions. Future changes may make it desirable or
necessary to expand the plant facilities. The land should be ideally flat, well drained and
have load-bearing characteristics. A full site evaluation should be made to determine the
need for piling or other special foundations.

Transport:

The transport of materials and products to and from plant will be an overriding
consideration in site selection. If practicable, a site should be selected so that it is close to

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at least two major forms of transport: road, rail, waterway or a seaport. Road transport is
being increasingly used, and is suitable for local distribution from a central warehouse.
Rail transport will be cheaper for the long distance transport. If possible the plant site
should have access to all three types of transportations. There is usually need for
convenient rail and air transportation facilities between the plant and the main company
head quarters, and the effective transportation facilities for the plant personnel are
necessary.

Availability of labors:

Labors will be needed for construction of the plant and its operation. Skilled construction
workers will usually be brought him from outside the site, but there should be ail adequate
pool of unskilled labors available locality, and labors suitable for training to operate the
plant. Skilled tradesmen will be needed for plant maintenance. Local trade union customs
and restrictive practices will have to be considered when assessing tile availability and
suitability of the labors for recruitment and training.

Availability of utilities:

The utilities is generally used for the ancillary services needed in the operation of any
production process. These services will normally be supplied from a central facility and
includes water, fuel and electricity which are briefly described as follows:

Water:-
Tile water is required for large industrial as well as general purposes, starting with water
for cooling washing, steam generation and as a raw material ]it the production of sulfuric
acid. The plant therefore must be located where a dependable water supply is available
namely lakes, rivers, wells, seas. It the water supply shows seasonal fluctuations, its
desirable to construct a reservoir or to drill several standby wells. Tile temperature, mineral
content, slit and sand content, bacteriological content, and cost for supply and purifications
treatment must also be considered when choosing a water supply. Demineralized water,

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from which all the minerals have been removed is used where pure water is needed for the
process use, in boiler feed. Natural and forced draft cooling towers are generally used to
provide the cooling water required on site.

Electricity:
Power and steam requirements are high in most industrial plants and fuel is ordinarily
required to supply these utilities. Power, fuel and stem are required for running, the various
equipments like generators, motors, turbines, plant lighting and general use and thus be
considered as one major factor is choice of plant site.

Environmental impact and effluent disposal:

Facilities must be provided for the effective disposal of the effluent without any public
nuisance. In choosing a plant site, the permissible tolerance levels for various effluents
should be considered and attention should be given to potential requirements for additional
waste treatment facilities. As all industrial processes produce waste products, full
consideration must be given to the difficulties and coat of their disposal. The disposal of
toxic and harmful effluents will be covered by local regulations, and the appropriate
authorities must be consulted during the initial site survey to determine the standards that
must be met.

Local community considerations:

The proposed plant must fit with and be acceptable to the local community. Full
consideration must be given to the safe location of the plant so that it does not impose a
significant additional risk to the community

Climate:

Adverse climatic conditions at site will increase costs. Extremes of low temperatures will
require the provision of additional insulation and special heating for equipment and piping.
Similarly, excessive humidity and hot temperatures pose serious problems must be

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considered for selection a site for the plant. Stronger structures will be needed at locations
subject to high wind loads or earthquakes.

Political and strategic consideration:

Capital grants tax concessions, and other inducements are often given by governments to
direct new investments to preferred locations, such as areas of high unemployment. The
availability of such grants can be the overriding considerations in site selection.

Taxation and legal restrictions:

State and local tax rates on property income, unemployment insurance, and similarly items
vary from one location to another. Similarly, local regulations on zoning, building codes,
nuisance aspects and other facilities can have influence in the final choice of the plant site.

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Chapter-11
Site selection parameter

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Site selection parameter

Plant layout:

After the flow process diagrams are completed and before detailed piping, structural and
electrical design can been, the layout of process units in a plant and the equipment within
these process unit must be planned. This layout can play an important part in determining
construction and manufacturing costs, and thus must be planned carefully with attention
been given to future problems that may arise.

Thus the economic construction and efficient operation of a process unit will depend on
how well the plant and equipment specified on the process flow sheet is laid out. Tile
principal factors that are considered are listed below:
1. Economic consideration: construction and operating costs.
2. Process requirements.
3. Convenience of operation.
4. Convenience of maintenance.
5. Health and safety considerations.
6. Future plant expansion.
7. Modular construction.
8. Waste disposal requirements.

Costs:

The cost of construction can be minimized by adopting a layout that gives the shortest run
of connecting pipe between equipment, and least amount of structural steel work.
However, this will not necessarily be the best arrangement for operation and maintenance.

Process requirements:

An example of the need to take into account process consideration is the need to elevate
the base columns to provide the necessary net positive suction head to pump.

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Convenience of operation:

Equipment that needs to have frequent attention should be located convenient to the
control room. Valves, sample points, and 4isti-umeiits should be located at convenient
positions and height. Sufficient working space and headroom must be provided to allow
easy access to equipment.

Convenience of maintenance:

Heat exchanges need to be sited so that the tube bundles can be easily withdrawal for
cleaning and tube replacement. Vessels that require frequent replacement of catalyst or
packing should be located on the outside of building. Equipment that requires dismantling
for maintenance, such as compressors and large pumps, should be places under cover.

Healthy and safety considerations:

Blast walls may be needed to isolate potentially hazardous equipment, and confine tile
effects of an explosion. At least two escape routes for operators must be provided from
each level in process buildings

Future plant expansion:

Equipment should be located so that it can be conveniently tied in with any future
expansion of the process. Space should be left on pipe alleys for future needs, and service
pipes over-sized to allow for future requirements.

Modular construction:

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In recent years there has been a move to assemble sections of plant at tile plant
manufacturers site. These modules will include the equipment, structural steel, piping and
its instrumentation. The modules are then transported to the plant site, by road or sea.
The advantages of modular construction are:
1. Improved quality control.
2. Reduces construction cost.
3. Less need for skilled labors on site.

The disadvantages of modular construction are:


1. Higher design costs & more structural steel work.

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PLANT LAYOUT

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Chapter-12
Economic evalution

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Economic evaluation
Basis Ton/day Working day Ton/year
Plant Capacity 30 350 10500

Raw Material costs:


Chemicals Rs./kg Ton/day Ton /year Rs./year
formaldehyde 22 42.855 14999.25 329983500
NH3 20 16.131 5645.85 112917000
Total 442900500

Operating Labor Costs:


Position Nos. Pay/month pay/year
M.D. 1 60000 720000
V.P. 0 40000 0
G.M. 1 35000 420000
Production
1 28000 336000
Manager
Plant Incharge 1 15000 180000
Product.
5 12000 720000
Engineer
Supervisor 10 6000 720000
Technician 3 3000 108000
Chemist 2 6000 144000
Clerk 6 3500 252000
Peon 4 2000 96000
Skilled labours 10 4000 480000
Unskilled
20 3000 720000
labours
Total 4896000

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Purchased Equipment Cost:

Total
Equipments No Capacity Price/unit
price
Reactor 1 10 M 1,700,000 1,700,000
Centrifuge 1 10hp 533617 533,617
Dryer 1 9M 1533617 1533617
NH3 liquefaction Plant 1 1000000 1000000
Pumps 8 5hp 41500 332,000
Storage tank 1 50M 932567 1865134
NH3 Storage tank 1 20M 465000 465,000
Water Storage tank 1 50M 932567 932567
Boiler 1 7M 1265655 1,265,655
Cooling Tower 1 355690 355,690
Holding Tank 2 20M 565000 1130000
Total 9,579,663

Estimation of fixed Capital Cost:


I. Direct Costs:
A purchase equipment cost 9579663
Installation including insulation and
1 painting 40 % P.E.C. 3831865.2
2 Instrument. & control installed 10 % P.E.C. 957966.3
3 Piping installed 80 % P.E.C. 7663730.4
4 Electrical installed 15 % P.E.C. 1436949.45
B Building, process and auxiliaries 70 % P.E.C. 6705764.1
Service facilities and yard
C improvement 70 % P.E.C. 6705764.1
D Land 6 % P.E.C. 574779.78

Direct cost 37456482.3

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II. Indirect Costs:

3745648.23
A Engineering and supervision 10 % D.C. 3
Construction expenses and contractor 7491296.46
B fee 20 % D.C. 6
3745648.23
C Contingency 10 % D.C. 3

Indirect Cost 14982592.9

Fixed Capital Investment:

(iii) F.C.I. = Direct cost + Indirect cost 52439075.3

Working Capital:

13109768.8
(iv) Working capital 15 % T.C. 2

Total Capital Investment:

T.C.I. = Fixed capital investment + 65548844.0


1.25F.C.I.
(v) working capital. 8

ESTIMATION OF TOTAL PRODUCT COST:

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Manufacturing Cost:

Direct Product Cost:

1 raw material cost 10 to 50 % T.P.C. 442900500


2 Operating labour 10 to 50 % T.P.C. 4896000
3 Direct supervisory & clerical labours 15 % O.L.C. 734400
4 Utilities 15 % T.P.C. 132870150
3146344.51
5 Maintenance and repair 6 % F.C.I. 6
471951.677
6 Operating supplies 15 % M & R 4
7 Lab charges 10 % O.L.C. 489600
8 Patent and Royalty 2 % T.P.C. 17716020
603224966.
Direct product cost
2

Fixed Charges:

1 Depreciation 10 % F.C.I.+2 % Building 5378022.808


2 Local taxes 1 % F.C.I. 524390.7526
3 Insurance 1 % F.C.I. 524390.7526
4 Rent 8 % land & Building 582443.5104
Fixed charges 7009247.824

Plant Overhead:

1 Plant Overhead 50 % (O.L.C + sup. + Main) 4388372.258

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Manufacturing Cost:

Manufacturing cost :- D.P.C. + F.C. + P.O.C. 614622586.3

General Expenses:

A Adm. Cost 15 % Plant Overhead 658255.8387


Distribution and selling
B cost 10 % T.P.C. 88580100
C R.N.D. 5 % T.P.C. 44290050
General Expenses 133528405.8

Total Production Cost:

T.P.C. = mfg + General expenses 748150992.1 Cost/year

Total production cost /kg. 71.25247544 Rs/Kg

Selling Price:

Selling price :- 75 Rs/Kg

Total Income:

Total Income :- 787500000 Rs./year

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Gross Earning:

Gross Earning :- Total income- T.P.C. 39349007.89 Rs/year

Net Profit:

Net Profit :- Gross Earning-40 %G.E. 23609404.73 Rs/year

Pay Out Period:

Pay out peroid :- F.C.I /Net profit 2.22110959

( F.C.I+Dep/year) /(Net
Pay out peroid :- profit+Dep/year) 1.994557744

Rate of Return:
Rate of Return :- net profit/(F.C.I.+W.C.)100 36.01803367

Turn Over Ratio:


Turn Over Ratio = Gross annual
15.01742729
sales/(F.C.I.)
B.E.P n = F.C./(S.P-D.P.C)

F.C. 144926026 Rs
D.P.C /Kg 57.449997 Rs/kg
Sell Price 75 Rs/kg

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Chapter-13
Important aspects of safety

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HEXAMINE 2013-2014

Important aspects of safety


HEXAMETHYLENE TETRAMINE

Product name: Hexamethylene Tetramine


Synonyms: Hexamine; Aminoform; HMTA; Methenamine; Urotropin
Chemical Formula: C6H12N4

Hazards Identification:
Emergency Overview CAUTION! May form combustion dust concentrations in air.
nuisanance dust Irritating to eyes and respiratory system..

Adverse Human Health Effects:


1) Inhalation: Dust may be formed under certain conditions of use.
2) Harmful by ingestion. Irritating to eyes and respiratory system. May irritate skin. Used
medicinally as an antiseptic.
3) If ingested in large quantities can cause gastro-intestinal upsets. crystites,haematuria
and renal lesions due to evolution of formaldehyde. Environmental Effects Exposure will
make the air polluted by fishlike smell

Physical and Chemical Hazards:


1) None with water.
2) Can react with oxidizer

First-Aid Measures:

Inhalation: Remove from exposure, rest and keep warm.


In severe cases, obtain medical attention.

Ingestion: Wash out mouth thoroughly with water and give plenty of water to drink.
Obtain Medical Attention.

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Skin Contact
1) Wash off thoroughly with water.
2) Remove contaminated clothing and wash before re-used.
3) In severe cases, Obtain Medical Attention.
Eye Contact Irrigate thoroughly with water for at least 10 minutes.
If discomfort persists, Obtain Medical Attention.
Fire-Fighting Measures:
Extinguishing Media Foam, water fog, dry chemical. Fire and Explosion Hazards Fine dust
dispersed in air in sufficient concentrations, and in the presence of an ignition source is a
potential dust explosion hazard.May evolve toxic fumes in fire. Special Firefighting
Procedures. Special Equipment for the Protection of Firefighters In the event of a fire, wear
full protective clothing and NIOSH-approved self-contained breathing apparatus with full
facepiece operated in the pressure demand or other positive pressure mode and full
protective clothing for Chemicals.

Accidental Release Measures:


Personal Precautions Wear appropriate personal protective equipment

Environmental Precautions:
1) Remove all sources of ignition.
2)This material should be kept out of sewage and drainage systems and all bodies of water.
3) Clean up releases as soon as possible
4) Ventilate the area of leak .

Methods for Cleaning Up:


1) Spray the water mist to Avoid dust formation
2) Spill water to clean the area of leak
3) Pick up the wastewater to sewage farm.

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Handling and Storage:


Handling: Avoid dust formation and control ignition sources.

Storage:
1) Keep the Storage area dry , drafty and cool.
2) Keep away from all sources of ignition.
3) Keep away from the oxidisers
4) Make sure the extinguisher and Fire-detecting system was setting in appropriate place.
5) Store in a tightly closed container.

Exposure Controls / Personal Protection:


Engineering Measure:
1) Use adequate general or local exhaust ventilation to keep airborne-concentrations
below the permissible exposure limits.
2) Employ grounding, venting and explosion relief provisions in accord with accepted
engineering practices in any process capable of generating dust and/or static electricity.
Control parameters Limit values: No information available. Biological Standards: No
information available

Personal Protective Equipment Respiratory Protection: Dust respirator


Hand Protection: plastic or rubber gloves
Eye Protection: Goggles or face shield
Skin and Body Protection: Plastic apron,sleeves,boots-if handing large quantities.

Specific Hygiene Measures:


1) Eye bath.
2) Washing facilities.
3) Safety shower.

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4) Impermeable boots and apron as required to avoid prolonged or repeated contact.

Physical and Chemical Properties:


Physical State: solid Form White to ivory granule or powdered color White to ivory, Odor
fishlike smell, pH: 7.0~9.0 (100gr/l aq. at 20 oC ) Boiling Point: 263 oC
Decomposition Temperature: 260~263 oC Flash Point: 250 oC
Explosion Properties: 15 g/m3
Vapor pressure: Vapor density 4.88 (Air=1)
Density: 1.33 g/cm3 at 20 oC, 1.27 g/cm3 at 25 oC
Bulk Density: 600kg/m3
Solubility: 1) 853 g/l in H2O/ at 25 oC
2) Ethanol/ at 20 oC, soluble
3) Chloroform/ at 20 oC, soluble
4) Ethyl Ether/ at 20 oC, Insoluble
Stability and Reactivity:
Stability Stable under ordinary conditions of use and storage.
Possible Hazardous Reactions Occurring under Specific Conditions
1) Can react with oxidising materials
2) Will react with Hydrogen Peroxide to product an explosive material
HMTP(Hexamethylene Triperoxide Diamine)
3) Will react with Nitric Acid to product :Cyclotrimethylene Trinitriamine
Conditions to Avoid Heat, flame, ignition sources, dusting, Static electricity and
incompatibles.
Toxicological Information:
Acute toxicity
1) LD10 oral : Mouth 512 mg/kg.
2) LD50 oral : Lungs: 9200 mg/kg.
Local effects 1) Irritating to eyes,skin and respiratory system.
Sensitization 1) Irritating to eyes respiratory system,and skin.

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2) If ingested in large quantities can cause gastro-intestinal upsets.


crystites,haematuria and renal lesions due to evolution of formaldehyde.
Chronic Toxicity or Long Term Toxicity long Term contact with Hexamine is harmful to
health. .
Ecological Information:

This material forms a strongly basic aqueous solution, and this property may cause
adverse environmental effects.
It has the following properties: A high biochemical oxygen demand and a potential to
cause oxygen depletion in aqueous systems, a high potential to affect aquatic organisms,
a high potential to affect secondary waste treatment microbial metabolism, a high potential
to affect the germination and/or early growth of some plants, a low potential to
affect the growth of some plant seedlings, a low potential to biodegrade (Low persistence)
with unacclimated microorganisms from activated sludge, a low potential to
bioconcentrate. After dilution with a large amount of water, followed by secondary waste
treatment, this material is not expected to cause adverse environmental effects.
Disposal Considerations:
Recommended Methods for Safe and Environmentally Preferred Disposal
Dispose of in a manner consistent with federal, state, and local regulations.

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MATERIAL SAFETY DATA SHEET


AMMONIA

Description:

Chemical Name: Ammonia, Anhydrous


Synonyms: Ammonia, Liquefied
Chemical Family: Ammonia
Formula: NH3
Mol. Wt.:17.03

Health Hazard:

HAZARD DESCRIPTION: Irritant and corrosive to skin, eye, respiratory tract and
mucous membranes. May cause severe burns, eye and lung injuries. Skin and respiratory
related diseases aggravated by exposure. Not recognized by OSHA as a carcinogen. Not
listed in the National Toxicology Program annual report. Not listed as a carcinogen by the
International Agency for Research on Cancer.

Effects Of Overexposure:

Eye: lachrymation, edema, blindness.

Skin: Irritation, corrosive burns, blisters formation. Contact with liquid will freeze the
tissue, then produces a caustic burn. Inhalation: heavy, acute exposure may result in severe
irritation of the respiratory tract, glottal edema, bronchialspasm, pulmonary edema and
respiratory arrest.

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Chronic effects: Bronchitis. Extreme exposure (5000 ppm) can cause immediate death
from spasm, inflammation or edema of larynx.

Emergency Aid:

Skin: flush with copious amounts of water while removing contaminated clothing and
shoes. Do not rub, or apply ointment on affected area Ingestion: if conscious, give large
amount of water to drink. Refer immediately to physician.

Eye: flush with copious amounts of water for 15 min. Eyelids should be held apart and
away from eyeball for thorough rinsing. Speed and thoroughness in rinsing the eye is most
important in preventing latent permanent injuries. Inhalation: remove to fresh air.
Administer oxygen or artificial respiration if necessary.

Note to Physician: Lung injury may appear as delayed phenomenon, pulmonary edema
may follow chemical bronchitis. Supportive treatment with necessary ventilation actions,
including oxygen, may warrant consideration.
Physical Data:

Boiling Pt: -33 C (-28 F)


Freezing Pt: -78 C (-108 F)
Vapor Density (AIR=1): 0.596 @ 0 C (32 F)
Vapor Pressure: 10 atm @ 25.7 C
Solubilty in Water: 89.9 g/100cc @ 0C
Specific Gravity (H2O=1): 0.682 @ 4 C (39 F)
Evaporation Rate (Water=1) Faster than water
Percent Volatile: 100%
Surface Tension: 23.4 Dynes/cm @ 11.1C
Appearance & Odor: Colorless gas/liquid and pungent odor

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Fire and Explosion Hazard Data:

Flash Point: None


Auto ignition Temp: 651 C (1204F) catalyzed by iron; 850 C (1562F) uncatalyzed
Flammable Limits In Air: LEL 15% UEL 28%
Extinguishing Media: Non-combustible

Special Fire-Fighting Procedures:


Must wear protective clothing and respiratory protection. Stop source if possible. Cool fire
exposed containers with water spray. Stay upwind and use water spray to knock down
vapor and dilute.

Unusual Fire and Explosion Hazards:

Not generally a fire hazard. If relief valves are inoperative, heat-exposed storage containers
may become explosion hazards. Ammonia contact with chemicals such as mercury,
chlorine, iodine, bromine, silver oxide, or hypochlorites can form explosive compounds.
Special hazards with chlorine to form chloramine gas, also a primary skin irritant and
sensitizer. Combustion may form toxic nitrogen oxides.

Chemical Reactivity

Stability:

Stable at room temperature. Ammonia will react exothermically with acids and water.

Conditions To Avoid:

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Avoid mixing with sulfuric acid or other strong mineral acids. Avoid mixing with
hypochlorites (chlorine bleach) or other halogens and sodium hydroxide. Avoid contact
with galvanized surfaces, copper, brass, bronze, aluminum alloys, mercury, gold, silver,
and strong oxidizers. Avoid heating.

Hazardous Decomposition Products:


Hydrogen and nitrogen gases above 450 C (842 F)
Steps To Be Taken:
Wear respiratory protection and protective clothing, see
Protective Equipment:

Stop source if possible. If Exposure concerns are present, stay upwind and use water spray
downwind of leak source to absorb ammonia gas and dilute.
CAUTION: Adding water directly to liquid spills will increase volatilization of ammonia,
thus increasing possibility of exposure.
Waste Disposal:

Listed as hazardous substance under CWA (40 CFR 1164.40 CFR 117.3 Reportable
Quantity 100 lbs. OR 45.4kg) Classed as a hazardous waste under RCRA (40 CFR 261.32
Corrosive # D002). Comply with all regulations. Suitably diluted product may be disposed
of on agricultural land as fertilizer. Keep spill from entering streams or lakes.

Special Protection And Procedures:

Respiratory Protection:

MSHA/NIOSH approved respiratory protection with full face piece for gas and vapor
contaminants effective for anhydrous ammonia and able to be used for entry and escape in
emergencies. Refer to 29 CFR 1910.134 and ANSI: Z88.2 for requirements and selection.

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Ventilation:

Local exhaust sufficient to keep ammonia gas below Permissible Exposure Limits. Refer to
29 CFR 1910.134 and ANSI: Z9.2 for requirements and selection.

Protective Equipment:

Splash-proof, chemical safety goggles, rubber gloves and boots to prevent contact.
Respiratory protection. Cotton work clothes recommended. Refer to 29 CFR 1910.132 to
1910.136 for requirements.
Special Precautions
Storage And Handling:

Store in cool, well-ventilated area with containers tightly closed. OSHA 29 CFR 1910.111
prescribes handling and storage requirements for anhydrous ammonia as a hazardous
material.
Work-Place Protective Equipment:

As discussed above should be near, but outside of ammonia area. Eyewash and safety
shower in immediate vicinity. See 29 CFR 1910.141 for workplace requirements.

Disposal:
Ammonia is listed as a hazardous substance under FWPCA. See WASTE

Personal:
Avoid unnecessary exposure. Use protective equipment as needed. Do not wear contact
lenses.

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MATERIAL SAFETY DATA SHEET


FORMALDEHYDE

Product Name: Formaldehyde 37% solution


Synonym: Formalin
Chemical Name: Formaldehyde
Chemical Formula: HCHO

Hazards Identification:
Potential Acute Health Effects:
Very hazardous in case of eye contact (irritant), of ingestion, . Hazardous in case of skin
contact (irritant, sensitizer, permeator), of eye contact (corrosive). Slightly hazardous in
case of skin contact (corrosive). Severe over-exposure can result in death. Inflammation of
the eye is characterized by redness, watering, and itching.

First Aid Measures

Eye Contact:
Check for and remove any contact lenses. Immediately flush eyes with running water for at
least 15 minutes, keeping eyelids open. Cold water may be used. Get medical attention
immediately.

Skin Contact:
In case of contact, immediately flush skin with plenty of water. Cover the irritated skin
with an emollient. Remove contaminated clothing and shoes. Cold water may be
used.Wash clothing before reuse. Thoroughly clean shoes before reuse. Get medical
attention.

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Serious Skin Contact:


Wash with a disinfectant soap and cover the contaminated skin with an anti-bacterial
cream. Seek immediate medical attention.
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is
difficult, give oxygen. Get medical attention immediately.
Serious Inhalation:
Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a
collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the victim is not
breathing, perform mouth-to-mouth resuscitation. WARNING: It may be hazardous to the
person providing aid to give mouth-to-mouth resuscitation when the inhaled material is
toxic, infectious or corrosive. Seek immediate medical attention.
Ingestion:
If swallowed, do not induce vomiting unless directed to do so by medical personnel. Never
give anything by mouth to an unconscious person. Loosen tight clothing such as a collar,
tie, belt or waistband. Get medical attention immediately.

Fire and Explosion Data

Flammability of the Product: Flammable.

Fire Hazards in Presence of Various Substances:


Flammable in presence of open flames and sparks, of heat.
Non-flammable in presence of shocks, of oxidizing materials, of reducing materials, of
combustible materials, of organic materials, of metals, of acids, of alkalis.

Fire Fighting Media and Instructions:


Flammable liquid, soluble or dispersed in water.
SMALL FIRE: Use DRY chemical powder.

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LARGE FIRE: Use alcohol foam, water spray or fog. Cool containing vessels with water
jet in order to prevent pressure build-up, autoignition or explosion.

Special Remarks on Fire Hazards:


Explosive in the form of vapor when exposed to heat or flame. Vapor may travel
considerable distance to source of ignition and flash back. When heated to decomposition,
it emits acrid smoke and irritating fumes.
CAUTION: MAY BURN WITH NEAR INVISIBLE FLAME (Methyl alcohol)

Special Remarks on Explosion Hazards:


Reaction with peroxide, nitrogen dioxide, and permformic acid can cause an explosion.
(Formaldehyde gas)

Accidental Release Measures

Small Spill:
Dilute with water and mop up, or absorb with an inert dry material and place in an
appropriate waste disposal container. If necessary: Neutralize the residue with a dilute
solution of sodium carbonate.

Large Spill:
Flammable liquid. Poisonous liquid.
Keep away from heat. Keep away from sources of ignition. Stop leak if without risk.
Absorb with DRY earth, sand or other non-combustible material. Do not get water inside
container. Do not touch spilled material. Use water spray to reduce vapors. Prevent entry
into sewers, basements or confined areas; dike if needed. Call for assistance on disposal.
Neutralize the residue with a dilute solution of sodium carbonate. Be careful that the
product is not present at a concentration level above TLV. Check TLV on the MSDS and
with local authorities.

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Handling and Storage:


Precautions:
Keep away from heat. Keep away from sources of ignition. Ground all equipment
containing material. Do not ingest. Do not breathe gas/fumes/ vapor/spray. In case of
insufficient ventilation, wear suitable respiratory equipment. If ingested, seek medical
advice immediately and show the container or the label. Avoid contact with skin and eyes.
Keep away from incompatibles such as oxidizing agents, reducing agents, acids, alkalis,
moisture.
Storage:
Store in a segregated and approved area. Keep container in a cool, well-ventilated area.
Keep container tightly closed and sealed until ready for use. Avoid all possible sources of
ignition (spark or flame).

Exposure Controls/Personal Protection


Engineering Controls:
Provide exhaust ventilation or other engineering controls to keep the airborne
concentrations of vapors below their respective threshold limit value. Ensure that eyewash
stations and safety showers are proximal to the work-station location.

Personal Protection:
Safety glasses. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator
or equivalent. Gloves (impervious).

Personal Protection in Case of a Large Spill:


Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained breathing
apparatus should be used to avoid inhalation of the product. Suggested protective clothing
might not be sufficient; consult a specialist

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Physical and Chemical Properties


Physical state and appearance: Liquid.
Odor: Pungent. Suffocating. (Strong.)
Taste: Not available.
Molecular Weight: 30.02
Color: Clear Colorless.
pH (1% soln/water): 3 [Acidic.] pH of the solution as is.
Boiling Point: 98C (208.4F)
Melting Point: -15C (5F)
Critical Temperature: The lowest known value is 240C (464F) (Methyl alcohol).
Specific Gravity: 1.08 (Water = 1)
Vapor Pressure: 2.4 kPa (@ 20C)
Vapor Density: 1.03 (Air = 1)
Volatility: 100% (w/w).
Odor Threshold: The highest known value is 100 ppm (Methyl alcohol)
Ionicity (in Water): Non-ionic.
Dispersion Properties: See solubility in water, diethyl ether, acetone.
Solubility:
Easily soluble in cold water, hot water.
Soluble in diethyl ether, acetone, alcohol
Section 10: Stability and Reactivity Data
Stability: The product is stable.
Instability Temperature: Not available.
Conditions of Instability: Heat, ignition sources (flames, sparks), incompatible materials
Incompatibility with various substances:
Reactive with oxidizing agents, reducing agents, acids, alkalis. Slightly reactive to reactive
with metals.
Corrosivity: Non-corrosive in presence of glass.
Polymerization: Will not occur.

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Toxicological Information
Routes of Entry: Absorbed through skin. Dermal contact. Eye contact. Inhalation.
Toxicity to Animals:
Acute oral toxicity (LD50): 42 mg/kg [Mouse]. (Formaldehyde)
Acute dermal toxicity (LD50): 15800 mg/kg [Rabbit]. (Methyl alcohol).
Acute toxicity of the mist(LC50): 454000 mg/m
4 hours [Mouse]. (Formaldehyde)
Toxic Effects on Humans:
Very hazardous in case of ingestion, .Hazardous in case of skin contact (irritant, sensitizer,
permeator), of eye contact (corrosive), of inhalation (lung corrosive). Slightly hazardous in
case of skin contact (corrosive). Ingestion: Prolonged or repeated ingestion may cause
gastrointestinal tract irritation and ulceration or bleeding from the stomach. Other effects
may be similar to that of acute ingestion.
Disposal Considerations
Waste Disposal:
Waste must be disposed of in accordance with federal, state and local environmental
control regulations.

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Chapter-14
Effluent treatment related to
product

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Effluent treatment related to product

WASTEWATER TREATMENT TECHNOLOGIES

Wastewater treatment can be divided into four major categories or steps-

1. Preliminary treatment - It involves a number of unit processes to eliminate undesirable


characteristics of wastewater. Processes include use of screen sand grates for removal of
large particles, communitors for grinding of coarse solids, pre-aeration for odour control
and some removal of grease.

2. Primary treatment- It involves removal of readily settable solids prior to biological


treatment. Sedimentation chambers are the main units involved but various auxiliary
processes such as floatation, flocculation and fine screening may also be used.

3. Secondary treatment- It involves purification of waste water primarily by


decomposition of suspended and dissolved organic matter by microbial action. A number
of processes are available but mainly used are land treatment, activated sludge process or
the biological filtration methods.

4. Auxiliary treatment- This mainly includes large number of physical and chemical
treatment processes that can be used before or after the biological treatment to meet the
treatment objectives.

PHYSICAL TREATMENT PROCESSES


Physical treatment separates solids from wastewater mechanically with screens or using
density difference as with sedimentation and floatation.

PRELIMINARY TREATMENT - These are mainly physical processes. This includes-

Grit chambers use gravity to remove grit and dirt which mainly consists of mineral
particles and coarse screens strain out large solids and when organic material enters as
large particles comminutors can be used to reduce particle size to enhance treatment in
later stages.

Equalisation- Equalisation is a process to equalise wastes by holding waste streams in a


tank for a certain period of time prior to treatment in order to obtain a stable waste
stream that is easier to treat. Equalisation helps in mixing smaller volumes of
concentrated wastes with larger volumes at lower concentrations. It also controls the pH
to prevent fluctuations that could upset the efficiency of treatment system, by mixing
acid and alkaline wastes. Equalisation tanks are equipped with agitators that help not
only in proper mixing of waste water but also prevent suspended solids from settling to
the bottom of the unit.

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Pre-aeration or pre-chlorination- This process helps in controlling odours if


wastewater becomes oxygen deficient while travelling through the sewer collection
system. It also helps in grease removal during primary clarification.

PRIMARY TREATMENT - These are also mainly physical processes. These include-

Sedimentation- Removal of readily settleable inert and organic solids is accomplished in


sedimentation. Fine screens may also be used in the treatment process. Sedimentation
chambers may also include baffles and oil skimmers to remove grease and floatable
solids and may include mechanical scrapers for removal of sludge at the bottom of the
chamber.

Dissolved air floatation- It is the process of using fine bubbles to induce suspended
particles to raise to the surface tank where they can be collected and removed. Gas
bubbles are introduced into the wastewater and attach themselves to the particles, thus
reducing their specific gravity and causing them to float. Bubbles may be generated by
dispersing air mechanically

Flocculation- It is physical- chemical process that encourages the aggregation of


coagulated colloidal and finely divided suspended matter by physical mixing or
chemical coagulant aids. Flocculation process consists of a rapid mix tank and a
flocculation tank. The waste stream is initially mixed with a coagulant in the rapid mix
tank and after mixing the coagulated waste water flows to the flocculation basin where
slow mixing of waste occurs which allows the particles to agglomerate into heavier
more settleable solids. Either mechanical paddles or diffused air provide mixing. Three
different types of chemicals used in coagulation are inorganic electrolytes, natural
organic polymers and synthetic poly electrolytes. The selection of a specific chemical
depends on the characteristics and chemical properties of the contaminants.

Emulsion breaking- It involves addition of chemicals and/or heat to cause dispersed oil
droplets to coalesce and separate from the wastewater. This process mainly used for
pre-treatment of oily wastewater. Commonly used method is acid cracking where
sulphuric or hydrochloric acid is added to the oil water mixture until pH reaches 1 or 2.
Another alternative to this is where emulsion breaking chemicals such as surfactants
and coagulants are added to the mixture and the contents are mixed. After the emulsion
bond is broken, oil residue is allowed to float to the top of the tank. Heat may be applied
to speed the separation process. The oil is then skimmed by mechanical means or the
water is decanted from the bottom of the tank.

Clarification- Clarification system utilise gravity to provide continuous, low cost


separation and removal of particulate, flocculated impurities and precipitates from
water and generally follow the processes which generate suspended solids such as
biological treatment. In a clarifier wastewater is allowed to flow slowly and uniformly,
permitting the solids more dense than water to settle down. The clarified water flows

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from the top of the clarifier over the weir. Solids get collected at the bottom and sludge
must be periodically removed, dewatered and disposed.

CHEMICAL TREATMENT PROCESSES


Chemical treatment may be used at any stage in the treatment process as and when
required. Mainly used methods are-

Neutralization- This process is used to adjust pH of the waste water to optimise


treatment efficiency. Untreated wastewater has a wide range of pH values and may
require neutralization to eliminate either high or low values prior to certain treatment.
Acids such as sulphuric or hydrochloric may be added to reduce pH or alkalis such as
sodium hydroxide may be added to raise pH values. Neutralization may take place in a
holding, rapid mix or an equalisation tank. It can be carried out mainly at the end of the
treatment system to control the pH of discharge in order to meet the standards.

Precipitation- It is carried to remove metal compounds from waste water. It is a two-


step process. In the first step precipitants are mixed with wastewater allowing the
formation of insoluble metal precipitants. Detention time depends on the wastewater
being treated, chemical used and the desired effluent quality. In the second step
precipitated metals are removed from wastewater through filtration or clarification and
the resulting sludge must be properly treated, recycled or disposed. Various chemicals
used are lime, sodium hydroxide, soda ash, sodium sulphide and ferrous sulphate.
Normally hydroxide precipitation which is effective in removing metals like antimony,
arsenic, chromium, copper, lead, mercury, nickel and zinc and sulphide precipitation
which is used in removing lead, copper, silver, cadmium etc. may be used.

SECONDARY TREATMENT

Biological treatment Processes

Biological treatment processes are used primarily for secondary treatment and use
microbial action to decompose suspended and dissolved organic wastewater. Microbes use
the organic compounds as both a source of carbon and as a source of energy. Success of
biological treatment depends on many factors such as the pH, temperature, nature of
pollutants, nutrient requirement of microbes, presence of inhibiting pollutants and the
variations in the feed stream loading.

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CONCLUSION

From the financial analysis it is clear that the capital investment required for
installing is not very high. The payback period is also not very high and the plant
gives very attractive returns.

The increase in the selling price of Ammonia is certainly considered very


challenging. Any small change in the market prices of the raw materials
consequently affects the payout period as well the rate of return. Thus we have to
constantly keep an eye on the present as well as the future market prices of the raw
materials and products.

For the adequate supply of the raw material formaldehyde, in the future we can set
up a plant of formaldehyde from methanol. And if the setup is efficiently managed
we can hopefully affect the profitability to the great extent.

As a conclusion Manufacture of Hexamine appears to be a attractive proposal.

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REFERENCES

I. Kirk & Othmer Encyclopedia of Chemical Technology (Volume 2)


II. Robert H Perry: Chemical Engineering Hand Book. (Sixth Edition)
III. Chemtech (Vol: IV) Pg 1.74
IV. M.Gopal Rao, Marshall Sitting Drydens Outlines of Chemical technology
V. Yash. Carl L Hand book of thermodynamics (Vol. 2, 4)
VI. Chemical weekly
VII. Peter & Timmerhaus- Plant Design and Economics for Chemical Engineers
VIII. B.K.Bhaskararao Text on petrochemical (2nd Edition) Pg 65
IX. www.sciencelab.com
X. www.chemicalland21.com

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