MODUL PRAKTIKUM

LABORATORIUM INSTRUKSIONAL TEKNIK KIMIA

TEKNIK POLIMERISASI
(POL)

Disusun oleh:
Hilman Prasetya Edi
Dr. IGBN Makertihartha
Dr. Melia Laniwati Gunawan
Dr. Ardiyan Harimawan

PROGRAM STUDI TEKNIK KIMIA

FAKULTAS TEKNOLOGI INDUSTRI
INSTITUT TEKNOLOGI BANDUNG
2014
Laboratorium Instruksional Teknik Kimia Teknik Polimerisasi

DAFTAR ISI

DAFTAR ISI.............................................................................................................................. 1
DAFTAR GAMBAR ................................................................................................................. 3
DAFTAR TABEL ...................................................................................................................... 4
BAB I PENDAHULUAN .......................................................................................................... 5
BAB II TUJUAN DAN SASARAN .......................................................................................... 6
II.1. Tujuan.......................................................................................................................... 6
II.2. Sasaran ........................................................................................................................ 6
BAB III RANCANGAN PERCOBAAN .................................................................................. 7
III.1. Perangkat dan Alat Ukur ............................................................................................. 7
III.2. Bahan ........................................................................................................................... 7
III.3. Skema Alat Percobaan ................................................................................................ 8
BAB IV PROSEDUR KERJA ................................................................................................... 9
IV.1. Prosedur Percobaan ................................................................................................... 10
IV.2. Tes I – Analisa Kadar Formaldehid Bebas................................................................ 11
IV.3. Tes II – pH Larutan ................................................................................................... 12
IV.4. Tes III – Penentuan Viskositas Sampel ..................................................................... 13
IV.5. Tes IV – Penentuan Kadar Resin .............................................................................. 13
IV.6. Tes V – Penentuan Densitas Sampel ......................................................................... 14
DAFTAR PUSTAKA .............................................................................................................. 14
LAMPIRAN A TABEL DATA MENTAH ............................................................................. 16
A.1. Penentuan Kinetika Reaksi........................................................................................ 16
A.2. Penentuan pH Larutan Sampel .................................................................................. 17
A.3. Penentuan Viskositas Larutan Sampel ...................................................................... 17
A.4. Penentuan Densitas Larutan Sampel ......................................................................... 17
A.5. Penentuan Kadar Resin ............................................................................................. 18
LAMPIRAN B PROSEDUR PERHITUNGAN ...................................................................... 19
B.1. Penentuan Jumlah Formadehid ................................................................................. 19
B.2. Penentuan Jumlah Urea ............................................................................................. 19
B.3. Penentuan Jumlah Katalis dan Buffer ....................................................................... 19
B.4. Penentuan Kadar Formaldehid Bebas ....................................................................... 20
B.5. Penentuan Orde dan Konstanta Laju Reaksi ............................................................. 20

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B.6. Penentuan Kadar Resin ............................................................................................. 25

B.7. Penentuan Konsentrasi Resin (Cr) ............................................................................. 25
B.8. Penentuan Viskositas Resin ...................................................................................... 25
B.9. Penentuan Densitas Resin ......................................................................................... 26
B.10. Penentuan Massa Molekul Rata-Rata (MR) ............................................................ 26
LAMPIRAN C DATA SPESIFIKASI DAN LITERATUR .................................................... 27
C.1. Densitas Air pada Berbagai Temperatur ................................................................... 27
C.2. Viskositas Air pada Berbagai Temperatur ................................................................ 27
C.3. Massa Molekul Relatif .............................................................................................. 27
C.4. Densitas Zat pada Temperatur Percobaan ................................................................. 28

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DAFTAR GAMBAR

Gambar 3.1. Skema Alat Percobaan .......................................................................................... 8

Gambar 4.1. Diagram Alir Prosedur Percobaan ...................................................................... 10

Gambar 4.2. Diagram Alir Prosedur Tes I ............................................................................... 12

Gambar 4.3. Diagram Alir Prosedur Tes II.............................................................................. 12

Gambar 4.4. Diagram Alir Prosedur Tes IV ............................................................................ 13

Gambar B.1. Kurva Orde Reaksi 1 .......................................................................................... 23

Gambar B.2. Kurva Orde Reaksi 2 .......................................................................................... 23

Gambar B.3. Kurva Orde Reaksi 0 .......................................................................................... 24

Gambar B.4. Kurva Orde Reaksi 1,5 ....................................................................................... 24

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DAFTAR TABEL

Tabel A.1. Data Penentuan Kineika Reaksi ............................................................................. 16

Tabel A.2. Data pH Larutan Sampel ........................................................................................ 17
Tabel A.3. Data Viskositas Sampel ......................................................................................... 17
Tabel A.4. Data Densitas Sampel ............................................................................................ 18
Tabel A.5. Data Kadar Resin ................................................................................................... 18
Tabel B.1. Contoh Data Percobaan .......................................................................................... 22
Tabel C.1. Densitas Air ............................................................................................................ 27
Tabel C.2. Viskositas Air ......................................................................................................... 27
Tabel C.3. Massa Molekul Relatif Bahan ................................................................................ 27
Tabel C.4. Densitas Bahan ....................................................................................................... 28

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BAB I
PENDAHULUAN

Polimer sudah menjadi material yang memenuhi kebutuhan hidup sehari-hari

manusia. Polimer dapat menjadi bahan bermacam-macam alat kebutuhan manusis seperti
botol, tali, plastik, teflon, dan lainnya. Penggunaannya semakin digemari karena sifatnya
yang ringan, tahan korosi, beberapa bahan relatif tahan asam, beberapa bahan relative tahan
sampai temperatur tinggi, dan kuat. Polimer adalah senyawa yang bermassa molekul relatif
besar dan terdiri atas monomer-monomer.
Urea-formaldehid resin adalah hasil kondensasi urea dengan formaldehid. Resin jenis
ini termasuk dalam kelas resin thermosetting yang mempunyai sifat tahan terhadap asam,
basa, tidak dapat melarut dan tidak dapat meleleh. Polimer termoset dibuat dengan
menggabungkan komponen-komponen yang bersifat saling menguatkan sehingga dihasilkan
polimer dengan derajat cross link yang sangat tinggi. Karena sifat-sifat di atas, aplikasi resin
urea-formaldehid yang sangat luas sehingga industri urea-formaldehid berkembang pesat.
Contoh industri yang menggunakan industri formaldehid adalah addhesive untuk plywood,
tekstil resin finishing, laminating, coating, molding, casting, laquers, dan sebagainya.
Pembuatan resin urea-formaldehid secara garis besar dibagi menjadi tiga. Reaksi
pertama adalah reaksi metiolasi, yaitu penggabungan urea dan formaldehid membentuk
monomer-monomer yang berupa monometilol dan dimetil urea. Reaksi kedua adalah
penggabungan monomer yang terbentuk menjadi polimer yang lurus dan menghasilkan uap
air. Tahap ini disebut tahap kondensasi. Proses ketiga adalah proses curing, dimana polimer
membentuk jaringan tiga dimensi dengan bantuan pemanasan dalam oven.
Pada praktikum ini akan dipelajari pengaruh beban rasio urea-formaldehid pada
pembentukan resin. Untuk itu digunakan variasi perbandingaan formaldehid dan urea (F/U).
Untuk mempelajari kinetika reaksi, sebelum proses curing larutan resin urea formaldehid
dideteksi konsentrasi jumlah formaldehid yang bebas.

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BAB II
TUJUAN DAN SASARAN

II.1. Tujuan

Tujuan pelaksanaan praktikum modul teknik polimerisasi adalah:

1. Praktikan mempelajari salah satu teknik polimerisasi, khususnya polimerisasi
kondensasi Urea-Formaldehid.
2. Praktikan mempelajari reaksi polimerisasi tersebut.
3. Praktikan mempelajari pengaruh-pengaruh kondisi operasi terhadap hasil reaksi
polimerisasi.

II.2. Sasaran

Sesuai tujuan di atas, hasil percobaan polimerisasi urea-formaldehid ini diharapkan

berupa:
1. Mekanisme reaksi polimerisasi kondensasi dan persamaan reaksinya.
2. Parameter-parameter persamaan reaksi polimerisasi.
3. Penggunaan persamaan Huggins untuk menentukan berat molekul polimer.

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BAB III
RANCANGAN PERCOBAAN

III.1. Perangkat dan Alat Ukur

Perangkat dan alat ukur yang akan digunakan untuk percobaan teknik polimerisasi
adalah:
1. Set perangkat modul teknik polimerisasi yang terdiri atas labu berdasar bundar
dimana reaksi dilangsungkan, yang dilengkapi dengan pengaduk yang digerakkan
oleh motor listrik, thermometer untuk mengamati suhu reaksi, refluks kondensor, dan
alat pengambil sampel.
2. Viscometer
3. Waterbath
4. Erlenmeyer
5. Piknometer
6. Labu volumetrik
7. Perangkat titrasi
8. Timbangan/ neraca
9. Oven
10. Cawan perselen

III.2. Bahan

Bahan-bahan yang akan digunakan untuk percobaan teknik polimerisasi adalah:

1. Urea
2. Formaldehid (dalam bentuk larutan formalin)
3. Na-sulfit
4. Na-karbobat
5. Alkohol
6. Indikator Corellin
7. Asam sulfat

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III.3. Skema Alat Percobaan

Gambar 3.1. Skema Alat Percobaan

Keterangan:

1. Waterbath.
2. Reaktor.
3. Tempat pengambil sampel.
4. Termometer.
5. Motor pengaduk.
6. Impeller.
7. Kondensor.

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CHAPTER IV
WORK PROCEDURE

The work procedure on this experiment is generally explained as follow:

1. Arrange the equipment according to the drawing sketch and check the condition of the
equipment.
2. Prepare analytical equipment.
3. Prepare the chemicals needed in the reaction, and calculated the amount of chemicals
according to the conditions of the experimental variation.
4. Experiment with a condensation reaction. Extent of reaction is observed by taking
samples at a certain time while the content of free formaldehyde is tested by Test I.
The reaction is stopped if the content of free formaldehyde has passed a constant level
of formaldehyde.
5. Analysis of the results of the reaction is carried out as follows:
a. pH analysis with pH paper
b. Analysis of free formaldehyde levels with Test I
c. Analysis of resin content with Test V
d. Analysis of viscosity, and "stroke cure" with Test III and IV A., B., C.
e. Density analysis with VI test. If viscosity data is needed for each sample, Test
IV A. is required.

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IV.1. Experiment Porcedure

Start

Fill the round flask with the formalin, add

catalyst, buffer, and additional materials. Stir
them until mixed

Add 5 cc of alcohol, and then chill it

Data
about Wait the mixture to react. After that, analys it
sample 0

Add enough urea, and then stir them until mixed

Add 5 cc of alcohol, and then chill it

Data
about Wait the mixture to react. After that, analys it
sample 1

Heat the mixture to taste. The reflux will happen.

When it happen, control it carefully

Add 5 cc of alcohol, and then chill it

Data
about Wait the mixture to react. After that, analys it
sample 2

Heat the mixture in 15 minutes

Add 5 cc of alcohol, and then chill it

Figure 4.1. Experiment Procedure Flow Chart

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Data
about Wait the mixture to react. After that, analys it
sample 3

Heat the mixture in 30 minutes

Add 5 cc of alcohol, and then chill it

Data
about Wait the mixture to react. After that, analys it
sample 4

Heat the mixture in 60 minutes

Add 5 cc of alcohol, and then chill it

Data
about Wait the mixture to react. After that, analys it
sample 5

Finish

Figure 4.2. Experiment Procedure Flow Chart (2)

IV.2. Test I – Free Formaldehyde Content Test

Test I is done to analyze free formaldehyde content using sodium sulfite. The procedure flow
chart is shown in Figure 4.3.
Basic reaction: NaOH formed, equivalent to the content of free formaldehyde in solution.
H2 O + CH2 O + Na2 SO4 → HO − CH2 − SO3 Na + NaOH

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Start

Mix 1 cc sample, 5 cc alcohol, and 3

to 5 drops of corralin indicator in
erlenmeyer, then close the
erlenmeyer.

Check pH with overtitration and backtitration

Add 25 cc 2N sodium sulfite aqueous. Wait the

mixture to react in 10 minutes. Shake it.

Titrate it with standar sulfate acid. Make

duplo titration

Data Compare the titration product to blank

analysis aqueous

Finish

Figure 4.3. Flow Chart of Test Procedure I

IV.3. Test II – Aqueous pH

Test II is done to analyze the pH of the solution using pH paper. The procedure flow chart is
shown in Figure 4.4.

Start

Dip pH tester paper into sample. Analys the

Sample
change of colour, compare the colour to
pH
standard pH colour

Finish

Gambar 4.4. Diagram Alir Prosedur Tes II

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IV.4. Test III – Determination of Sample Viscosity

Test III is done to determine the viscosity of the liquid using the Ostwald viscometer at a
constant temperature. The viscometer is calibrated using water at a certain temperature to get
the K value.

IV.5. Test IV – Determination of Resin Levels

The IV test is done to determine curing time. The procedure flow chart is shown in Figure
4.5.
Start

Heat the 10 diameter porcelain

dish in 140oC in 1 hour

Empry
Chill the porcelain dish with exicator,
dish
then weigh it.
mass

Dish and
Add resin to the cooled dish, resin
then weigh them. mass 1
(G1)

Heat dish and resin in 140oC in

1,5 hours

Dish and
Chill the dish and resin with exicator, resin
then weigh it. mass 2
(G2)

Heat dish and resin in 140oC in

1,5 hours again

Dish and
Chill the dish and resin with exicator, resin
then weigh it. mass 3
(G3)

Has it been done

twice?

Finish

Gambar 4.5. Diagram Alir Prosedur Tes IV

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IV.6. Test V – Determination of Sample Density

The V test is done to determine the density of the liquid using a pycnometer. Pycnometers are
calibrated using water at a certain temperature.

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BIBLIOGRAPY

Billmeyer Jr., F.W., Textbook of Polymer Science, John Wiley and Sons, 1994, pp. 186-219
D’Alelio, G.F., Experimental Plastics and Synthetic Reisns, John Wiley and Sons, 1952, pp.
163-166
Kirk-Orthmer, Encyclopedia of Chemical Technology, 2nd Edition., Vol. 2, pp. 225-258
Other books that contain Polycondensation topics

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APPENDIX A
RAW DATA TABLE

A.1. Penentuan Kinetika Reaksi

F/U =
Formalin volume = mL
Urea mass = g
Amonia mass = g
Buffer mass = g
H2SO4 concentration = M
Sample volume = mL
o
Temperature = C

Table A.1. Measurement of reaction kinetics

t H2SO4 volume (mL) T

Sample CF
(minute) I II Average (oC)
Blanko
0
1
2
3
4
5
6
7

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A.2. PH Sample Solution Determination

Tabel A.2. Measurement of pH sample solution data

Sample Colour pH
Blanko
0
1
2
3
4
5
6
7

A.3. Determination of Sample Solution Viscosity

Time for aqua dm = second

Aqua dm specific gravity =
aqua dm viskosity (Texperiment) = cP

Table A.3. Measurement of Sample Viscosity Data

No Cr (g/100mL) t (second)
1
2
3
4
5

A.4. Determination of Sample Solution Density

Empty pycnometer mass = g

Pycnometer + aqua dm mass = g
Aqua dm density (texperiment) = g/ml
Pycnometer volume = mL
Pycnometer + resin mass = g

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Table A.4. Measurement of Sample Density Data

Sampel Aqua dm pycno + Resin Resin mass (g) Resin density

No. mass (g) (g/mL)
volume (mL) volume (mL)
1
2
3
4
5

A.5. Determination of Resin Levels

Table A.5. Resin Content Data

Empty dish Dish + wet Dish + resin Dish + resin Resin mass (g)
No. mass G2 (g) mass G3 (g)
mass G1 (g) resin mass
1
2
3
4
5
6
7

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APPENDIX B
CALCULATION PROCEDURE

B.1. Determination of the Amount of Formaldehyde

Formalin solution mass = ρ*V

formalin solution density = 1.079 g/mL
for example, V(experiment volume) = 500 mL
then → formalin solution mass = 500 mL*1,079 g/mL
formalin solution mass = 539,5 g
If formalin solution contains 36% formaldehyde,
then formaldehyde mass = 0,36*539,5 = 194,22 g

Formaldehyde mass
Mol Formaldehyde =
MR
194,22
Mol Formaldehyde = = 6,47 mol
30

B.2. Determination of Amount of Urea

For example, F/U = 1,65

Then → mol urea = F/1,65 = 6,474/1,65 = 3,924 mol
Urea mass = mol urea* MR urea = 3,924 mol*66 g/mol
Urea mass = 235,418 g

B.3. Determination of Number of Catalysts and Buffers

For example, mixture total mass =Xg
Catalyst mass 5% total mass = 0,05 X
Buffer mass 5% Catalyst mass = 0,05*0,05*X
X = (formalin + urea + katalis + buffer) mass
X = 539,5 + 235,418 + 0,05X + 0,05*0,05*X
0,9475 X = 774,918
X = 817,855 g

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NH4OH mass added = 40,89 g

NH4OH used 21%-W/W = 194,73 g
NH4OH volume added (21%-solution W/W) is:
mass 194,73
(density) solution = = 208,49 mL
0,934

Na2CO3 mass added = 2,5.10-3.X = 2,045 g

B.4. Determination of Free Formaldehyde Content

For example Cc,blanko = 0,2

Cc,titrant H2SO4 = 0,7
In that condition, Csampel = 1,5
then→ free formaldehyde concentration is:
mass CH2 O (g) 3 ∗ (Cc,titrant − Cc,blanko ) ∗ NH2 SO4
CF = =
100 mL Cc,sample
3 ∗ (0,7 − 0,2) ∗ 1
CF = ( ) = 1,05 g/100 mL
1,5

B.5. Determination Orde and Reaction Rate Constants

General equation of the reaction rate:

dCF
− = k ∗ CF n
dt
To determine the order and reaction rate constants, simply using integral method:
1. If it is assumed that the reaction is orde 1, the reaction kinetics equation is:
dCF
− = k ∗ CF1
dt
The integration of these equations is as follows:
CF t
dCF
∫ = − ∫ k ∗ dt
C0 CF 0

CF
ln = −k ∗ t
C0
ln CF = ln C0 − kt
Thus, if ln Cf vs t (time) graph is made, a linear relationship will be obtained with
the perpendicular gradient indicating the reaction rate constant.

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2. If it is assumed that the reaction is orde 2, the reaction kinetics equation is:
dCF
− = k ∗ CF 2
dt
The integration of these equations is as follows:

CF t
dCF
∫ = − ∫ k ∗ dt
C0 CF 2 0

1 1
− = −kt
C0 CF
1 1
= + kt
CF C0

Thus, if 1/Cf vs t (time) graph is made, a linear relationship will be obtained with
the perpendicular gradient indicating the reaction rate constant.

3. If it is assumed that the reaction is orde 0, the reaction kinetics equation is:
dCF
− =k
dt
The integration of these equations is as follows:

CF t
∫ dCF = − ∫ k ∗ dt
C0 0

CF − C0 = −kt
CF = C0 − kt

Thus, if Cf vs t (time) graph is made, a linear relationship will be obtained with the
perpendicular gradient indicating the reaction rate constant.

4 If it is assumed that the reaction is orde 1,5, the reaction kinetics equation is:
dCF
− = k ∗ CF1,5
dt
The integration of these equations is as follows:

CF t
dCF
∫ = − ∫ k ∗ dt
C0 CF1,5 0

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2 ∗ (CF −0,5 − C0 −0,5 ) = −kt

1
CF −0,5 = − kt + C0 −0,5
2

Dengan demikian, bila dialurkan Cf terhadap t (waktu) akan diperoleh hubungan

linier dengan gradien garis –0,5.k. Konstanta laju reaksi adalah 2 kali gradien.

Berikut contoh data percobaan:

Tabel B.1. Contoh Data Percobaan

t V H2SO4 (mL) T CF^

Sampel CF ln CF 1/ CF
(menit) I II Rata-rata (oC) -0,5
Blanko 0,2 0,2 0,2 26
0 0 2,8 3,0 2,9 26 8,1 2,092 0,124 0,351
1 15 1,4 1,2 1,3 70 3,3 1,194 0,303 0,551
2 45 0,9 1,1 1 70 2,4 0,876 0,417 0,646
3 60 0,7 0,8 0,75 70 1,65 0,501 0,607 0,779
4 75 0,7 0,7 0,7 70 1,5 0,406 0,667 0,817
5 90 0,65 0,8 0,725 70 1,575 0,454 0,635 0,797
6 120 0,7 0,75 0,725 70 1,575 0,454 0,635 0,797
7 140 0,75 0,7 0,725 70 1,575 0,454 0,635 0,797

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Jika persamaan kinetika laju reaksi tersebut diasumsikan mengikuti orde 1:

Gambar B.1. Kurva Orde Reaksi 1

Jika persamaan kinetika laju reaksi tersebut diasumsikan mengikuti orde 2:

Gambar B.2. Kurva Orde Reaksi 2

Jika persamaan kinetika laju reaksi tersebut diasumsikan mengikuti orde 0:

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Gambar B.3. Kurva Orde Reaksi 0

Jika persamaan kinetika laju reaksi tersebut diasumsikan mengikuti orde 1,5:

Gambar B.4. Kurva Orde Reaksi 1,5

Dari kempat pendekatan/tebakan orde reaksi tersebut, yang paling mendekati kurva
linear adalah jika persamaan kinetika reaksi tersebut dimodelkan sebagai persamaan
aju reaksi orde 2 (R2 paling mendekati 1 yaitu 0,727).

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Dan konstanta laju reaksi persamaan kinetika tersebut adalah 0,035. Maka secara
umum persamaan kinetika reaksi polimerisasi urea formaldehid sesuai rangkaian data
tersebut adalah:

dCF
− = 0,0035CF 2
dt

B.6. Penentuan Kadar Resin

Persamaan yang digunakan adalah:

G3 − G1
%Kadar Resin = × 100%
Massa sampel resin

B.7. Penentuan Konsentrasi Resin (Cr)

Persamaan yang digunakan adalah:

CR = ρResin × Kadar Resin × V Sampel

B.8. Penentuan Viskositas Resin

Persamaan yang digunakan adalah:

μaqua dm Qsampel
μdinamik = × × t sampel
t aqua dm SGaqua dm

μdinamik
μspesifik = −1
t aqua dm (T)
μspesifik
= μintrinsik + k(μintrinsik )2 × CR
CR

SG adalah specific gravity. Dengan mengalurkan grafik μspesifik/CR terhadap CR, akan
diperoleh garis yang menunjukkan fungsi linear dengan slope μintrinsik.

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B.9. Penentuan Densitas Resin

Persamaan yang digunakan adalah:

G3 − G1
%Resin = × 100%
Berat Resin Sampel

B.10. Penentuan Massa Molekul Rata-Rata (MR)

Persamaan yang digunakan adalah:

μintrinsik = k × (MR)a

Nilai k didapat dari penyelesaian grafik μspesifik/CR terhadap CR. Gradien garis tersebut
adalah k. μintrinsik2. Jika μintrinsik dan k diketahui, maka MR polimer dapat dihitung.

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APPENDIX C
SPECIFICATION AND LITERATURE DATA

C.1. Water Density at Various Temperatures

Table C.1. Water density

Temperature (oC) ρ (g/mL)

25
26
27
28

C.2. Water Viscosity at Various Temperatures

Tabel C.2. Water viscosity

Temperature (oC) µ (cP)

25
26
27
28

C.3. Relative Molecular Mass

Table C.3. Relative Molecular Mass of Materials

Materials Molecular Formula MR

Urea CO(NH2)2 60
Formaldehid CH2O 30
Amoniak NH4OH 35
Natrium Karbonat Na2CO3 106
Natrium Sulfit Na2SO3 126

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C.4. Substance Density at Experimental Temperature

Table C.4. Material Density

Materials Molecular Formula ρ (g/mL)

Urea CO(NH2)2
Formaldehid CH2O
Amoniak NH4OH
Natrium Karbonat Na2CO3
Natrium Sulfit Na2SO3

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