Black,
Development
of
Dehydration
with
Glycols
The first glycol type dehydrators for natural gas were custom designed and nonportable units with fairly elaborate reboiling and refluxing equipment. Most units were designed in a manner similar to the ambient-temperature lean oil gasoline plants in use in about 1945. Diethylene glycol was generally used although some used ethylene glycol. Most units were limited t o dew p o i n t depressions o f a b o u t 40OF - 5 0 O F . Until about 1947-1948, when triethylene glycol (TEG) u n i t s were introduced on the market, dry desiccant dehydration was necessary w h e n dew p o i n t depressions greater t h a n a b o u t 50OF w e r e r e q u i r e d . Continued progress w i t h TEG u n i t s now a l l o w s dew p o i n t depressions as great a s 160OF f o r f i e l d units. The pattern of progress has been about as indicated in Table I below. The spread of temperatures listed indicates the effect of contact temperatures in the range of 70F to 160OF. Pressure has no measurable effect except as it affects the amount of water to be removed. TABLE I
YEAR 1947 1948 1950 1953 1957 1958 1959 1964 1966
Residual water contents a s l o w a s 0 . 1 5 l b . p e r MMSCF a n d w a t e r dew p o i n t s as low as -57F have been attained w i t h TEG i n f i e l d units. At the same time there has been little increase in glycol dehydration cost due to refinements that have allowed increased capacity and decreased utility costs. The most significant development i n TEG d e h y d r a t i o n began in 1946. At that time, Professor Laurance S. R e i d , U n i v e r s i t y of Oklahoma, began work on samples of triethylene glycol with strong support f r o m Mr. L e s P o l d e r m a n of Union Carbide Chemicals Company
H-2 During the next five or six years considerable effort was devoted to taking laboratory data for the system triethylene glycol-waternatural gas. Professor Reid directed several graduate students in numerous investigations, some of which were sponsored by fellowships. Professor R e i d a n d J . A. P o r t e r reported some of the early findings in 1949 (5) Professor Reid and.Prolessor Mark Townsend made additional reports i n 1 9 5 1 a n d 1 9 5 3 ~6, 7 , 8 ) . Major emphasis was placed on the use of triethylene glycol in 1948 and 1949 with the introduction on the market of greatly simplified and packaged wellhead glycol dehydration units. One of the first formal reoorts of such installations was that o f Mr. L . H. Peahl in 1959 (3) Figure 1 is a picture of one of the 1949 model units discussed b y Mr. P e a h l . Further progress with glycol dehydration units was slow until 1957 when both Black, Sivalls and Bryson, Inc. and Parkersburg developed the stripping gas method of super-reconcentration of glycols. Further progress was delayed until more accurate equilibrium data were developed. Design Variables
Until a b o u t 1 9 5 7 , glycol d e h y d r a t i o n was considered in terms of 65OF dew p o i n t depressions, 3 gallons/pound water circulation, and a 4-tray contactor tower. Today specific units are designed f o r dew point depressions f r o m 40OF t o 1 6 0 F , f o r g l y c o l circulation rates of from 1 gal./lb, of water to as much as 8 gal./lb, of water and for trays from 2 to as many as 16. Even more trays will be used in special cases in the future. Table encountered II below in 1950 indicates the and in 1967. usual range of design variables
TABLE II
USUAL R A N G E OF DESIGN VARIABLES
Year Number trays Dew p o i n t depression - OF Reboiler temperatures - OF Glycol rates - gal./lb, water Contact temperatures - OF Glycol concentrations - % Pressure - psig
1950 4 40 3 50 96 I00 98 350 60 1967 2 40 375 i 40 99 12 140 400 8 160 99.98
500
1200
25 -
2500
Initially, regeneration techniques provided for lean glycol solutions o f 95% t o 96% g l y c o l . In reality, concentrations as high as about 98.5% were probably initially attained but existing analytical and field sampling techniques did not allow detection of this fact until about 1953. The development of more sophiticated regeneration techniques and m o r e a c c u r a t e analytical methods have allowed regeneration of triethylene glycol up to as high as 99.98% glycol
H-3 C o n s i s t e n t r e g e n e r a t i o n to c o n c e n t r a t i o n s has been a t t a i n e d in field units from s t a n d a r d tration r e g e n e r a t o r s . as high as 9 9 . 9 8 % T E G d e s i g n e d high concen-
A brief visual c o m p a r i s o n of the first T E G d e h y d r a t o r s with those f a b r i c a t e d today will not indicate a great change For instance, compare Figure 2, a picture of a recent s i m i l a r sized unit~ w i t h that of Figure I. C o m p a r i s o n s of the process f l o w diagrams for the two units w o u l d also indicate little change. In spite o:f the small outward a p p e a r a n c e changes, d e h y d r a t o r p e r f o r m a n c e s have been g r e a t l y improved. For example, $ 9 ~ s i d e r F i g u r e 3. The curve i n d i c a t e d was first p u b l i s h e d in 1952 x~'. At that time the curve indicated the m a x i m u m a b s o r b e r c o n t a c t t e m p e r a t u r e at w h i c h 7 lb. per M M S C F w a t e r c o n t e n t could be a t t a i n e d at various a b s o r b e r pressures. The basis for the curve was a 65F w a t e r dew point depression, the g r e a t e s t that could be relied upon at that time. Today the same curve almost e x a c t l y r e p r e s e n t s the m a x i m u m a b s o r b e r c o n t a c t t e m p e r a t u r e at w h i c h 1/4 Ibo per MMSCF w a t e r content can be obtained. Improved Data for System Gas-Water-TEG
An i m p o r t a n t step in the r e f i n e m e n t of glycol d e h y d r a t o r performance has been in more a c c u r a t e l y e s t a b l i s h i n g e q u i l i b r i u m water dew points in the T E G - W A T E R - G A S sMstem. Figure 4 i n d i c a t e s two sets of data for the s y s t e m in 1966 for one c o n t a c t temperature. It is s i g n i f i c a n t to note that n o t h i n g has c h a n g e d r e g a r d i n g the true e q u i l i b r i u m b e t w e e n w a t e r and TEG. The only thing that has c h a n g e d has been the a c c u r a c y of our k n o w l e d g e of the system. Curve number B of Figure 4 r e p r e s e n t s p r e d i c t e d p e r f o r m ~ e based on e x p e r i m e n t a l d a t ~ _ ~ a k e n by P r o f e s s o r Mark T o w n s e n d <oj and by Wiser Puck and F a i l e y <~). S c a u z i l l o ~2) u t i l i z e d a c t i v i t y c o e f f i c i e n t s from data taken by T o w n s e n d and Wise to predict the e q u i l i b r i u m i n d i c a t e d on Curve B. Curve number A of Figure 4 r e p r e s e n t s p r e d i c t e d p e r f o r m a n c e based on the e x t r a p o l a t i o n to infinite number of trays and to infinite glycol rates of actual data taken from field size glycol units. This curve r e p r e s e n t s r e f i n e m e n t of the s u g g e s t e d e q u i l i b r i u m curve r e p o r t e d by L o o m e r and Welch (i) in 1961. All of the data r e p r e s e n t e d by Figure 4 are for 100F c o n t a c t t e m p e r a t u r e only. Figure 5 re~resents the equilibrium for temperature ranges from 30F to 170UF. As i n t h e c a s e f o r c u r v e A of Figure 4, the values were developed from actual dehydration unit performance data~ Although some data was taken at widely varying temperatures and glycol concentrations, most data was collected in the glycol concentration range f r o m 99% TEG t o 9 9 9 8 % TEG a n d a t t e m p e r a t u r e s varying from 60F to 140F. How New D a t a Figure Was D e v e l o p e d 6 is a flow diagram of test equipment used for a very
H-4 exhaustive s t u d y o f dew glycol. The tests were test facilities included of gas at pressures up drop in the closed gas w i t h u p t o 20 c o n t a c t o r tions. point depressions obtainable with triethylene conducted with full-scale size equipment. The provisions for circulating u p t o l 0 MMSCF/D to 1,000 psi with as much as 100 psi pressure system. Additional studies are in progress trays and at a wide range of operating condi-
Referring to Figure 6 the test gas leaves the recirculation compressor, passes through a heater where it is preheated, and then is contacted with water in a multi-tray vessel. The water enters the saturation vessel a t 180OF o r h i g h e r . The preheated gas and water provides for the heat of vaporization for the water that is vaporized into the dry-gas stream. The wet, hot gas stream then is cooled down to the planned operating temperature. Care is taken to make sure that water continuously accumulates in the separator just ahead of the dehydration contactor in order to assure saturation of the inlet g a s s t r e a m . Glycol, having consistent concentrations i n t h e r a n g e f r o m 98 to 99.98 per cent, was obtained from the regeneration system. The desiccant was circulated over varying numbers of trays in the contacting tower. W a t e r dew p o i n t s were taken between trays and downs t r e a m f r o m the unit w i t h both an e l e c t r i c a l dew point a n a l y z e r and the U. S. B u r e a u of M i n e s dew point tester. It of that data was high as typical is s i g n i f i c a n t to note that the g l y c o l u t i l i z e d w a s t y p i c a l in field use r a t h e r than new, clean glycol. Some of the taken with glycol that had been exposed to temperatures as 450OF for extended periods of time in order to reproduce field conditions.
O v e r 1 , 0 0 0 dew p o i n t s were taken in the initial series of runs. Glycol concentrations were varied f r o m 98 t o 9 9 . 9 7 p e r c e n t . Pressures were varied from 200 to 900 psi. Temperatures were varied from 600 to 130OF. Glycol circulation rates were varied from 1 gal. t o 15 g a l s . of glycol/lb, of water in the inlet gas stream. T h e dew p o i n t data were plotted and correlated so that the effects of glycol concentrations, glycol circulation rates, contact temperatures, contact pressures and number of contact trays could be predicted. Small refinements have been effected as a result of careful studies made on field operating units during the past 8 years. All glycol samples, whether from field units or from the laboratory field size unit, are analyzed for water content by the Karl Fischer titration method. Comparison of many duplicate samples indicates reproducibility as follows: TEG G l y c o l Concentration Range 100.00% 99.95% 99.50% 99.00% Difference Between Duplicates
H-5
New R e g e n e r a t i o n
Method
The most e f f e c t i v e r e f i n e m e n t in the p e r f o r m a n c e of t r i e t h y l e n e glycol d e h y d r a t i o n units has been in the method of r e g e n e r a t i o n as indicated in U. S. Patent No. 3 , 1 0 5 , 7 4 8 and C a n a d i a n Patent No. 733,820. In summary, the new r e g e n e r a t i o n p r i n c i p l e i n v o l v e s the r e m o v a l of w a t e r from glycol by c o n v e n t i o n a l r e g e n e r a t i o n t e c h n i q u e s up to about 99.1% glycol and the f u r t h e r p u r i f i c a t i o n by gas stripping. The gas s t r i p p i n g t e c h n i q u e c o n s i s t s of p r e h e a t i n g a very small q u a n t i t y of natural gas and c o n t a c t i n g it countercurrently w i t h 99.1% t r i e t h y l e n e glycol as it leaves the r e b o i l e r and flows to the storage tank. The small amount of c o u n t e r c u r r e n t l y f l o w i n g n a t u r a l gas r e d u c e s the partial p r e s s u r e of w a t e r vapor in contact w i t h the p a r t i a l l y r e g e n e r a t e d glycol to a very low quantity. This f o r c e s a shaft of the e q u i l i b r i u m so that a d d i t i o n a l w a t e r vapor leaves the glycol and e n t e r s the vapor phase at e s s e n t i a l l y the same t e m p e r a t u r e r e s u l t i n g in very low r e s i d u a l w a t e r contents. This t e c h n i q u e is p a r t i c u l a r l y e f f e c t i v e w h e n a c c o m p l i s h e d w i t h c o u n t e r c u r r e n t contacting techniques. Figure 7 represents the expected glycol concentrations under various conditions of regeneration. As n o t e d , a 400F reboiler temperature at 1200 feet elevation will result i n a b o u t 9 9 . 1 % TEG with no stripping gas being injected. The effect of installation and operation at higher elevations is to allow higher concentrations than indicated at any stripping gas rate. The glycol concentration resulting f r o m 400OF r e b o i l e r temperature and zero stripping gas at sea level i s a b o u t 9 9 . 0 % TEG. S i m i l a r c u r v e s to those i n d i c a t e d in F i g u r e 7 can be drawn for any r e g e n e r a t o r t e m p e r a t u r e or any elevation. The effect of lower r e b o i l e r t e m p e r a t u r e s is p a r a l l e l c u r v e s at somewhat lower concentrations. If s t r i p p i n g gas is injected d i r e c t l y into the r e b o i l e r the r e s u l t s are as indicated by the lower curve. The upper curve r e p r e s e n t s the glycol c o n c e n t r a t i o n r e s u l t i n g from c o u n t e r - c u r r e n t l y i n j e c t i n g s t r i p p i n g gas after the major amount of w a t e r vapor has been removed. The d r a m a t i c d i f f e r e n c e in the glycol c o n c e n t r a t i o n s produced from the two m e t h o d s r e s u l t s from two major principles. One is the p r i n c i p l e of mass t r a n s f e r by countercurrent contact of the liquid and gas p h a s e s as c o m p a r e d to a single c o c u r r e n t contact of the phases. The second p r i n c i p l e is the g r e a t e r d r i v i n g force r e s u l t i n g from i n j e c t i o n of s t r i p p i n g gas after most of the w a t e r is p r e v i o u s l y r e m o v e d by the a p p l i c a t i o n of heat. This is c o m p a r e d to the lower d r i v i n g force r e s u l t i n g from i n j e c t i o n of s t r i p p i n g gas in the same area w h e r e the bulk of the w a t e r is r e l e a s e d by boiling. The p r i n c i p l e of i n j e c t i o n of s t r i p p i n g g a s into the r e b o i l e r was a standard f e a t u r e on all Standard r e g e n e r a t o r s f u r n i s h e d in
H-6
1950 by Black, S i v a l l s & Bryson, Inc. The p r a c t i c e was d i s c o n t i n u e d in early 1951 because of lack of e v i d e n c e of e f f e c t i v e r e s u l t s that would j u s t i f y the q u a n t i t y of s t r i p p i n g gas required. The later d e v e l o p m e n t of s t a b i l i z e d Karl F i s c h e r r e a g e n t and the e l e c t r o n i c d e t e c t i o n of the a n a l y t i c a l end points allows a c c u r a t e m e a s u r e m e n t s of small changes. In addition, the d e v e l o p m e n t of e l e c t r o n i c w a t e r a n a l y z e r s for gas s t r e a m s a l l o w s a c c u r a t e d e t e c t i o n of a few d e g r e e s c h a n g e in dew points.
Super-Dehydration
Applications
E f f e c t i v e u t i l i z a t i o n of glycol d e h y d r a t i o n for dew point d e p r e s s i o n s in e x c e s s of 100OF o f f e r s new p o t e n t i a l s for savings in e q u i p m e n t costs and o p e r a t i n g costs. For example, it is now more often p r a c t i c a l than in the past to d e h y d r a t e at high p i p e l i n e f l o w i n g t e m p e r a t u r e s r a t h e r than cool the gas s t r e a m and s e p a r a t e any c o n d e n s e d liquids prior to d e h y d r a t i o n w i t h solid or liquid d e s i c c a n t s . This s i t u a t i o n has come about as the result of c a r e f u l s t u d i e s of the effect of glycol r a t e s and trays upon dew point d e p r e s s i o n s as well as from a better k n o w l e d g e of the true e q u i l i b r i u m and the a v a i l a b i l i t y of higher TEG c o n c e n t r a t i o n s . The o p t i m u m a p p l i c a t i o n of s u p e r - d e h y d r a t i o n n e c e s s i t a t e s c a r e f u l c o n s i d e r a t i o n of many variables. For example, c o n s i d e r the d e h y d r a tion of a high t e m p e r a t u r e and low p r e s s u r e gas stream. The gas will c o n t a i n several hundred pounds of w a t e r per MMSCFD. T h e r e is a need to m i n i m i z e the amount of glycol c i r c u l a t e d to r e d u c e the fuel and p u m p i n g power r e q u i r e m e n t s . E x h a u s t i v e s t u d i e s have indicated it is p r a c t i c a l to u t i l i z e as little as 1 gal. TEG/lb. of w a t e r removed in some cases. This is practical, however, only w i t h a d d i t i o n a l trays and higher TEG c o n c e n t r a t i o n s . In addition, a c c u r a t e k n o w l e d g e of the t h e r m o d y n a m i c s of the s y s t e m must be known and c o n s i d e r a t i o n s must be given to the type of gas being treated. For example, c o n s i d e r F i g u r e 8. The t e m p e r a t u r e data w e r e taken f r o m a unit w h e r e several h u n d r e d pounds of w a t e r per M M S C F D were being removed. Heat evolved by the a b s o r p t i o n of w a t e r vapor by the glycol r e s u l t e d in a c o n s i d e r a b l e i n c r e a s e in the c o n t a c t t e m p e r a t u r e .
Note
following: Gas outlet temperature temperature 17F higher than the inlet the outlet
15F
higher
than than
7OF h i g h e r
the
It is also s i g n i f i c a n t to note that the above t e m p e r a t u r e d i f f e r e n c e s " change w i t h the s p e c i f i c g r a v i t y of the gas being d e h y d r a t e d when all
H-7 other variables remain unchanged. This fact results from a change in the heat absorbing capacity of the gas due to the changed mass of gas and, to a smaller degree, the changed specific heat of the gas.
W h e n t e m p e r a t u r e b u l g e s of the t y p e i n d i c a t e d in F i g u r e 7 occur, c a r e f u l e v a l u a t i o n m u s t be m a d e of b o t h the t e m p e r a t u r e and e q u i l i b r i u m b u l g e s t h a t o c c u r w i t h i n the c o n t a c t o r tower.
In spite of the apparent complications discussed above, Figure represents an actual application where dehydration at 140OF inlet temperature to 22OF dew point was justified instead of cooling prior to dehydration. Most dehydration applications water to be removed and therefore in temperature in the contactor. have result
Perhaps, the greatest use for super-dehydration with glycols will be in the area of gas conditioning ahead of refrigerated lean oil absorption plants. In many cases glycol dehydration will apply where outlet dew points in the range of -20OF to -50OF are required. This method prevents many potential problems of glycol distribution and glycol - condensate separation that occur with glycol injection systems. Figure 9 indicates the relationship of glycol concentration changes for normal application with a larger number of trays. In general, straight lines result but they are sometimes affected when large quantities of water are removed with relatively low glycol rates.
Use of D i r e c t Fired Reboilers
Super dehydration can 400F or lower. The lower ping gas or more elaborate TEG c o n c e n t r a t i o n .
be attained at reboiler temperatures of reboiler temperatures require more stripregeneration equipment to attain the same
operation fails to
Figure I0 indicates typical flue gas and metal skin temperatures for a direct fired glycol reboiler firetube with 400OF bulk temperature. The temperatures are representative of an average flux rate of about 8,000 BTU/hr. - ft. 2. While looking at Figure l0 it is easy to visualize what effects will result by changing the length of the firetube so that the average flux rate varies from 6,000 to i0,000 BTU/hr. - ft. 2. In this manner, it is easily seen that the maximum tube wall temperature in contact with the boiling glycol solution is not changed by changing the average design flux rate.
M a x i m u m f l u x r a t e s in d i r e c t f i r e d r e b o i l e r f i r e t u b e s is a f u n c t i o n of the f o r c e d c o n v e c t i o n c o e f f i c i e n t on the i n s i d e and the m e a n b e a m l e n g t h of the r a d i a t i o n c o m p o n e n t . D i r e c t and h a r d i m p i n g e m e n t of the f l a m e a g a i n s t the f i r e t u b e s h o u l d be a v o i d e d , h o w e v e r .
H-8
By r e f e r r i n g to F i g u r e I0 and F i g u r e ii, it is easy to v i s u a l i z e that the use of high p r e s s u r e s t e a m for r e b o i l e r h e a t i n g m e d i a can result in m u c h higher skin t e m p e r a t u r e s than when u t i l i z i n g a d i r e c t fired reboiler. For example, c o n s i d e r the use of 500OF steam. The c o n d e n s i n g s t e a m heat t r a n s f e r c o e f f i c i e n t is about equal to the boiling glycol coefficient. In that event the metal skin t e m p e r a ture in c o n t a c t w i t h the b o i l i n g glycol w o u l d be about 450F. The use of h i g h velocity, h i g h t e m p e r a t u r e heat t r a n s f e r oil can also result in m e t a l skin t e m p e r a t u r e s that are in e x c e s s of those for d i r e c t fired r e b o i l e r s if not p r o p e r l y designed.
Summary Super-dehydration with glycols is an effective method of reducing capital equipment costs and operating costs in most applications w h e r e h i g h dew p o i n t d e p r e s s i o n s are required. It can be effectively applied to almost any gas, at almost any pressure and at a wide range of contact temperatures.
H-9
Bibliography . "Some Critical Aspects of Designing for High Dew Point Depression with Glycols," J. A. Loomer and J. W. Welch, Gas Conditioning Conference, University of Oklahoma, March, 1961 Scauzillo, Triethylene Technology, Frank R., "Equilibrium Ratios Glycol-Natural Gas System," July, 1961. of Water in the WaterJournal of Petroleum a Skid 13, 1 9 5 0 ,
Peahl, L. H . , " I n s t a l l a t i o n , Operation and Performance of Mounted Gas Dehydration Plant," Oil and Gas Journal, July pp. 92-96
J o h n M. C a m p b e l l a n d L a w t o n L. L a u r e n c e , "Glycol Dehydration," Part III of "Dehydration of Natural Gas and Hydrocarbon Liquids," Petroleum Refiner, V o l . 3 1 , No. 11, p p . 109 ( 1 9 5 2 ) Porter, J . A. a n d R e i d , L. S . , p r e s e n t e d San Antonio, Texas, October, 1949. Politziner, I., Townsend, F. M., and Reid, meeting A.I.M.E., Petroleum Branch (1951) at A.I.M.E. L. S., St. meeting, Louis
5. 6. 7.
.
Townsend, F. M. "Vapor-Liquid Equilibrium Data for DEG and TEGWater-Natural Gas System," Gas Conditioning Conference, May, 1953. T o w n s e n d , F . M., " E q u i l i b r i u m Water Contents of Natural Gas Dehydrated by Aqueous Diethylene and Triethylene Glycol Solutions at Various Temperatures and Pressures," Ph.D. dissertation, The University of Oklahoma (1955) Wise, H . , Chemistry,
U. S.
9.
Puck, T. T. and Failey, C. F., Journal of Physical (1950) 54, 734 No. 3,105,748 No. 733,820 assigned assigned to Black, to Black, Sivalls Sivalls & Bryson, & Bryson,
i0.
Patent
Inc.
ll.
Canadian Inc.
Patent
Fig.
High
Concentration Dehydrator
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140 144 148 152 156 I ~ 164 168 IT~ TEMPERATURE- F FIG, 8 GAS AND GLYCOL TEMPERATURE I:~ORLES FOR FIE~WY WATER LOAOS.
124 128
132
136
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407 F
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FIG. I0
TYPICAL DIRECT FIRED GLYCOL REBOILER TEMPERATURE PROFILES OF FLUE GAS AND FIRE TUBE.
~ L O W RESISTANT BOILING
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Q ~
.rTH,s ~RF,C E ,N C O N T A C T
I WITH BOILIN6 GLYCOL SECTION OF FIRE T U B E WALL
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_/-
~
, ,, 4 4 5 " F METAL KIN TEMP GAS 51DE
ULK TEMP. = 4 0 0 F .... I AT ,AT ~T GLYCOL = 3 0 F METAL = #5F FLUE GAS = 2155F
-"---POINT
FLUE
FIG. If