CN101723919A - Method for removing carbon dioxide aqueous solution by ethylene oxide/ethylene glycol synthesized recycle gas - Google Patents

Method for removing carbon dioxide aqueous solution by ethylene oxide/ethylene glycol synthesized recycle gas Download PDF

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Publication number
CN101723919A
CN101723919A CN200810196779A CN200810196779A CN101723919A CN 101723919 A CN101723919 A CN 101723919A CN 200810196779 A CN200810196779 A CN 200810196779A CN 200810196779 A CN200810196779 A CN 200810196779A CN 101723919 A CN101723919 A CN 101723919A
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pressure
solution
acid
gas
steam
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王祥云
储政
朱道平
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Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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Research Institute of Nanjing Chemical Industry Group Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Abstract

The invention belongs to the technical field of gas purification technology. Adopting novel high selectivity catalyst in response to synthesis of ethylene oxide and ethylene glycol needs to reduce CO2 content in recycled gas, as a result, the method of adopting decarburized aqueous solution is proposed. The aqueous solution is composed of potassium carbonate and activating agent; the two-section absorption technology suitable for flow distribution and temperature control is adopted; a new voltage transformation regeneration energy saving technology for carrying out adsorption stripping on the solution is adopted; the chimney effect of a tunable supersonic speed steam injector on a constant pressure regenerating column is employed to form differential pressure between a pressurizing regenerating column and the constant pressure regenerating column; mixed gas containing a large quantity of water vapor is pumped and sucked for gas stripping and regeneration of the pressurizing regenerating column. With the method of the invention adopted, the remaining CO2 in the decarburized recycle gas can be reduced by big margins; meanwhile solution regeneration heat loss is reduced by more than 30% compared with the solution regeneration heat loss in the normal potassium carbonate decarburization process.

Description

The ethylene oxide/ethylene glycol synthetic cyclic gas removes the aqueous solution and the method for carbonic acid gas
Technical field: the invention belongs to the gas purification technique field, be specifically related to a kind ofly from the ethylene oxide/ethylene glycol synthetic cyclic gas that contains a large amount of hydro carbons and a certain amount of oxygen, remove CO 2The aqueous solution and method.
Background technology: adopt high-purity ethylene and purity oxygen oxidation to generate oxyethane (EO), oxyethane makes high purity ethylene glycol (EG) product through water absorption, desorb, absorption, evaporation concentration rectifying again.Generate a certain amount of CO of generation in the oxyethane process at oxidation of ethylene 2, it must be removed from synthetic cyclic gas, could keep catalyzed reaction efficient.
Along with the Application and Development of novel high-selectivity oxidation catalyzer makes the ethene utilization ratio improve constantly, require CO in the circulation gas simultaneously 2Concentration is lower, is reduced to 2mol% from original 5mol%, even requires to be lower than 1mol%.Under the solvent of original circulation gas decarburization and processing condition, transform, main way strengthens circulation gas exactly and goes the unitary shunting ratio of decarburization, promptly increase the circulating flow rate enter the decarburization absorption tower, existing absorption tower and column internals thereof be difficult to by, circulation gas decarburization unit must be transformed like this.
Because CO in the carbon rejection process in the ethylene oxide/ethylene glycol synthetic cyclic gas 2Dividing potential drop is lower all the time, promptly is in the lean solution state of cycle operation, therefore, and the CO in the solution 2Desorb is difficulty more, adopts existing single tower reclaiming process, the every standard cubic meter CO of desorb from absorb rich solution 2Hear rate reach 9000～15000kJ/Nm 3CO 2Reduce CO in the absorption tower outlet purified gas 2Residual quantity satisfies the operational conditions of new catalyst, and another way will make that lean solution regeneration is more thorough, also just needs to consume more steam.
Because decarbonizing solution is in the lean solution state of cycle operation, it is the power-saving technology that power removes to aspirate the double tower pressure swing regeneration of normal pressure regenerator column mode that the patent that can not adopt us to develop: ZL98100929.8 presses resurgent gases with the band of pressurization regenerator column, needs the new pressure variable regeration tech flow process of exploitation to realize energy-conservation.
In view of the gas composition of ethylene oxide/ethylene glycol synthetic cyclic gas, in order to reduce the loss of hydro carbons, existing apparatus adopts the salt of wormwood decarbonization process usually, and selects for use vanadate and borate as activator.Along with residual CO in the gas after the decarburization 2Index reduce, the composition of salt of wormwood and activator and concentration proportioning also need to adjust.
Therefore, at the CO that reduces in the ethylene oxide/ethylene glycol synthetic cyclic gas 2Concentration needs to set about from many-sides such as technology, equipment, solvents simultaneously, the novel solvent and the method for the decarburization of exploitation salt of wormwood.
Summary of the invention: the objective of the invention is to reduce CO in the circulation gas at the novel high-selectivity catalyst of ethylene oxide/ethylene glycol 2Residual quantity, and the aqueous formulation and the Technology that propose are characterized in:
(1) outside the composition of the aqueous solution dewaters, also comprise salt of wormwood and inorganic activator, inorganic activator is potassium metavanadate and boric acid, it perhaps is one or more the mixture in potassium metavanadate and boric acid and selenous acid, metaantimmonic acid, the telluric acid, according to different technology, appointed condition and index request, its proportioning can have more significantly variation.
Salt of wormwood weight concentration 10～40% (preferred 15～35%); Inorganic activator total concentration by weight 1～50%.
Potassium metavanadate KVO in the inorganic activator 3Weight concentration 0.1～30% (preferred 0.5～25%); Activator boric acid H 3BO 3Weight concentration 1～50% (preferred 2～35%); And one or more the mixture in the selenous acid, metaantimmonic acid, telluric acid, weight concentration 0～5%.
(2) absorption tower changes existing one section absorption technique in the flow process of the present invention, adopts two sections absorptions.Lean solution is after the lean pump pressurization, separated into two parts, 60～90% (preferred 70～85%) directly enter on the second section filler in bottom, absorption tower, and other 10～40% (preferred 15～30%) enter (every section filler can be divided into 1 layer～4 layers) on the first section filler in top, absorption tower after the lean solution chiller temperature is reduced to 60～100 ℃ (preferred 70～90 ℃).Small volume of solution is reduced temperature not only can reduce liquid phase CO 2Dividing potential drop reduces the absorption tower and goes out CO in the tower purified gas 2Content; Can also reduce purified gas heat exchange refrigerative thermal load; Change the scheme that whole lean solutions are lowered the temperature into than original one section absorption, the heat of cooling loss reduces 60～80%.
(3) solution stripping changes existing single tower reclaiming process in the flow process of the present invention, adopt double tower pressure swing regeneration power-saving technology newly developed, after the absorption rich solution decompression of coming out at the bottom of the absorption tower, enter the carbonate solution flash tank, carbonate solution after the flash distillation enters pressurization regenerator column top, utilize the open steam heat air to carry and make solution stripping regeneration, and solution further boils regeneration in the reboiler at the bottom of the tower.The tower top pressure of pressurization regenerator column is brought up to 0.04～0.14MPa (table) (preferred 0.06～0.12MPa (table)), and it is stable to keep-up pressure by regulating loop.Because the carbonate solution boiling point was brought up to 115～124 ℃ (preferred 118～122 ℃) at the bottom of pressure improved tower, made solution stripping go out CO 2More, residual CO in the lean solution 2Still less, just can realize that reducing the absorption tower goes out CO in the tower purified gas 2The target of content; Because pressure improves, water vapor and CO in the resurgent gases that the pressurization regeneration overhead is come out 2Ratio from 3～4: 1 reduces to 1.2～2: 1, make the steam vapour amount of taking out of by resurgent gases reduce 40～60%, can realize the target that solution regeneration hear rate reduces significantly simultaneously.
(4) solution that has certain pressure and comparatively high temps that comes out from pressurization regenerator column bottom in the flow process of the present invention is sent into normal pressure regenerator column middle part through relay pump, utilize power steam by the suction function of adjustable supersonic injectors to the normal pressure regenerator column, solution is further regenerated, and from this tower lean solution, release and contain the gas mixture of a large amount of water vapors, send into pressurization regenerator column bottom as open steam, thereby reduce the open steam consumption.
(5) the used power steam pressure of adjustable supersonic speed steam injector is 0.04～0.16Mpa (table) (preferred 0.06～0.12MPa (table)) in the flow process of the present invention, temperature is 141～200 ℃ (being preferably 158～187 ℃), and the power steam consumption is determined according to unit scale and technology; The steam of releasing from the normal pressure regenerator column and the weight ratio of power steam have been saved about 50% jet vapor consumption 0.8～1.4 (being preferably 0.9～1.2).
(6) adopt new double tower pressure swing regeneration power-saving technology in the flow process of the present invention, by adjustable supersonic speed steam injector the suction function of normal pressure regenerator column is made between pressurization regenerator column and two towers of normal pressure regenerator column and to form pressure reduction, the regeneration overhead of wherein pressurizeing pressure-controlling is at 0.05～0.14MPa (table) (preferred 0.06～0.12MPa (table)), normal pressure regeneration overhead pressure-controlling is at 0.01～0.09Mpa (table) (preferred 0.02～0.08Mpa (table)), makes that the solution boiling point produces 8～20 ℃ the temperature difference (being generally 10～16 ℃) at the bottom of two towers.Increased the solution stripping impellent, saved jet vapor consumption, because the lean solution temperature after the flash distillation reduces about 10 ℃, also reduced the calorific loss of lean solution cooling in the lean solution water cooler.
Adopt the present invention when the ethylene oxide/ethylene glycol synthetic cyclic gas removes carbonic acid gas, not only reduce CO in the absorption tower outlet purified gas 2Residual quantity satisfies the operational conditions of new catalyst; And can make solution regeneration hear rate reduce more than 30%.
Description of drawings: accompanying drawing is an embodiment of the invention process flow diagram.
In the accompanying drawing 1, the 1-absorption tower; 2-normal pressure regenerator column; The 3-regenerator column that pressurizes; 4-carbonate solution flash tank; The 5-feed preheater; 6-lean solution water cooler; The 7-gas heat exchanger; 8-purified gas water cooler; 9-resurgent gases water cooler; 10-adjustable steam injector; The 11-purge gas separator; 12-resurgent gases separator; 13-solution relay pump; The 14-solution circulation pump; The 15-solution reboiler.
Embodiment: the present invention is described in detail below in conjunction with drawings and Examples.
As accompanying drawing 1, the gas that goes out the ethylene oxide/ethylene glycol synthetic tower enters the decarburization unit through recycle compressor and wherein shunts a part of circulation gas after heating with feed preheater (5), enter the bottom of absorption tower (1), hot and cold lean solution counter current contact under Ta Nei and top of tower, middle part removes carbonic acid gas, CO2 content drops to below the index in the outlet purified gas, through interchanger (7), and water cooler (8), after separator (11) was back and the circulation gas of decarburization does not converge, bout became the unit.
After the absorption rich solution decompression of coming out at the bottom of the absorption tower, enter carbonate solution flash tank (4), flash off gas containing hydrocarbon and send next unit.Carbonate solution after the flash distillation enters pressurization regenerator column (3) top, utilize the open steam heat air to carry and make solution stripping regeneration, and solution further boils desorb in the reboiler at the bottom of the tower (15).The tower top pressure of pressurization regenerator column (3) keep-ups pressure stable by regulating loop, because the raising of pressure, also by a relatively large margin the raising of carbonate solution boiling point makes solution stripping go out CO at the bottom of the tower 2More, residual CO in the lean solution 2Still less, just can realize that reduction goes out CO the tower purified gas from the absorption tower 2The target of content.
The solution that has certain pressure and comparatively high temps that comes out from pressurization regenerator column (3) bottom is sent into normal pressure regenerator column (2) middle part through newly-increased relay pump (13), utilize adjustable steam injector (10) solution further to be regenerated, and extract a large amount of steam out the suction function of normal pressure regenerator column (2).Enter pressurization regenerator column (3) bottom by adjustable supersonic speed steam injector (10) gas mixture that contains a large amount of steam of releasing as open steam as power by the steam of certain pressure, propose regeneration for solution gas, thereby reduce pressurization regenerator column open steam consumption significantly.
The lean solution of coming out at the bottom of the normal pressure regenerator column, after solution circulation pump (14) pressurization, separated into two parts, major part directly enters absorption tower second layer filler, and small portion enters the top, absorption tower after lean solution water cooler (6) temperature is reduced to design load.Small volume of solution reduction temperature not only can further reduce the absorption tower and go out CO in the tower purified gas 2Content; Reduced purified gas heat exchange refrigerative thermal load; Also reduced the heat that the solution cooling consumes.
Behind the resurgent gases process feed preheater (5) that comes out in pressurization regenerator column (3) top, the water cooler (9), by sending behind separator (12) the separating and condensing water, water of condensation is then sent to Waste Water Treatment.
Embodiment 1
An ethylene oxide/ethylene glycol synthesis cycle gas decarbonization unit adopts concentration of potassium carbonate 15 (m) %, activator potassium metavanadate KVO 3Concentration 5 (m) %, activator boric acid H 3BO 3Concentration 20 (m) %, activator selenous acid 2 (m) %; Two sections absorptions are taked on the absorption tower, and the hot and cold lean solution counter current contact of coming in circulation gas that enters at the bottom of the tower and top of tower, middle part removes carbonic acid gas, absorb at the bottom of 70 ℃ of the temperature cats head, tower of operation 105 ℃, pressure 2.2Mpa (table), and circulation gas is gone into tower CO 2Content is 4mol%, goes out the residual CO in absorption tower 2＜0.9mol% satisfies ethylene oxide/ethylene glycol synthetic cyclic gas CO 2The requirement of＜1.0mol%.Adopt new double tower pressure swing regeneration, pressurization regeneration overhead pressure is that 0.08MPa (table) keeps stable by pressure regulation circuit, the carbonate solution boiling point is brought up to about 120 ℃ at the bottom of the tower, the steam that adopts 1.0MPa (table) pressure is as power, make normal pressure regeneration overhead pressure-controlling at 0.03Mpa (table) by the adjustable steam injector, make that the solution boiling point produces 10 ℃ the temperature difference at the bottom of two towers, the steam of releasing from the normal pressure regenerator column and the weight ratio of power steam are 1.0, saved 50% jet vapor consumption thus, solution regeneration hear rate reduces more than 30%.
Embodiment 2
An ethylene oxide/ethylene glycol synthesis cycle gas decarbonization unit adopts concentration of potassium carbonate 20 (m) %, activator potassium metavanadate KVO 3Concentration 1 (m) %, activator boric acid H 3BO 3Concentration 4 (m) %; Two sections absorptions are taked on absorption tower (2.1 meters of diameters), the hot and cold lean solution counter current contact of coming in the 3886Kmol/h circulation gas that enters at the bottom of the tower and top of tower, middle part removes carbonic acid gas, absorb at the bottom of 80 ℃ of the temperature cats head, tower of operation 109 ℃, pressure 1.8Mpa (table), circulation gas is gone into tower CO 2Content is 3mol%, goes out the residual CO in absorption tower 2＜0.6mol% satisfies ethylene oxide/ethylene glycol synthetic cyclic gas CO 2The requirement of＜0.9mol%.Adopt new double tower pressure swing regeneration, pressurization regeneration overhead pressure is that 0.08MPa (table) keeps stable by pressure regulation circuit, the carbonate solution boiling point is brought up to about 120 ℃ at the bottom of the tower, the steam that adopts 0.80MPa (table) pressure is as power, make normal pressure regeneration overhead pressure-controlling at 0.03Mpa (table) by the adjustable steam injector, make that the solution boiling point produces 10 ℃ the temperature difference at the bottom of two towers, the steam of releasing from the normal pressure regenerator column and the weight ratio of power steam are 1.0, saved 50% jet vapor consumption thus, solution regeneration hear rate reduces more than 30%.
Embodiment 3
An ethylene oxide/ethylene glycol synthesis cycle gas decarbonization unit adopts concentration of potassium carbonate 30 (m) %, activator potassium metavanadate KVO 3Concentration 8 (m) %, activator boric acid H 3BO 3Concentration 30 (m) %, activator selenous acid 1 (m) %; Two sections absorptions are taked on absorption tower (2.6 meters of diameters), and 7350Kmol/h circulation gas that enters at the bottom of the tower and hot and cold lean solution counter current contact remove carbonic acid gas, absorb at the bottom of 70 ℃ of the temperature cats head, tower of operation 110 ℃, pressure 1.8Mpa (table), and circulation gas is gone into tower CO 2Content is 2.36mol%, goes out the residual CO2＜0.35mol% in absorption tower, satisfies ethylene oxide/ethylene glycol synthetic cyclic gas CO 2The requirement of＜0.4mol%.Adopt new double tower pressure swing regeneration, pressurization regeneration overhead pressure is 0.09MPa (table), the carbonate solution boiling point is brought up to about 125 ℃ at the bottom of the tower, the steam that adopts 1.0MPa (table) pressure is as power, make normal pressure regeneration overhead pressure-controlling at 0.04Mpa (table) by the adjustable steam injector, make that the solution boiling point produces 11 ℃ the temperature difference at the bottom of two towers, the steam of releasing from the normal pressure regenerator column and the weight ratio of power steam are 1.0, saved 50% jet vapor consumption thus, the regeneration hear rate of solution reduces more than 30%.
Embodiment 4
An ethylene oxide/ethylene glycol synthesis cycle gas decarbonization unit adopts concentration of potassium carbonate 35 (m) %, activator potassium metavanadate KVO 3Concentration 9 (m) %, activator boric acid H 3BO 3Concentration 40 (m) %, activator metaantimmonic acid 1 (m) %; Two sections absorptions are taked on the absorption tower, and the hot and cold lean solution counter current contact of coming in circulation gas that enters at the bottom of the tower and top of tower, middle part removes carbonic acid gas, absorb at the bottom of 80 ℃ of the temperature cats head, tower of operation 110 ℃, pressure 2.4Mpa (table), and circulation gas is gone into tower CO 2Content is 3.6mol%, goes out the residual CO in absorption tower 2＜0.6mol% satisfies ethylene oxide/ethylene glycol synthetic cyclic gas CO 2The requirement of＜0.9mol%.Adopt new double tower pressure swing regeneration, pressurization regeneration overhead pressure is that 0.08MPa (table) keeps stable by pressure regulation circuit, the carbonate solution boiling point is brought up to about 122 ℃ at the bottom of the tower, the steam that adopts 1.0MPa (table) pressure is as power, make normal pressure regeneration overhead pressure-controlling at 0.03Mpa (table) by the adjustable steam injector, make that the solution boiling point produces 12 ℃ the temperature difference at the bottom of two towers, the steam of releasing from the normal pressure regenerator column and the weight ratio of power steam are 1.0, saved 50% jet vapor consumption thus, solution regeneration hear rate reduces more than 30%.

Claims (7)

1. an ethylene oxide/ethylene glycol synthetic cyclic gas removes the aqueous solution of carbonic acid gas, it is characterized in that solution composition dewaters outside, also comprise salt of wormwood and inorganic activator, salt of wormwood weight concentration 10～40%, inorganic activator total concentration by weight 1～50%; Inorganic activator is potassium metavanadate and boric acid, perhaps is one or more the mixture in potassium metavanadate and boric acid and selenous acid, metaantimmonic acid, the telluric acid, and wherein the potassium metavanadate weight concentration 0.1～30%, boric acid H 3BO 3Weight concentration 1～40%; The mixture of one or more in selenous acid, metaantimmonic acid, the telluric acid, weight concentration 0～5%.
2. the aqueous solution as claimed in claim 1 is characterized in that salt of wormwood weight concentration 15～35%, wherein inorganic activator potassium metavanadate KVO 3Weight concentration 0.5～25%, inorganic activator boric acid H 3BO 3Weight concentration 2～35%, the mixture of one or more in selenous acid, metaantimmonic acid, the telluric acid, weight concentration 0～5%.
3. an ethylene oxide/ethylene glycol synthetic cyclic gas removes the method for carbonic acid gas, it is characterized in that in two sections absorptions of absorption tower employing, lean solution is after the lean pump pressurization, separated into two parts, 60～90% directly enter the second section filler in bottom, absorption tower, and 10～40% enter the first section filler in top, absorption tower after the lean solution chiller temperature is reduced to 60～100 ℃; The pressure swing regeneration power-saving technology is adopted in the desorb of solution, working power steam, by the suction function of adjustable supersonic injectors to the normal pressure regenerator column, make between pressurization regenerator column and two towers of normal pressure regenerator column and form pressure reduction, the regeneration overhead of wherein pressurizeing pressure-controlling is at gauge pressure 0.05～0.14MPa, normal pressure regeneration overhead pressure-controlling is at gauge pressure 0.01～0.09Mpa, makes that the solution boiling point produces 8～20 ℃ the temperature difference, water vapor and CO in the resurgent gases that the regeneration overhead of pressurizeing is thus come out at the bottom of two Tatas 2Mol ratio reduce to 0.8～1.2: 1.
4. method as claimed in claim 3, it is characterized in that lean solution is after the lean pump pressurization, separated into two parts, 70～85% directly enter on the second section filler in absorption tower, 15～30% enter the first section filler in top, absorption tower after the lean solution chiller temperature is reduced to 70～90 ℃, every section filler can be divided into 1 layer～4 layers.
5. method as claimed in claim 3, the regeneration overhead pressure-controlling that it is characterized in that pressurizeing be at gauge pressure 0.06～0.12MPa, and normal pressure regeneration overhead pressure-controlling is at gauge pressure 0.02～0.08Mpa, makes that the solution boiling point produces 10～16 ℃ the temperature difference at the bottom of two towers.
6. method as claimed in claim 3 is characterized in that the used power steam pressure of adjustable supersonic speed steam injector is gauge pressure 0.04～0.16Mpa, and temperature is at 141～200 ℃, and the consumption of power steam is determined according to unit scale and processing condition; The steam of releasing from the normal pressure regenerator column and the weight ratio of power steam are 0.8～1.4.
7. method as claimed in claim 6 is characterized in that the used power steam pressure of adjustable supersonic speed steam injector is gauge pressure 0.06～0.12MPa, and temperature is at 158～187 ℃; The steam of releasing from the normal pressure regenerator column and the weight ratio of power steam are 0.9～1.2.
CN200810196779A 2008-10-13 2008-10-13 Method for removing carbon dioxide aqueous solution by ethylene oxide/ethylene glycol synthesized recycle gas Pending CN101723919A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102441316A (en) * 2011-09-23 2012-05-09 中国石油化工股份有限公司 Decarburization solution containing vanadate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102441316A (en) * 2011-09-23 2012-05-09 中国石油化工股份有限公司 Decarburization solution containing vanadate

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Application publication date: 20100609