CN112191077A - Chloromethane gas dehydration process in butyl rubber production process - Google Patents
Chloromethane gas dehydration process in butyl rubber production process Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1425—Regeneration of liquid absorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/263—Drying gases or vapours by absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/80—Water
Abstract
A chloromethane gas dehydration process in the production process of butyl rubber, belonging to the technical field of separation and purification. The method comprises the following steps of sending industrial materials containing certain water into an absorption tower through a pipeline, wherein the operation conditions of the absorption tower are preferably as follows: the temperature is 25 ℃, the absolute pressure is 4atm, and the theoretical plate number is 6. The water content in the industrial material is 0.1-2% (mass fraction, the same below), the ionic liquid rich in water at the bottom of the tower enters a first flash tank firstly to remove most of the chloromethane contained in the ionic liquid, then enters a second flash tank to remove the water contained in the ionic liquid, the ionic liquid extracted from the bottom of the second flash tank is recycled, and finally the water content in the gas discharged from the tower reaches the ppm level.
Description
Technical Field
The invention relates to a chloromethane gas dehydration process in the production process of butyl rubber. The absorbent is selected from single ionic liquid, cations of the ionic liquid can be imidazoles, pyridines, quaternary ammonium salts and the like, and anions can be bis (trifluoromethanesulfonimide), tetrafluoroborate, hexafluorophosphate, acetate, diethyl sulfate and the like. Belongs to the technical field of separation and purification.
Background
In industry, methyl chloride is an indispensable solvent in the production of butyl rubber, and the water content in the methyl chloride directly influences the quality of a final product. The butyl rubber device methyl chloride dehydration process usually adopts an activated alumina adsorption method to remove water in wet methyl chloride, and can basically meet the production requirements, but the drying agent has short service cycle, frequent regeneration and large energy consumption, and brings a series of problems of poor production stability, high operation cost, environmental pollution and the like. On the basis of wide reference of technical data and communication with experts and academia at home and abroad, a new process for adding ionic liquid to pre-dehydration in front of a drying tower in the prior art is provided by taking the relevant documents of ionic liquid in natural gas dehydration, carbon dioxide dehydration, oxygen dehydration and pentafluoroethane dehydration as reference. Finally selecting proper ionic liquid as a dehydration solvent through calculation and comparison, and carrying out detailed design on key process parameters in the new process, such as the number of absorption tower plates, the amount of the absorption solvent, a flash tank, a heat exchanger and the like. In the research method, the flow simulation calculation is mainly adopted.
In addition, many other dewatering methods are reported in the literature, such as physical dewatering: removing water in methane chloride by using a NaA molecular sieve: the method has the advantages that the adsorbent can be regenerated and reused; the method has the disadvantages that the adsorbent is heated by high-temperature inert gas to gasify water, the residual material gas in the adsorbent is difficult to recover, the pollution is large, and the regeneration energy consumption is high; dehydrating triethylene glycol: the method has the advantages that the triethylene glycol has high hygroscopicity, low steam pressure and small regeneration loss, no inert gas is required to be introduced in the regeneration process, and the environmental pollution is small; the defects that triethylene glycol still has certain saturated vapor pressure and can generate certain loss; the long-time operation is easy to generate oxidation reaction to generate acidic organic acid, so that equipment is corroded; triethylene glycol is easy to foam, and a defoaming agent is required to be added, so that the cost is increased; the desorption tower is used in the regeneration process, the mass transfer and diffusion efficiency of water from triethylene glycol is low, the regeneration temperature is high (generally at 180 ℃) to achieve a better regeneration effect, and the energy consumption is high. In addition, triethylene glycol has high solubility to some gases, increases equipment investment in a regeneration process, and has complex regeneration process and high operation.
In conclusion, the ionic liquid has the advantages of no toxicity, almost no volatilization, chemical stability, thermal stability and the like, so that the ionic liquid after desorption can be recycled by using the ionic liquid dehydration method. The method completes the dehydration process in one absorption tower, simplifies the process flow, has low energy consumption, reduces equipment investment, conforms to the characteristics of energy conservation, emission reduction and miniaturization, and avoids the problems of high energy consumption, environmental pollution and the like caused by using the traditional method.
Disclosure of Invention
The invention aims to provide a chloromethane gas dehydration process in the production process of butyl rubber, which adopts ionic liquid as an absorbent to remove water in industrial materials, the water content of materials at the top of a tower is less than 20ppmw, the ionic liquid can be recycled through flash evaporation, and a gas stripping process is added in a second flash tank, so that the water content of regenerated ionic liquid is greatly reduced, the water content of product gas is greatly reduced, and the ionic liquid is hardly lost.
The invention provides a chloromethane gas dehydration process in the production process of butyl rubber, wherein an absorbent is ionic liquid, and the dehydration process is characterized in that the operation conditions of an absorption tower are as follows: the temperature is 20-30 ℃, the absolute pressure is 350-450kp, the theoretical plate number is 4-8, and 6 are preferred; feeding the water-containing industrial material from the bottom of the absorption tower, adding the single ionic liquid as an absorbent from the top of the absorption tower, wherein the solvent ratio is 0.1-2 (the solvent ratio is the ratio of the mass flow of the ionic liquid added into the absorption tower to the mass flow of the raw material gas), and the water content in the industrial material is 0.1-1% (mass fraction, the same below); generally, after the water content of the dried material is less than 20ppmw, the ionic liquid rich in water at the bottom of the tower enters a first flash tank to remove most of methyl chloride contained in the ionic liquid, and the operating conditions of the first flash tank are as follows: the temperature is 45-55 ℃, the pressure is 0.03-0.07atm, then the mixture enters a second flash tank to remove the water contained in the mixture, and the operating conditions of the second flash tank are as follows: the temperature is 130-150 ℃, the pressure is 0.03-0.07atm, the ionic liquid extracted from the bottom of the second flash tank is recycled, and the gas phase extracted from the upper part enters the next treatment process after being condensed.
The operating conditions of the absorption tower are preferably as follows: the temperature is 25 ℃, the absolute pressure is 4atm, and the theoretical plate number is 6.
A pre-heat exchanger B4 is added between the absorption tower and the first flash tank, a heat exchanger B7 is added between the first flash tank and the second flash tank, and the ionic liquid extracted from the bottom of the flash tank is cooled to room temperature in a cooler B6.
And adding a heat exchanger B10 at the top of the first flash tank to cool the gas discharged from the tower, adding a heat exchanger B14 at the top of the second flash tank to cool the gas discharged from the tower, and adding B4 at the bottom of the flash tank to circulate the ionic liquid.
And further optimizing, in order to reduce the water content of the regenerated ionic liquid, adding isobutene gas when stripping and strengthening dehydration are carried out on the ionic liquid in the second flash tank, adding isobutene by continuously conveying isobutene gas flow, enabling the isobutene gas flow to flow in a counter-current manner relative to the ionic liquid from bottom to top, enabling the mass flow ratio of the ionic liquid flow to the isobutene gas flow to be 100 (5-60), and cooling the regenerated ionic liquid with lower water content to room temperature through a cooler B6 for continuous use, so that a better dehydration effect can be achieved.
The absorbent is a single ionic liquid or a mixture of two ionic liquids. The adopted ionic liquid cations are imidazoles, pyridines, quaternary ammonium salts, quaternary phosphonium salts and the like, and the anions are bis (trifluoromethanesulfonimide), tetrafluoroborate, hexafluorophosphate, acetate, diethyl sulfate and the like.
When the traditional monochloromethane dehydration technology is adopted, the operation is complex, the energy consumption is high, the service cycle is short, deep dehydration cannot be realized, and when the ionic liquid is adopted for dehydration, the water content in the final material can reach the ppm level, so that the problems of high energy consumption, environmental pollution and the like caused by the traditional method are avoided, the process and the equipment are simple, the investment is low, the energy consumption is low, and the industrial cost is greatly reduced.
Drawings
FIG. 1 is a process flow diagram of water removal from methyl chloride by ionic liquid under normal pressure. Wherein, B1 is a first delivery pump; b2 is an absorption tower; b3 is a second delivery pump; b4 is a preheater; b5 is a first storage tank; b6 is a first cooler; b7 is a heat exchanger; b8 is a first flash tank; b9 is a first vacuum pump: b10 is a second cooler; b11 is a third delivery pump; b12 is a second flash tank; b13 is a second vacuum pump; b14 is a third cooler; b15 is a fourth delivery pump; b16 is a second storage tank, and the absorbent is single ionic liquid.
Detailed Description
The present invention will be described in terms of the following examples, but the present invention is not limited to the following examples, and various modifications are included within the technical scope of the present invention without departing from the scope of the present invention.
As shown in figure 1, the process flow comprises an absorption tower, a heat exchanger, a solvent flash tank and the like. In the figure, a technical material containing a small amount of water is fed from the bottom of the absorption column, and an ionic liquid is fed as an absorbent from the top of the absorption column. The material flow extracted from the bottom of the absorption tower enters a first flash tank through a pre-heat exchanger, then enters a second flash tank through a heat exchanger, other gas and water absorbed in the ionic liquid are removed by flash evaporation respectively, the ionic liquid extracted from the bottom of the flash tank is conveyed to a cooler through a centrifugal pump and then enters the absorption tower for recycling, and the gas phase extracted from the upper part enters the next treatment process after being condensed through the heat exchanger.
Example 1
The absorption scheme is shown in FIG. 1. The operating conditions of the absorption column were: the temperature is 25 ℃, the pressure absolute pressure is 400kp, the theoretical number of towers is 6, a stream of industrial materials (mass fractions of methane chloride, isobutene, water, hexane and isoprene are 94.66%, 4.72%, 0.3%, 0.2 and 0.12) from the halogenation reaction is fed from the bottom of the absorption tower, the mass flow is controlled at 1000kg/h, and ionic liquid [ EMIM ] is added]+[BF4]-(1-ethyl-3-methylimidazolium tetrafluoroborate) is added from the top of the absorption tower as an absorbent, the mass flow is 535kg/h, the water content of the material at the top of the tower is 50ppm at this time, which indicates that the water in the material can be obviously removed simultaneously by adopting an ionic liquid dehydration technology, the ionic liquid rich in water at the bottom of the absorption tower enters a first flash tank to remove most of the methyl chloride contained in the ionic liquid, and the operation conditions of the first flash tank are as follows: the temperature is 50 ℃, the pressure is 0.05atm, and then the mixture enters a second flash tank to remove the water contained in the mixture, and the operating conditions of the second flash tank are as follows: the temperature is 140 ℃, the pressure is 0.05atm, the water content of the material at the bottom of the flash tank is less than 500ppm (mass fraction, the same below), the mass fraction of the ionic liquid is 99.5 percent, and the ionic liquid extracted from the bottom of the flash tank is recycled.
The flow rate of the ionic liquid is changed to 250kg/h, other conditions are unchanged, and the water content of the overhead material is 54 ppmw.
The flow rate of the ionic liquid is changed to 350kg/h, other conditions are unchanged, and the water content of the overhead material is 53 ppmw.
The flow rate of the ionic liquid is changed to be 450kg/h, other conditions are unchanged, and the water content of the tower top material is 51 ppmw.
The flow rate of the ionic liquid is changed to 550kg/h, other conditions are unchanged, and the water content of the tower top material is 49 ppmw.
The flow rate of the ionic liquid is changed to 650kg/h, other conditions are unchanged, and the water content of the overhead material is 48 ppmw.
The flow rate of the ionic liquid is changed to 750kg/h, other conditions are unchanged, and the water content of the overhead material is 47 ppmw.
The flow rate of the ionic liquid is changed to 850kg/h, other conditions are unchanged, and the water content of the overhead material is 46 ppmw.
The flow rate of the ionic liquid is changed to 950kg/h, other conditions are unchanged, and the water content of the overhead material is 43 ppmw.
The flow rate of the ionic liquid is changed to 1050kg/h, other conditions are unchanged, and the water content of the overhead material is 42 ppmw.
Example 2
The absorption scheme is shown in the figure. The operating conditions of the absorption column were: the temperature is 25 ℃, the absolute pressure is 400kp, the theoretical number of the towers is 6, a stream of industrial materials (the mass fractions of methane chloride, isobutene, water, hexane and isoprene are 94.66%, 4.72%, 0.3%, 0.2 and 0.12) from the halogenation reaction is fed from the bottom of the absorption tower, the mass flow is controlled to be 1000kg/h, and ionic liquid [ EMIM ]]+[BF4]-(1-ethyl-3-methylimidazolium tetrafluoroborate) is added from the top of the absorption tower as an absorbent, the mass flow is 535kg/h, the water content of the material at the top of the tower is 50ppm, which indicates that the water in the material can be obviously removed by adopting an ionic liquid dehydration technology, the ionic liquid rich in water at the bottom of the absorption tower enters a first flash tank to remove most of the methyl chloride contained in the ionic liquid, and the operation conditions of the first flash tank are as follows: the temperature is 50 ℃, the pressure is 0.05atm, and then the mixture enters a second flash tank to remove the water contained in the mixture, and the operating conditions of the second flash tank are as follows: temperature 140 ℃ and pressure 0.And 05atm, adding isobutene for gas stripping, wherein the flow is 50kg/h, the water content of the material at the bottom of the flash tank is 57ppmw, the mass fraction of the ionic liquid is 99.5%, and the ionic liquid extracted at the bottom of the flash tank is recycled.
The isobutylene flow is changed to be 0kg/h, other conditions are not changed, and the water content of the ionic liquid circulated from the second flash tank is 716 ppmw.
The isobutene flow is changed to 50kg/h, other conditions are not changed, and the water content of the ionic liquid circulated from the second flash tank is 57 ppmw.
Changing the flow rate of isobutene to be 100kg/h, keeping the other conditions unchanged, and discharging the circulating ionic liquid from the second flash tank to have the water content of 33 ppmw.
The isobutylene flow is changed to 150kg/h, other conditions are not changed, and the water content of the ionic liquid circulated from the second flash tank is 24 ppmw.
Changing the flow rate of the isobutene to 200kg/h, keeping the other conditions unchanged, and discharging the circulating ionic liquid from the second flash tank to have the water content of 20 ppmw.
The isobutene flow is changed to be 250kg/h, other conditions are not changed, and the water content of the ionic liquid circulated from the second flash tank is 17 ppmw.
Example 3
The absorption scheme is shown in the figure. The operating conditions of the absorption column were: the temperature is 25 ℃, the absolute pressure is 400kp, the theoretical number of the towers is 6, a stream of industrial materials (the mass fractions of methane chloride, isobutene, water, hexane and isoprene are 94.66%, 4.72%, 0.3%, 0.2 and 0.12) from the halogenation reaction is fed from the bottom of the absorption tower, the mass flow is controlled to be 1000kg/h, and ionic liquid [ EMIM ]]+[BF4]-(1-ethyl-3-methylimidazolium tetrafluoroborate) is added from the top of the absorption tower as an absorbent, the mass flow is 535kg/h, the water content of the material at the top of the tower is 50ppm, which indicates that the water in the material can be obviously removed by adopting an ionic liquid dehydration technology, the ionic liquid rich in water at the bottom of the absorption tower enters a first flash tank to remove most of the methyl chloride contained in the ionic liquid, and the operation conditions of the first flash tank are as follows: the temperature is 50 ℃, the pressure is 0.05atm, and then the mixture enters a second flash tank to remove the water contained in the mixture, and the operating conditions of the second flash tank are as follows: the temperature is 140 ℃, the pressure is 0.05atm, the isobutene is added for air stripping, the flow is 50kg/h, and the flashThe water content of the material at the bottom of the flash tank is 57ppmw, the mass fraction of the ionic liquid is 99.5%, and the ionic liquid extracted at the bottom of the flash tank is recycled.
The flow rate of isobutene was changed to 0kg/h, and the water content of methyl chloride in the absorption tower was 50ppmw, while the other conditions were unchanged.
The flow rate of isobutene was changed to 50kg/h, and the water content of methyl chloride in the absorption tower was 4ppmw without changing other conditions.
The flow rate of isobutene was changed to 100kg/h, and the water content of chloromethane in the absorption tower was 2.3ppmw without changing other conditions.
The flow rate of isobutene was changed to 150kg/h, and the water content of methyl chloride in the absorption tower was 1.7ppmw without changing other conditions.
Claims (9)
1. A chloromethane gas dehydration process in the production process of butyl rubber is characterized in that the operating conditions of an absorption tower are as follows: the temperature is 20-30 ℃, the absolute pressure is 350-450kp, the theoretical plate number is 4-8, and 6 are preferred; feeding the water-containing industrial material from the bottom of the absorption tower, adding the single ionic liquid as an absorbent from the top of the absorption tower, wherein the solvent ratio is 0.1-2 (the solvent ratio is the ratio of the mass flow of the ionic liquid added into the absorption tower to the mass flow of the raw material gas), and the water content in the industrial material is 0.1-2% (mass fraction, the same below); generally, after the water content of the dried material is less than 20ppmw, the ionic liquid rich in water at the bottom of the tower enters a first flash tank to remove most of methyl chloride contained in the ionic liquid, then enters a second flash tank to remove water contained in the ionic liquid, the ionic liquid collected from the bottom of the second flash tank is recycled, and the gas phase collected from the upper part enters the next treatment process after being condensed.
2. The process for dehydrating methyl chloride gas in the production process of butyl rubber according to claim 1, wherein the operating conditions of the first flash tank are as follows: the temperature is 45-55 ℃, and the pressure is 0.03-0.07 atm.
3. The process of claim 1, wherein the second flash tank is operated under the following conditions: the temperature is 130-150 ℃, and the pressure is 0.03-0.07 atm.
4. The process for dehydrating methyl chloride gas in the production process of butyl rubber according to claim 1, wherein a pre-heat exchanger B4 is added between the absorption tower and the first flash tank, a heat exchanger B7 is added between the first flash tank and the second flash tank, and the ionic liquid extracted from the bottom of the flash tank is cooled to room temperature in a cooler B6.
5. The methyl chloride gas dehydration process in the production process of butyl rubber according to claim 1, characterized in that in order to reduce the water content of the regenerated ionic liquid, isobutylene gas is added when the ionic liquid is subjected to stripping strengthening dehydration in the second flash tank, isobutylene is added by continuously conveying isobutylene gas flow, the isobutylene gas flow counter-flows from bottom to top relative to the ionic liquid, the mass flow ratio of the ionic liquid flow to the isobutylene gas flow is 100 (5-60), and the regenerated ionic liquid with lower water content is cooled to room temperature by a cooler B6 and then is continuously used, so that better dehydration effect can be achieved.
6. The process for dehydrating chloromethane gas in the production process of butyl rubber according to claim 1, wherein the ionic liquid cation is selected from imidazoles, pyridines, quaternary ammonium salts and quaternary phosphonium salts, and the anion is selected from bis (trifluoromethanesulfonyl) imide, tetrafluoroborate, hexafluorophosphate, acetate and diethyl sulfate.
7. The process of claim 1, wherein the industrial material is an aqueous product material from a halogenation reaction comprising water, methyl chloride, isoprene, isobutylene, hexane.
8. The process for dehydrating methyl chloride gas in the production process of butyl rubber according to claim 1, wherein the tower gas is cooled by adding a heat exchanger B10 at the top of the first flash tank, the tower gas is cooled by adding a heat exchanger B14 at the top of the second flash tank, and the ionic liquid is circulated by adding B4 at the bottom of the flash tank.
9. The process for dehydrating methyl chloride gas in the production of butyl rubber according to claim 1, wherein the operating conditions of the absorption tower are preferably: the temperature is 25 ℃, the absolute pressure is 4atm, and the theoretical plate number is 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114028919A (en) * | 2021-11-25 | 2022-02-11 | 浙江信汇新材料股份有限公司 | Drying regeneration process and equipment for solvent chloromethane gas in butyl rubber production |
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| US3720041A (en) * | 1971-12-08 | 1973-03-13 | J Alvarez | Process for drying methyl chloride in a polymer plant |
| CN104826455A (en) * | 2015-04-21 | 2015-08-12 | 北京化工大学 | Method using ionic liquid for gas drying and dehydration |
| CN106474869A (en) * | 2016-10-14 | 2017-03-08 | 浙江大学 | A kind of method of absorption and separation lighter hydrocarbons from dry gas or industrial tail gas |
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