CN115770623A - Preparation method of ion exchange membrane for camphor esterification reaction - Google Patents
Preparation method of ion exchange membrane for camphor esterification reaction Download PDFInfo
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- CN115770623A CN115770623A CN202211589056.6A CN202211589056A CN115770623A CN 115770623 A CN115770623 A CN 115770623A CN 202211589056 A CN202211589056 A CN 202211589056A CN 115770623 A CN115770623 A CN 115770623A
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- 239000003014 ion exchange membrane Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005886 esterification reaction Methods 0.000 title abstract description 13
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 title description 4
- 241000723346 Cinnamomum camphora Species 0.000 title description 3
- 229930008380 camphor Natural products 0.000 title description 3
- 229960000846 camphor Drugs 0.000 title description 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 94
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 238000002791 soaking Methods 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000007599 discharging Methods 0.000 claims abstract description 17
- 238000005470 impregnation Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000012528 membrane Substances 0.000 claims description 28
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 5
- -1 polyethylene Polymers 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 230000008961 swelling Effects 0.000 claims 2
- 230000003247 decreasing effect Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002585 base Substances 0.000 description 39
- 210000004379 membrane Anatomy 0.000 description 15
- 238000007654 immersion Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000007172 homogeneous catalysis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 1
- 210000002469 basement membrane Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229930006739 camphene Natural products 0.000 description 1
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229940085790 synthetic camphor Drugs 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
-
- 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
- Y02P20/10—Process efficiency
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- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a preparation method of an ion exchange membrane for camphor-esterification reaction, which belongs to the technical field of chemical product preparation, can safely prepare the ion exchange membrane for camphor-esterification reaction with high catalytic efficiency by using the method, and has the characteristics of simple process, safety and environmental protection; the method comprises the following steps: (1) Taking a base film, fixing the base film, placing the base film in a reaction tank, adding impregnation liquid into the reaction tank, heating and soaking, and discharging the impregnation liquid in the reaction tank; (2) Adding a curing liquid into the reaction tank, heating and soaking, discharging the curing liquid in the reaction tank, and wiping the upper and lower surfaces of the film and the interior of the reaction tank; (3) Adding the expansion liquid into the reaction tank, heating and soaking, and discharging the expansion liquid in the reaction tank; (4) Adding concentrated sulfuric acid into the reaction tank, heating and soaking, and discharging the concentrated sulfuric acid in the reaction tank after cooling; (5) Adding sulfuric acid with the concentration reduced sequentially into the reaction tank for multiple times; and (6) adding clear water into the reaction tank for cleaning.
Description
Technical Field
The invention relates to the technical field of chemical product preparation, in particular to a preparation method of an ion exchange membrane for camphoration reaction.
Background
In the existing production of synthetic camphor, a catalytic system is utilized to cause camphene and formic acid or glacial acetic acid to generate addition esterification reaction to generate the isobornyl organic acid. The catalytic systems used can be divided into homogeneous catalysis and heterogeneous catalysis. Homogeneous catalysis uses liquid inorganic acid as a catalyst, such as sulfuric acid and the like, but the reaction of the acid esterification has the problems of poor reaction selectivity, a plurality of byproducts, difficult subsequent separation, easy corrosion of equipment, generation of a large amount of acid-containing wastewater and the like. The heterogeneous catalyst takes ion exchange resin, zeolite, molecular sieve and the like as catalysts, and the catalysts can improve the selectivity of the reaction, reduce or avoid the corrosion of equipment and the discharge of acid wastewater, and are the most ideal esterification method.
The existing ion exchange membrane for the camphoration reaction is generally made of a polyethylene film, and the manufacturing process comprises the following steps: (1) Soaking the film in divinylbenzene to swell the film, and then soaking the film in warm water for curing; (2) Wiping off the moisture on the surface of the solidified film, and sulfonating the film by using dichloroethane solution containing chlorosulfonic acid; (3) Putting the film subjected to sulfonation treatment into hot water containing alkali for hydrolysis; (4) Soaking the hydrolyzed film in dichloroethane solution, and sulfonating the film in high-temperature concentrated sulfuric acid; (5) And gradually cleaning the sulfonated film with dilute sulfuric acid to obtain the sulfonated film.
The existing ion exchange membrane for the camphor-esterification reaction also has the problems of quick catalyst deactivation and long catalytic reaction time, and the sulfonation reaction in the membrane preparation process belongs to a special process, so that the preparation difficulty is increased. Therefore, it is desired to provide a method for easily and safely producing an ion exchange membrane for camphoration reaction, which solves the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of an ion exchange membrane for camphor-esterification reaction, which can be used for preparing the ion exchange membrane for camphor-esterification reaction with high catalytic efficiency more safely and has the characteristics of simple process, safety and environmental protection.
The technical scheme of the invention is as follows:
a preparation method of an ion exchange membrane for camphoration reaction comprises the following steps:
(1) Taking a base film, fixing the base film, placing the base film in a reaction tank, adding impregnation liquid into the reaction tank, heating and soaking, and discharging the impregnation liquid in the reaction tank;
(2) Adding a curing liquid into the reaction tank, heating and soaking, discharging the curing liquid in the reaction tank, and wiping the upper and lower surfaces of the film and the interior of the reaction tank;
(3) Adding the expansion liquid into the reaction tank, heating and soaking, and discharging the expansion liquid in the reaction tank;
(4) Adding concentrated sulfuric acid into the reaction tank, heating and soaking, and discharging the concentrated sulfuric acid in the reaction tank after cooling;
(5) Adding sulfuric acid with the concentration reduced sequentially into the reaction tank for multiple times, and emptying the sulfuric acid in the reaction tank before adding the sulfuric acid each time;
(6) And adding clear water into the reaction tank for cleaning, and taking out the film from the reaction tank.
Further, in the step (1), the selected base film is a polyethylene film, and the impregnation liquid is one of styrene, divinylbenzene and xylene.
Further, in the step (1), the temperature in the reaction tank is controlled to be 60-65 ℃ when the base film is soaked in the impregnation liquid, and the soaking is completed until the thickness of the base film is increased by 140 mm.
Further, in the step (2), the added curing solution is azobisisobutyronitrile, and when the base film is soaked in the curing solution, the temperature in the reaction tank is controlled to be 68-72 ℃, and the soaking time is 5 hours.
Further, in the step (3), the added expansion liquid is dichloroethane or pinene, the temperature in the reaction tank is controlled to be 48-52 ℃ when the base membrane is soaked in the expansion liquid, and the soaking is completed until the thickness of the base membrane is increased by 20 mm.
Further, in the step (4), the base film is soaked in concentrated sulfuric acid, the temperature in the reaction tank is controlled to be 79-83 ℃, and the heating is stopped after the base film is soaked for 8 hours.
Further, in the step (5), 2 times of sulfuric acid with the concentration being reduced sequentially is added into the reaction tank, and the concentration of the sulfuric acid added 2 times is 25% and 15% sequentially.
Further, the method also comprises a step (7) of cutting the film according to the specification and storing the film in a wet state.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the ion exchange membrane for the camphor-esterification reaction comprises the steps of taking a base membrane, fixing the base membrane, placing the base membrane in a reaction tank, sequentially and respectively adding immersion liquid, curing liquid, expansion liquid and concentrated sulfuric acid into the thin membrane for immersion reaction, and cleaning the base membrane by using sulfuric acid and clear water with sequentially reduced concentrations to obtain the ion exchange membrane for the camphor-esterification reaction. According to the method, the thickening condition, the temperature and the soaking time of the film during the soaking reaction by adding the immersion liquid, the curing liquid and the expansion liquid into the film are controlled, so that the thickness of the film can be effectively increased, the expansion effect of the film is better, the contact area of a catalyst is effectively increased, and the catalytic efficiency is improved; the ion exchange membrane with good catalytic performance can be obtained by acidifying the ion exchange membrane by concentrated sulfuric acid, the preparation difficulty in the preparation process is lower, the safety coefficient is higher, too much acid-containing wastewater cannot be generated, the ion exchange membrane is more environment-friendly, the catalytic reaction time of the prepared ion exchange membrane is shorter, and the activity is more durable.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited thereto.
The invention relates to a preparation method of an ion exchange membrane for camphoration reaction, which comprises the following steps:
(1) Taking and fixing the base film, placing the base film in a reaction tank, adding the impregnation liquid into the reaction tank, heating and soaking, and discharging the impregnation liquid in the reaction tank.
The selected base film is a polyethylene film, the base film is generally cut according to specifications and then placed into a reaction tank, the cut base film needs to be fixed on 2 rollers, the base film is clamped and fixed through a fastening roller on the rollers, the base film is required to be leveled and fixed when being rolled, one side of each roller is required to be marked, the other side of the base film spans across a fastening roller of the other roller and is fixed, and the rollers are fixedly placed in the reaction tank. The impregnation liquid is one of styrene, divinylbenzene and xylene. The impregnation liquid added into the reaction tank immerses two thirds of the height of the base film, the temperature in the reaction tank is controlled to be 60-65 ℃ when the base film is immersed in the impregnation liquid, a roller is rotated every 3-5 minutes during immersion to ensure that the base film is immersed more fully, and the temperature, namely the immersion time, of the base film during immersion is controlled. Soaking until the thickness of the base film is 1030-1050 mm, namely, the reaction is finished after the thickness of the base film is increased by 140 mm. The discharged impregnation liquid is required to be placed in a barrel and needs to be marked in a good state during storage. After the immersion liquid is put in, 2 rollers are required to be taken out to dry the immersion liquid on the basement membrane.
(2) And adding the curing liquid into the reaction tank, heating and soaking, discharging the curing liquid in the reaction tank, and wiping the upper surface and the lower surface of the film and the interior of the reaction tank.
Wherein the added curing liquid is azobisisobutyronitrile, the temperature in the reaction tank is controlled to be 68-72 ℃ when the base film is soaked in the curing liquid, the soaking time is 5 hours, and the roller is rotated every 15 minutes during soaking to ensure that the base film is soaked more fully. The curing liquid is obtained by dissolving the curing agent in water at the temperature of 70 ℃, and the added curing liquid is required to be 3cm above the ground surface of the film. After the solidified liquid in the reaction tank is discharged, the upper and lower surfaces of the film and the interior of the reaction tank must be wiped dry, otherwise the next soaking effect is affected.
(3) Adding the expansion liquid into the reaction tank, heating and soaking, and discharging the expansion liquid in the reaction tank.
Wherein, the added expansion liquid is dichloroethane or pinene, the temperature in the reaction tank is controlled to be 48-52 ℃ when the base membrane is soaked in the expansion liquid, and the roller is rotated every 5 minutes during soaking to ensure that the base membrane is soaked more fully. The soaking is completed after the thickness of the base film is increased by 20mm, and the base film is soaked in the expanding liquid at the temperature, so that the soaking effect is optimal. After soaking, the expansion liquid is discharged and placed in a barrel, and the state is marked during storage for subsequent treatment.
(4) Adding concentrated sulfuric acid into the reaction tank, heating and soaking, and discharging the concentrated sulfuric acid in the reaction tank after cooling.
The base film is soaked in concentrated sulfuric acid, the temperature in the reaction tank is controlled to be 79-83 ℃, heating is stopped after soaking for 8 hours, and the concentrated sulfuric acid is kept in the temperature range in the soaking process, so that the acidification effect of the base film can be ensured. When concentrated sulfuric acid is put into the reaction tank, the concentrated sulfuric acid needs to be slowly added to the position from the liquid level to two thirds of the base membrane. The roller is rotated every 15 minutes in the soaking process, so that the acidification reaction is more sufficient. When the reacted concentrated sulfuric acid is discharged, the concentrated sulfuric acid needs to be barreled and placed, and the state needs to be marked when the concentrated sulfuric acid is stored.
(5) Sulfuric acid with the concentration reduced sequentially is added into the reaction tank for multiple times, and the sulfuric acid in the reaction tank is emptied before the sulfuric acid is added each time.
Wherein, the sulfuric acid with the concentration reduced sequentially is added into the reaction tank for 2 times, and the concentration of the sulfuric acid added for 2 times is 25 percent and 15 percent sequentially. Adding sulfuric acid into the reaction tank to the liquid level of two thirds of the base film, shaking the roller after adding the sulfuric acid, discharging the sulfuric acid in the reaction tank, and placing the discharged sulfuric acid in a barrel to be marked when storing.
(6) And adding clear water into the reaction tank for cleaning, and taking out the film from the reaction tank to obtain the film.
Preferably, the reaction tank is washed by adding clean water in 2 times, and the water in the reaction tank is emptied before adding the clean water each time.
Further, the method also comprises the step (7) of putting the obtained ion exchange membrane into a membrane soaking pool for cleaning again, cutting according to specifications, and storing in a wet state.
According to the preparation method of the ion exchange membrane for the camphor esterification reaction, the thickening condition, the temperature and the soaking time of the soaking reaction of adding the immersion liquid, the curing liquid and the expansion liquid into the membrane are controlled, so that the thickness of the membrane can be effectively increased, the expansion effect of the membrane is better, the contact area of the catalyst is effectively increased, and the catalytic efficiency is improved; and the ion exchange membrane with good catalytic performance can be obtained by acidifying the ion exchange membrane by concentrated sulfuric acid, the preparation difficulty in the preparation process is lower, the safety coefficient is higher, too much acid-containing wastewater cannot be generated, and the ion exchange membrane is more environment-friendly. The catalytic reaction time of the prepared ion exchange membrane is 15-20% shorter than that of the existing ion exchange membrane. The activity lasting time of the prepared ion exchange membrane is 12-17% longer than that of the existing ion exchange membrane, so that the performance of the ion exchange membrane prepared by the preparation method is better than that of the existing ion exchange membrane.
The above description is only exemplary of the invention, and any modification, equivalent replacement, and improvement made within the spirit and scope of the present invention should be considered within the scope of the present invention.
Claims (8)
1. A preparation method of an ion exchange membrane for camphoration reaction is characterized by comprising the following steps:
(1) Taking a base membrane, fixing the base membrane and placing the base membrane in a reaction tank, adding an impregnation liquid into the reaction tank, heating and soaking, and discharging the impregnation liquid in the reaction tank;
(2) Adding a curing liquid into the reaction tank, heating and soaking, discharging the curing liquid in the reaction tank, and wiping the upper and lower surfaces of the film and the interior of the reaction tank;
(3) Adding an expansion liquid into the reaction tank, heating and soaking, and discharging the expansion liquid in the reaction tank;
(4) Adding concentrated sulfuric acid into the reaction tank, heating and soaking, and discharging the concentrated sulfuric acid in the reaction tank after cooling;
(5) Adding sulfuric acid with the concentration reduced sequentially into the reaction tank for multiple times, and emptying the sulfuric acid in the reaction tank before adding the sulfuric acid each time;
(6) And adding clear water into the reaction tank for cleaning, and taking out the film from the reaction tank.
2. The method of claim 1, wherein in the step (1), the base film is a polyethylene film, and the impregnation liquid is one of styrene, divinylbenzene and xylene.
3. The method of claim 2, wherein the step (1) comprises immersing the base membrane in the impregnation solution while controlling the temperature in the reaction tank to be 60-65 ℃ until the thickness of the base membrane increases by 140 mm.
4. The method of claim 1, wherein the curing solution added in step (2) is azobisisobutyronitrile, and the temperature of the base membrane in the reaction tank is controlled to be 68-72 ℃ and the soaking time is 5 hours when the base membrane is soaked in the curing solution.
5. The method of claim 1, wherein the swelling solution added in step (3) is dichloroethane or pinene, the temperature of the base membrane in the reaction tank is controlled to be 48-52 ℃ when the base membrane is soaked in the swelling solution, and the soaking is completed until the thickness of the base membrane is increased by 20 mm.
6. The method of claim 1, wherein the base membrane is immersed in concentrated sulfuric acid at a temperature of 79-83 ℃ for 8 hours, and then heating is stopped.
7. The method of claim 1, wherein the sulfuric acid is added to the reaction tank 2 times at decreasing concentrations, and the sulfuric acid is added to the reaction tank 2 times at 25% and 15% in the sequence.
8. The method of claim 1, further comprising the step of (7) cutting the membrane to a predetermined size and storing the membrane in a wet state.
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| CN202211589056.6A CN115770623B (en) | 2022-12-09 | 2022-12-09 | Preparation method of ion exchange membrane for camphoresterification reaction |
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| CN202211589056.6A CN115770623B (en) | 2022-12-09 | 2022-12-09 | Preparation method of ion exchange membrane for camphoresterification reaction |
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