CN109485766A - A kind of preparation method of cation exchange resin - Google Patents
A kind of preparation method of cation exchange resin Download PDFInfo
- Publication number
- CN109485766A CN109485766A CN201710815591.1A CN201710815591A CN109485766A CN 109485766 A CN109485766 A CN 109485766A CN 201710815591 A CN201710815591 A CN 201710815591A CN 109485766 A CN109485766 A CN 109485766A
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- China
- Prior art keywords
- solution
- added
- exchange resin
- cation exchange
- pearl
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/24—Treatment of polymer suspensions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/36—Sulfonation; Sulfation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention provides a kind of preparation method of cation exchange resin, includes the following steps, distilled water and polyvinyl alcohol are added in the reaction vessel；Heating, while it being stirred to react container, keep polyvinyl alcohol dissolution abundant；After solution is cooling, the monomer mixture solution of meaning initiator is added into solution；Agitating solution, while reaction vessel is heated to 80 DEG C, so that monomer is dissipated into pearl；Keep reaction temperature, sustained response 2h；Continuing heating hardens pearl；Pearl is taken out, is then successively washed, is filtered, it is dry；Dichloroethane solution is added in pearl, and is heated to 60 DEG C；Silver sulfate is added, then the concentrated sulfuric acid is added dropwise, then proceedes to be heated up to 85 DEG C；Reaction temperature is kept, the reaction was continued；Complete sulfonating reaction；Sulfonated products are cooling, sulfuric acid solution is then added, distilled water dilution is added dropwise under stirring；The dichloroethanes in solution is removed, is washed out no acidic to filtrate；Washing is filtered, dry, obtains cation exchange resin.
Description
Technical field
The present invention relates to ion exchange resin production technical fields, and in particular to a kind of preparation side of cation exchange resin
Method.
Background technique
Ion exchange resin is a kind of functional polymer compound for having functional group, is widely used in water process, food
Industry, chemical company etc..Traditional ion exchange resin is macromolecule figure network structure polymer, most resin preparations
When need two step process, first synthesize three-dimensional netted skeleton, then by introducing functional group on reaction skeleton.Polystyrene-diethyl
Alkene benzene sulfonic acid cation exchange resin is resin most wide in ion exchange resin application, passes through the concentrated sulfuric acid, chlorosulfonic acid, three oxidations
Sulfonation of strong oxidizers such as sulphur and oleum or so introduces sulfonic group on the styrene phenyl ring of crosslinking and is made, preparation process
Complexity, activity time is long, while consuming a large amount of sulfuric acid, and operating process is dangerous, and does not wash clean clearly, the discharge of sulfuric acid
Lead to the pollution to environment.
The exchange capacity of cation exchange resin has obtained effective raising at present, but pore-size distribution is uneven, aperture ratio
Excessive, water intermediate ion needs to penetrate into inside resin when exchange, so exchange velocity is low, while the resin regeneration time is long.
The preparation method of existing cation exchange resin is long there are the period in reaction time, product stability is not high, reacted
The defects of journey is not easily controlled.
Summary of the invention
Goal of the invention: the present invention provides a kind of preparation method of cation exchange resin, can shorten reaction time, improves
Product quality.
Technical solution: to achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of cation exchange resin, includes the following steps,
Step 1: distilled water and polyvinyl alcohol being added in the reaction vessel；
Step 2: heating reaction vessel, while it being stirred to react container, keep polyvinyl alcohol dissolution abundant；
Step 3: after step 2 acquired solution is cooling, the monomer mixture solution of meaning initiator being added into solution；
Step 4: agitating solution, while reaction vessel is heated, so that monomer is dissipated into pearl；
Step 5: keeping reaction temperature, sustained response；
Step 6: continuing heating hardens pearl；
Step 7: pearl is taken out, is then successively washed, is filtered, it is dry；
Step 8: dichloroethane solution is added in pearl, and is heated；
Step 9: silver sulfate is added, then the concentrated sulfuric acid is added dropwise, then proceedes to heat；
Step 10: keeping reaction temperature, the reaction was continued；Complete sulfonating reaction；
Step 11: sulfonated products are cooling, sulfuric acid solution is then added, distilled water dilution is added dropwise under stirring；
Step 12: the dichloroethanes in removal step 11 acquired solution is washed out no acidic to filtrate；
Step 13: washing is filtered, dry, obtains cation exchange resin.
Preferably, in step 3, the monomer mixture is the mixture of styrene and benzoyl peroxide.
Preferably, in step 4, it is heated up to 80-90 DEG C.
Preferably, in step 5, reaction temperature 2-3h.
Preferably, in step 8, it is heated up to 60-70 DEG C.
Preferably, in step 9, it is continuously heating to 75-85 DEG C.
The utility model has the advantages that the present invention improves cation exchange tree by adjusting reaction time, reaction temperature, reaction step
Rouge conventional preparation techniques substantially reduce the reaction time of traditional preparation methods, improve product quality；Step letter of the present invention
It is single, it is easily manipulated, is capable of the quality of stable prod well.
Specific embodiment
Further explanation is done to the present invention below with reference to embodiment.
Embodiment 1:
A kind of preparation method of cation exchange resin, includes the following steps,
Step 1: distilled water and polyvinyl alcohol being added in the reaction vessel；
Step 2: heating reaction vessel, while it being stirred to react container, keep polyvinyl alcohol dissolution abundant；
Step 3: after step 2 acquired solution is cooling, the monomer mixture solution of meaning initiator being added into solution；
Step 4: agitating solution, while reaction vessel is heated to 80 DEG C, so that monomer is dissipated into pearl；
Step 5: keeping reaction temperature, sustained response 2h；
Step 6: continuing heating hardens pearl；
Step 7: pearl is taken out, is then successively washed, is filtered, it is dry；
Step 8: dichloroethane solution is added in pearl, and is heated to 60 DEG C；
Step 9: silver sulfate is added, then the concentrated sulfuric acid is added dropwise, then proceedes to be heated up to 85 DEG C；
Step 10: keeping reaction temperature, the reaction was continued；Complete sulfonating reaction；
Step 11: sulfonated products are cooling, sulfuric acid solution is then added, distilled water dilution is added dropwise under stirring；
Step 12: the dichloroethanes in removal step 11 acquired solution is washed out no acidic to filtrate；
Step 13: washing is filtered, dry, obtains cation exchange resin.
Obtain cation exchange resin.
Embodiment 2:
A kind of preparation method of cation exchange resin, includes the following steps,
Step 1: distilled water and polyvinyl alcohol being added in the reaction vessel；
Step 2: heating reaction vessel, while it being stirred to react container, keep polyvinyl alcohol dissolution abundant；
Step 3: after step 2 acquired solution is cooling, the monomer mixture solution of meaning initiator being added into solution；
Step 4: agitating solution, while reaction vessel is heated to 90 DEG C, so that monomer is dissipated into pearl；
Step 5: keeping reaction temperature, sustained response 3h；
Step 6: continuing heating hardens pearl；
Step 7: pearl is taken out, is then successively washed, is filtered, it is dry；
Step 8: dichloroethane solution is added in pearl, and is heated to 70 DEG C；
Step 9: silver sulfate is added, then the concentrated sulfuric acid is added dropwise, then proceedes to be heated up to 75 DEG C；
Step 10: keeping reaction temperature, the reaction was continued；Complete sulfonating reaction；
Step 11: sulfonated products are cooling, sulfuric acid solution is then added, distilled water dilution is added dropwise under stirring；
Step 12: the dichloroethanes in removal step 11 acquired solution is washed out no acidic to filtrate；
Step 13: washing is filtered, dry, obtains cation exchange resin.
Obtain cation exchange resin.
According to following embodiments, the present invention can be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies specific material proportion, process conditions and its result described in example and is merely to illustrate the present invention, without that should will not limit
The present invention described in detail in claims processed.
Claims (6)
1. a kind of preparation method of cation exchange resin, which is characterized in that include the following steps,
Step 1: distilled water and polyvinyl alcohol being added in the reaction vessel；
Step 2: heating reaction vessel, while it being stirred to react container, keep polyvinyl alcohol dissolution abundant；
Step 3: after step 2 acquired solution is cooling, the monomer mixture solution of meaning initiator being added into solution；
Step 4: agitating solution, while reaction vessel is heated, so that monomer is dissipated into pearl；
Step 5: keeping reaction temperature, sustained response；
Step 6: continuing heating hardens pearl；
Step 7: pearl is taken out, is then successively washed, is filtered, it is dry；
Step 8: dichloroethane solution is added in pearl, and is heated；
Step 9: silver sulfate is added, then the concentrated sulfuric acid is added dropwise, then proceedes to heat；
Step 10: keeping reaction temperature, the reaction was continued；Complete sulfonating reaction；
Step 11: sulfonated products are cooling, sulfuric acid solution is then added, distilled water dilution is added dropwise under stirring；
Step 12: the dichloroethanes in removal step 11 acquired solution is washed out no acidic to filtrate；
Step 13: washing is filtered, dry, obtains cation exchange resin.
2. a kind of preparation method of cation exchange resin according to claim 1, which is characterized in that described in step 3
Monomer mixture is the mixture of styrene and benzoyl peroxide.
3. a kind of preparation method of cation exchange resin according to claim 1, which is characterized in that in step 4, heating
To 80-90 DEG C.
4. a kind of preparation method of cation exchange resin according to claim 1, which is characterized in that in step 5, reaction
Temperature is 2-3h.
5. a kind of preparation method of cation exchange resin according to claim 1, which is characterized in that in step 8, heating
To 60-70 DEG C.
6. a kind of preparation method of cation exchange resin according to claim 1, which is characterized in that in step 9, continue
It is warming up to 75-85 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710815591.1A CN109485766A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of cation exchange resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710815591.1A CN109485766A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of cation exchange resin |
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| CN109485766A true CN109485766A (en) | 2019-03-19 |
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| CN201710815591.1A Withdrawn CN109485766A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of cation exchange resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574229A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Method for preparing isosorbide by dehydrating sorbitol and preparation method of copolymer-based catalyst thereof |
| WO2021238315A1 (en) * | 2020-05-25 | 2021-12-02 | 浙江大学 | Grafted quaternary ammonium group cation resin and preparation method therefor |
-
2017
- 2017-09-12 CN CN201710815591.1A patent/CN109485766A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574229A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Method for preparing isosorbide by dehydrating sorbitol and preparation method of copolymer-based catalyst thereof |
| CN112574229B (en) * | 2019-09-29 | 2022-03-29 | 中国石油化工股份有限公司 | Method for preparing isosorbide by dehydrating sorbitol and preparation method of copolymer-based catalyst thereof |
| WO2021238315A1 (en) * | 2020-05-25 | 2021-12-02 | 浙江大学 | Grafted quaternary ammonium group cation resin and preparation method therefor |
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Application publication date: 20190319 |