CN110372889A - A kind of preparation method of solion - Google Patents
A kind of preparation method of solion Download PDFInfo
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- CN110372889A CN110372889A CN201910709858.8A CN201910709858A CN110372889A CN 110372889 A CN110372889 A CN 110372889A CN 201910709858 A CN201910709858 A CN 201910709858A CN 110372889 A CN110372889 A CN 110372889A
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- Prior art keywords
- alkali film
- solion
- industrial
- chlor
- reaction kettle
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/096—Nitrogen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/11—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids from solid polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers 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 a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers 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 alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/10—Homopolymers or copolymers of unsaturated ethers
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
A kind of preparation method of solion of the present invention, it is main to use the industrial chlor-alkali film of recycling, the perfluorinated sulfonic resin of purification the inside carries out preparing solion, it has main steps that and is first started the cleaning processing with the industrial chlor-alkali film surface to recycling such as hydrochloric acid, then industrial chlor-alkali film is subjected to high-temperature digestion using dimethylformamide (DMF) in reaction kettle, then fiber filter is fallen by layering technique, finally obtain the solion containing perfluorinated sulfonic resin (PFSI), the present invention is in flow battery, fuel cell, electrolysis water membrane electrode, sensor, the fields such as cylinder body, which are electroplated, has extensive use.
Description
Technical field
The present invention relates to polymeric material field, in particular to a kind of preparation method of solion.
Background technique
Existing perfluorinated sulfonic resin solion needs in common preparation method using the complete of finished product or semi-finished product
Perfluorosulfonic acid resin causes prepared industrial chlor-alkali film cost also high because of its price height.
Summary of the invention
In view of the deficienciess of the prior art, the object of the present invention is to provide a kind of preparation methods of solion.
The technical scheme adopted by the invention is that: a kind of preparation method of solion is characterized in that, comprising with
Lower step:
Step 1, using the industrial chlor-alkali film containing perfluorinated sulfonic resin of recycling, using industrial alcohol, technical hydrochloric acid as cleaning
Liquid successively cleans industrial chlor-alkali film surface, and the visual foreign substance cleaning in surface is fallen；
Step 2, industrial chlor-alkali film is cut with scissors broken；
Step 3, the industrial chlor-alkali film and dimethylformamide organic solvents blended is added in reaction kettle, dimethylformamide
Dosage is added according to the content of perfluorinated sulfonic resin on industrial chlor-alkali film, and perfluorinated sulfonic resin and dimethylformamide press matter
Amount is than 1:17~25, and between 190 DEG C~240 DEG C, the temperature of reaction kettle is controlled 190 DEG C~210 the Oil-temperature control of reaction kettle
Between DEG C, the pressure of reaction kettle is controlled between 0.5Mpa~0.7Mpa, through high temperature pressure maintaining processing until industrial chlor-alkali film and diformazan
Base formamide is completely dissolved；
Step 4, after industrial chlor-alkali film and dimethylformamide are completely dissolved, cooling treatment is carried out, is cooled to 30 DEG C -45 DEG C i.e.
It can；
Step 5, the liquid in reaction kettle is filtered processing, prepared solion can be obtained.
In above scheme, step 2 and the interchangeable sequence of step 1.
In above scheme, after filtering technique, it will be greater than 20 microns of insoluble foreign matter and remove, until visual condition
Under, there is no insoluble substance in solution.
The beneficial effects of the present invention are: the preparation method for the solion that the present invention uses, uses the product of waste and old recycling
Industrial chlor-alkali film reacts after rubbing cleaning with dimethylformamide organic solvents as raw material, obtains and contains perfluorinated sulfonic acid tree
The solion of rouge, this method reduce preparation cost using the industrial chlor-alkali film of recycling, while also providing a kind of for work
The recycling mode of industry chlor-alkali film.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.Without departing from the idea of the above method of the present invention, it is made according to ordinary skill knowledge and customary means
Various replacements or change, should be included in the scope of the present invention.
Embodiment 1:
The preparation method of the solion used in the present embodiment, comprising the following steps:
Step 1: taking 10kg industry chlor-alkali film, perfluorinated sulfonic resin content about 80%, fiber content 20% is 32% using concentration
Hydrochloric acid its surface is cleaned, after it is rinsed with clear water.The present embodiment to concentration of hydrochloric acid with no restrictions, can basis
Actual conditions are selected.Using concentration be 95% industrial alcohol to industrial chlor-alkali film surface carry out secondary cleaning, after use clear water
It is rinsed；Industrial chlor-alkali film is finally put into drying equipment and carries out 40 DEG C of drying process.
Step 2: industrial chlor-alkali film being cut with scissors broken.The present embodiment uses pulverizer, and industrial chlor-alkali film is cut with scissors broken about 1cm × 1cm
Fritter, it is therefore an objective to convenient for the quick progress of subsequent technique.
Step 3, the broken industrial chlor-alkali film of 136kg organic solvent dimethylformamide and hinge is poured into reaction kettle, instead
The kettle temperature for answering kettle is 190 DEG C, and oil temperature is 195 DEG C, pressure 0.5Mpa, and the sulfonate resin on industrial chlor-alkali film is completely dissolved.；
Wherein, perfluorinated sulfonic resin and dimethylformamide 1:17 in mass ratio.
Step 4,31 DEG C of room temperature are naturally cooling to, decompression valve is slowly adjusted to normal pressure.
Step 5, it will be filtered out no more than 20 microns of insoluble foreign matter, such as fibrous foreign matter, under the conditions of visually in solution
Stopping when not having an insoluble substance, it is molten to can be obtained the required ion containing perfluorinated sulfonic resin and dimethylformamide
Liquid.
Obtained is that solion parameter and standard is not less than: 5 wt% of concentration, 1000 g/eq of equivalent, 1.0 meq/ of acid capacity
G, 1.0 g/cm of density3.Compared to existing using the solion containing perfluorinated sulfonic resin obtained, there is processing system
The advantages of standby at low cost, simple and reliable process.
Embodiment 2:
The preparation method for the solion that the present embodiment uses, comprising the following steps:
Step 1: industrial chlor-alkali film being cut with scissors broken.The present embodiment uses pulverizer, and industrial chlor-alkali film is cut with scissors the small of broken about 2cm × 2cm
Block, it is therefore an objective to convenient for the quick progress of subsequent technique.
Step 2: taking 20kg industry chlor-alkali film, perfluorinated sulfonic resin content about 78%, fiber content 22% is dense using 33%
The hydrochloric acid of degree cleans its surface, after it is rinsed with clear water；Using the industrial alcohol of 96% concentration to industrial chlor-alkali
Film surface carry out secondary cleaning, after rinsed with clear water；Industrial chlor-alkali film room temperature is finally dried processing.
Step 3: by 312kg organic solvent dimethylformamide and to cut with scissors broken industrial chlor-alkali film according to quality proportioning be 20:1
It is poured into reaction kettle, until sulfonate resin is completely dissolved.At 215 DEG C, the temperature of reaction kettle controls the Oil-temperature control of reaction kettle
At 200 DEG C, the pressure of reaction kettle is controlled in 0.6Mpa.
Step 4, slow air-cooled thermal conductive oil pipeline, and then 38 DEG C of room temperature are cooled to, it slowly adjusts dropping valve and is depressurized to
Normal pressure.
Step 5: by filtering technique, the insoluble foreign matter no more than 20 microns being filtered out, such as ties up foreign matter, until visual item
Under part, there is no insoluble substance in solution, after the obtained mixed liquor of perfluorinated sulfonic resin and dimethylformamide, it is obtained from
Sub- solution parameter standard is not less than: 5 wt% of solution concentration, 1000 g/eq of equivalent, 1.0 meq/g of acid capacity, 1.0 g/ of density
cm3.It has preparation method at low cost simple and reliable compared with existing preparation process.
Embodiment 3:
The preparation method for the solion that the present embodiment uses, comprising the following steps:
Step 1,30kg industry chlor-alkali film is taken, wherein perfluorinated sulfonic resin content about 83%, fiber content 17% are using concentration
35% hydrochloric acid cleans its surface, after it is rinsed with clear water；
Using concentration be 97% industrial alcohol to industrial chlor-alkali film surface carry out secondary cleaning, after rinsed with clear water；
Industrial chlor-alkali film is finally air-dried processing.
Step 2, industrial chlor-alkali film is cut with scissors broken.Using pulverizer, industrial chlor-alkali film is cut with scissors to the fritter of broken about 3cm × 3cm, mesh
The quick progress for being easy for subsequent technique.
Step 3, the broken industrial chlor-alkali film of 622.5kg organic solvent dimethylformamide and hinge is poured into reaction kettle,
Quality proportioning is 25:1.Wherein, axe temperature is 210 DEG C, and oil temperature is 240 DEG C, pressure 0.7Mpa, by the sulfonic acid on industrial chlor-alkali film
Resin is completely dissolved.
Step 4, slow water cooling thermal conductive oil pipeline, and then 45 DEG C of room temperature are cooled to, it slowly adjusts dropping valve and is depressurized to normal pressure.
Step 5, by filtering technique, the insoluble foreign matter no more than 20 microns is filtered out, such as fibrous foreign matter, until visually
Under the conditions of, stopping when not having insoluble substance in solution.
The mixed liquor of obtained perfluorinated sulfonic resin and dimethylformamide, obtained is that solion parameter and standard is not low
In: 5 wt% of concentration, 1000 g/eq of equivalent, 1.0 meq/g of acid capacity, 1.0 g/cm of density3。
Present disclosure, it is ensured that the consistency of correlation performance parameters, the repetition operability of preparation process.
Raw material is cheap industrial chlor-alkali film, and preparation process is simple and reliable, has practical application value.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (3)
1. a kind of preparation method of solion, which is characterized in that comprise the steps of:
Step 1, using the industrial chlor-alkali film containing perfluorinated sulfonic resin of recycling, using industrial alcohol, technical hydrochloric acid as cleaning
Liquid successively cleans industrial chlor-alkali film surface, and the visual foreign substance cleaning in surface is fallen；
Step 2, industrial chlor-alkali film is cut with scissors broken；
Step 3, the industrial chlor-alkali film and dimethylformamide organic solvents blended is added in reaction kettle, dimethylformamide
Dosage is added according to the content of perfluorinated sulfonic resin on industrial chlor-alkali film, and perfluorinated sulfonic resin and dimethylformamide press matter
Amount is than 1:17~25, and between 190 DEG C~240 DEG C, the temperature of reaction kettle is controlled 190 DEG C~210 the Oil-temperature control of reaction kettle
Between DEG C, the pressure of reaction kettle is controlled between 0.5Mpa~0.7Mpa, through high temperature pressure maintaining processing until industrial chlor-alkali film and diformazan
Base formamide is completely dissolved；
Step 4, after industrial chlor-alkali film and dimethylformamide are completely dissolved, its temperature is down to 30 DEG C~45 DEG C；
Step 5, the liquid in reaction kettle is filtered processing, prepared solion can be obtained.
2. the preparation method of solion as described in claim 1, which is characterized in that step 2 and the interchangeable sequence of step 1.
3. the preparation method of solion as described in claim 1, which is characterized in that after filtering technique, will be greater than 20
The insoluble foreign matter of micron is removed, until not having insoluble substance in solution under the conditions of visually.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910709858.8A CN110372889A (en) | 2019-08-02 | 2019-08-02 | A kind of preparation method of solion |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910709858.8A CN110372889A (en) | 2019-08-02 | 2019-08-02 | A kind of preparation method of solion |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699450A (en) * | 2005-05-13 | 2005-11-23 | 华东理工大学 | Process for preparing perfluorinated sulfonic resin solution by using waste perfluorinated ion membrane |
| CN1884352A (en) * | 2005-06-24 | 2006-12-27 | 大连新源动力股份有限公司 | Process for preparing perfluorinated sulfonic resin solution by using waste ion exchange membrane in chlor-alkali industry |
| CN103304945A (en) * | 2012-03-09 | 2013-09-18 | 陈铭 | Perfluorosulfonic acid ion exchange membrane and preparation method thereof |
| CN109824930A (en) * | 2019-02-15 | 2019-05-31 | 朝阳华鼎储能技术有限公司 | A kind of ion exchange membrane preparation method based on waste and old resin recovery technology |
-
2019
- 2019-08-02 CN CN201910709858.8A patent/CN110372889A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699450A (en) * | 2005-05-13 | 2005-11-23 | 华东理工大学 | Process for preparing perfluorinated sulfonic resin solution by using waste perfluorinated ion membrane |
| CN1884352A (en) * | 2005-06-24 | 2006-12-27 | 大连新源动力股份有限公司 | Process for preparing perfluorinated sulfonic resin solution by using waste ion exchange membrane in chlor-alkali industry |
| CN103304945A (en) * | 2012-03-09 | 2013-09-18 | 陈铭 | Perfluorosulfonic acid ion exchange membrane and preparation method thereof |
| CN109824930A (en) * | 2019-02-15 | 2019-05-31 | 朝阳华鼎储能技术有限公司 | A kind of ion exchange membrane preparation method based on waste and old resin recovery technology |
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Application publication date: 20191025 |
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