CN106283333B - A kind of electrolyte membrane, preparation method and the usage - Google Patents
A kind of electrolyte membrane, preparation method and the usage Download PDFInfo
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- CN106283333B CN106283333B CN201510264388.0A CN201510264388A CN106283333B CN 106283333 B CN106283333 B CN 106283333B CN 201510264388 A CN201510264388 A CN 201510264388A CN 106283333 B CN106283333 B CN 106283333B
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Abstract
The present invention relates to a kind of electrolyte membranes comprising fabric and the coating being overlying on fabric；The textile includes the polyphony thioether short fiber of the polyphenylene sulfide sulfone staple fiber and 0 70 parts by weight of 30 100 parts by weight；The coating is containing polyphenylene sulfide sulfone resinous coat or to contain polyflon coating.The present invention also provides the preparation methods of the electrolyte membrane, and its non-asbestos diaphragm application is used as in water electrolysis hydrogen producing, water electrolytic oxygen generating, chlor-alkali electrolytic cells, which improves heat resistance, are conducive to extend the service life of non-asbestos diaphragm, improve efficiency.
Description
Technical field
The present invention relates to a kind of diaphragm preparation methods more particularly to one kind for water electrolysis hydrogen producing to contain polyphenylene sulfide sulfone
Fiber or polyphenylene sulfide sulfone fiber and polyphenylene sulfide fibre mixed textile product contain a kind of polyphenylene sulfide sulfone or poly- four on textile
Vinyl fluoride coating, and the preparation method of thus obtained diaphragm.
Background technology
Water electrolysis hydrogen producing technology has had more than 200 years developing history, especially in recent decades, water electrolysis hydrogen producing
Technology has a great development.Water electrolysis hydrogen production method becomes one of the important means of mass production hydrogen in the world.Electrolysis water
The hydrogen and oxygen of generation are separated by the diaphragm in electrolytic cell, and the effect of diaphragm for electrolytic cell is to prevent the generation at electrolytic cell the two poles of the earth
Object mutually mixes, and its presence must not interfere the migration of ion between electrodes in solution.The performance of diaphragm is wanted
Ask as follows：(1) bubble should not penetrate；(2) it can be soaked by electrolyte, the ion in solution is enable smoothly to pass through；(3) there is foot
Enough mechanical strengths；(4) in the electrolytic solution not by alkali liquid corrosion, chemical stability is strong；(5) cheap, it is suitble to industrial
Extensive use.Previous diaphragm is usually made of asbestos, but since asbestos friction material is harmful, and pollutes environment, in the world
Most countries have disabled asbestos.For this purpose, some enterprises generally use textile made of polyphenylene sulfide fibre as diaphragm,
For water electrolysis hydrogen producing, related patents have 200710144822.7 etc..But the glass transition temperature of polyphenylene sulfide fibre only has 85-
90 DEG C, and the working temperature of water electrolysis hydrogen producing is most of from 80 DEG C or so original raisings to 90 DEG C or more, using polyphenylene sulfide
Diaphragm made of ether fiber works in 90 DEG C or more of solution for a long time, i.e., the glass transition temperature of polyphenylene sulfide fibre with
On, diaphragm has softened, and mechanical strength can be caused it in portion by large effect since polyphenylene sulfide heat resistance is insufficient
Divide the reduced service life under worst hot case.Or because under oxygen-enriched operating mode, under high temperature, oxygen is generated due to the unstable of SO keys
Change loses mechanical strength, to influence its effective utilization.
Invention content
Aiming at the above shortcomings existing in the prior art, technology to be solved by this invention is that polyphenylene sulfide is introduced in diaphragm
The material of ether sulfone makes its glass transition temperature be up to 215 DEG C due to introducing highly polar sulfuryl (- SO2-) in strand, and
And there is very excellent oxidative resistance and strength retention at high temperature, while the material still has excellent mechanics, resistance to
Chemical corrosivity, radiation hardness and anti-flammability etc..
Polyphenylene sulfide sulphone resin usually can be by preparing or buying acquisition, preparation method such as normal pressure anhydrous Na2S methods：
Under normal pressure, with 4,4 '-dichloro diphenyl sulfones (DCDPS) and anhydrous Na2S is that monomer is polymerize, using hexamethylphosphoramide
(HMPA) it is used as solvent with dimethylformamide (DMAC) volume ratio 1: 1, with sodium benzoate (NaCOOPh) and nitro paracide
For catalyst and auxiliary agent, 5h~6h is reacted.For another example high pressure anhydrous Na2S methods：The method is with anhydrous Na2S methods and DCDPS are monomer in height
It presses and carries out polycondensation reaction in kettle, with N-Methyl pyrrolidone (NMP) for solvent, 5h is reacted at 200 DEG C, catalyst system is with carboxylic acid
The effect of salt is preferable, and 20% or so that catalyst amount is DCDPS mass.Shanghai synthetic resin research institute, Sichuan University are
Obtain this kind of resin.Shanghai Qian Feng Fabritex S.r.l has used the resinoid in N-Methyl pyrrolidone (NMP) solution,
The staple fiber of 1.5D and 2D are obtained with wet spinning technology, intensity is in 2-4cN/dtex.
Polyphony thioether short fiber has also quantified to produce, and main supplier has toray company, Japanese Japan to spin company, four
River Deyang company etc., staple fiber product mainly have the cotton or medium-length staple fiber of 1.5D and 2D, and fibre strength is in 3-5cN/
dtex。
The present invention provides a kind of electrolyte membranes comprising fabric and the coating being overlying on fabric；
The textile includes the polyphenylene sulfide of the polyphenylene sulfide sulfone staple fiber and 0-70 parts by weight of 30-100 parts by weight
Staple fiber；
The coating is to contain polyphenylene sulfide sulphone resin or polyflon coating.
Preferably, the textile further includes the polytef flocks of 10-20 parts by weight.
Preferably, the polyphenylene sulfide sulfone staple fiber is preferably the 2D*51mm of Shanghai Qian Feng Fabritex S.r.l production
Polyphenylene sulfide sulfone staple fiber；The polyphony thioether short fiber is preferably the 2D*51mm or 1.5D*38mm of toray company production
Polyphony thioether short fiber；The polytef flocks are that the polytetrafluoroethylene (PTFE) of the 2D*51mm of DuPont Corporation's production is short
Fiber.
The present invention also provides the preparation methods of the electrolyte membrane comprising following steps：
(1) it by polyphenylene sulfide sulfone staple fiber and polyphony thioether short fiber, mixes, be combed into item, be spun by cotton blender machine
Yarn；
(2) fabric is made by loom in yarn；
(3) fabric is impregnated in the N methyl pyrrole network alkanone solution containing polyphenylene sulfide sulphone resin, is then passed through
200~250 DEG C of drying, or impregnate in the polytetrafluoroethylene (PTFE) aqueous emulsion containing polyphenylene sulfide sulphone resin, then pass through 120~
150 DEG C of drying, are made and contain cated electrolyte membrane.
It is preferred in the present invention,
Manufactured yarn described in step (1) is 6-60 English branch, further preferably 15-40 English branch.
Fabric described in step (2) can be plain cloth, twills or satin fabric.
The grammes per square metre of step (2) described fabric is every square metre 100 grams -1000 grams, further preferably every square metre 200
Grams -600 grams.
This field common process is may be used by the method that fabric is made in loom in yarn in step (2).Specifically
, Ke Yiwei：
By the polyphenylene sulfide sulfone staple fiber (weight percent 30-100%) of 2D*51mm with 2D*51mm's or 1.5D*38mm
Polyphony thioether short fiber (weight percent 0-70%) is sufficiently mixed by cotton blender machine, is then carded to item, using rove, carefully
The processes such as yarn, doubling and yarn steaming obtain 6-60 English count yarns.
It is knitted in arrow shaft with the technique of per inch 10--500 roots warp thread and per inch 10--500 root weft yarns using the yarn
On machine, by being woven according to the plain weave technique under on 1 time or 2 on 12, it is every square metre 100 grams -1000 grams to obtain grammes per square metre
Plain cloth；Or
By yarn with the technique of per inch 10--500 roots warp thread and per inch 10--500 root weft yarns, in rapier loom,
By being woven according to the twill technique under on 2 times 2 on 1 time 2 on 1 time or 3 on 11, obtain grammes per square metre be 100 grams every square metre-
1000 grams of twills；Or
By yarn with the technique of per inch 10--500 roots warp thread and per inch 10--500 root weft yarns, in rapier loom,
By being woven according to the satin weave technique under on 2 times 4 on 1 time or 4 on 43, it is every square metre 100 grams -1000 grams to obtain grammes per square metre
Satin fabric.
Step (3) by above-mentioned fabrics a concentration of 1~10% (weight percent) polyphenylene sulfide sulfone/N methyl pyrrole network alkane
It is impregnated in ketone solution 3~30 seconds, then passes through 200~250 DEG C of drying, drying time is 1~10 minute；Or above-mentioned fabrics are existed
It is impregnated in the aqueous emulsion of a concentration of 2~20% polyflon 3~30 seconds, then passes through 120~150 DEG C of drying, dry
The dry time is 1~10 minute.Obtain the separator fabrics containing coating (weight percent is 0.1~10%).
The present invention also provides the electrolyte membranes in water electrolysis hydrogen producing, water electrolytic oxygen generating, chlor-alkali electrolytic cells etc.
Purposes.
After the electrolyte membrane is cut growth * wide=(40~300cm) * (40~300cm), can directly by single layer or
Multilayer electrolyte membrane is fixed in the partition boards such as electrolysis hydrogen, and the diaphragm as water electrolysis hydrogen producing, water electrolytic oxygen generating, chlor-alkali electrolytic cells makes
With.
Compared with prior art, the present invention having the following advantages that：
After polyphenylene sulfide sulfone, compared with conventional polyphenylene sulfide fabric, heat resistance is obviously improved,
It is found by thermal aging test, when polyphenylene sulfide sulfone content reaches 30% or more, the heat resistance of fabric is promoted apparent.It is logical
Too fast speed heat burn-in test, fabric of the present invention improve 40% or more than the hot strength retention of polyphenylene sulfide fabric, the present invention
More suitable for the process conditions of electrolysis hydrogen, electrolysis oxygen or chloric alkali electrolysis under worst hot case, service life can carry substantially fabric
It is high.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
30 kilograms of the polyphenylene sulfide sulfone staple fiber of the 2D*51mm of Shanghai Qian Feng Fabritex S.r.l production is eastern with Japan
70 kilograms of the polyphony thioether short fiber of the 2D*51mm of beautiful company's production is sufficiently mixed by cotton blender machine, is then carded to item, then pass through
The processes such as rove, spun yarn, doubling and yarn steaming are crossed, 20 English is obtained and props up two strands.
Using the yarn, with the technique of per inch 69 warp thread and 48 weft yarns of per inch, in rapier loom, by pressing
It is woven according to the plain weave technique under on 11, obtains the plain cloth that the grammes per square metre of textile is 300 grams every square metre.
Above-mentioned fabrics are impregnated in polyphenylene sulfide sulfone/N methyl pyrrole network alkanone solution of a concentration of 2% (weight percent)
25 seconds, then pass through 250 DEG C of drying, drying time is to obtain within 5 minutes the diaphragm containing coating (weight percent 0.5%) to knit
Object.
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, four layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Embodiment 2
50 kilograms of the 1.5D*38mm polyphenylene sulfide sulfone staple fiber of Shanghai Qian Feng Fabritex S.r.l production is eastern with Japan
50 kilograms of the 1.5D*38mm polyphony thioether short fibers of beautiful company's production are sufficiently mixed by cotton blender machine, are then carded to item, then pass through
The processes such as rove, spun yarn, doubling and yarn steaming are crossed, 60 English is obtained and props up two strands.
Using the yarn, passed through in rapier loom with the technique of 120 warp thread of per inch and 80 weft yarns of per inch
It is woven according to the satin weave technique under on 41, obtains the satin fabric that the grammes per square metre of textile is 100 grams every square metre.
Above-mentioned fabrics are impregnated 15 seconds in the aqueous emulsion of a concentration of 5% polyflon, then pass through 130 DEG C
Drying, drying time are 2 minutes.Obtain the separator fabrics containing coating (weight percent 2%).
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, ten layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Embodiment 3
80 kilograms of the 1.5D*38mm polyphenylene sulfide sulfone staple fiber of Shanghai Qian Feng Fabritex S.r.l production is eastern with Japan
20 kilograms of the 1.5D*38mm polyphony thioether short fibers of beautiful company's production are sufficiently mixed by cotton blender machine, are then carded to item, then pass through
The processes such as rove, spun yarn, doubling and yarn steaming are crossed, 40 English is obtained and props up two strands.
Using the yarn, with the technique of per inch 76 warp thread and 42 weft yarns of per inch, in rapier loom, by pressing
It is woven according to the twill technique under on 31, obtains the twills that the grammes per square metre of textile is 200 grams every square metre.
Above-mentioned fabrics are impregnated 30 seconds in the aqueous emulsion of a concentration of 10% polyflon, then pass through 150
DEG C drying, drying time be 10 minutes.Obtain the separator fabrics containing coating (weight percent 5%).
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, five layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Embodiment 4
100 kilograms of the 2D*51mm polyphenylene sulfide sulfone staple fiber that Shanghai Qian Feng Fabritex S.r.l is produced, passes through comb
Cotton is then carded to item, using processes such as rove, spun yarn, doubling and yarn steamings, obtains 6 English and props up 6 strands.
Using the yarn, with the technique of inch 30 warp thread and 20 weft yarns of per inch, in rapier loom, by according to
Plain weave technique under 1 on 1 is woven, and the plain cloth that the grammes per square metre of textile is 1000 grams every square metre is obtained.
Above-mentioned fabrics impregnate in polyphenylene sulfide sulfone/N methyl pyrrole network alkanone solution of a concentration of 10% (weight percent)
30 seconds, then pass through 250 DEG C of drying, drying time is 10 minutes, obtains the diaphragm containing coating (weight percent 10%)
Fabric.
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, one layer of fabric is fixed in electrolytic hydrogen production equipment
It is used as diaphragm.
Embodiment 5
70 kilograms of the 2D*51mm polyphenylene sulfide sulfone staple fiber and toray that Shanghai Qian Feng Fabritex S.r.l is produced
30 kilograms of the 2D*51mm polyphony thioether short fibers of company's production are sufficiently mixed by cotton blender machine, item are then carded to, using thick
The processes such as yarn, spun yarn, doubling and yarn steaming obtain 16 English and prop up six strands.
Using the yarn, with the technique of per inch 54 warp thread and 36 weft yarns of inch, in rapier loom, by according to
Satin weave technique under 1 on 4 is woven, and the plain cloth that the grammes per square metre of textile is 600 grams every square metre is obtained.
Above-mentioned fabrics impregnate 30 in polyphenylene sulfide sulfone/N methyl pyrrole network alkanone solution of a concentration of 5% (weight percent)
Second, then pass through 250 DEG C of drying, drying time is 8 minutes, obtains the separator fabrics containing coating (weight percent 6%).
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, two layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Embodiment 6
By 70 kilograms of the 2D*51mm polyphenylene sulfide sulfone staple fiber of Shanghai Qian Feng Fabritex S.r.l production, toray
The polytetrafluoroethylene (PTFE) of 10 kilograms of the 2D*51mm polyphony thioether short fibers of company's production and the 2D*51mm of DuPont Corporation's production
20 kilograms of staple fiber is sufficiently mixed by cotton blender machine, is then carded to item, using processes such as rove, spun yarn, doubling and yarn steamings,
It obtains 16 English and props up six strands.
Using the yarn, with the technique of per inch 54 warp thread and 36 weft yarns of inch, in rapier loom, by according to
Satin weave technique under 1 on 4 is woven, and the plain cloth that the grammes per square metre of textile is 600 grams every square metre is obtained.
Above-mentioned fabrics impregnate 30 seconds in the aqueous emulsion of a concentration of 20% polyflon, then pass through 150 DEG C
Drying, drying time are 10 minutes, obtain the separator fabrics containing coating (weight percent 8%).
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, two layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Comparative example 1
The 1.5D*38mm polyphony thioether short fibers that toray company is produced are then carded to item by cotton carding, then
By processes such as rove, spun yarn, doubling and yarn steamings, obtains 40 English and prop up two strands.
Using the yarn, with the technique of per inch 76 warp thread and 42 weft yarns of per inch, in rapier loom, by pressing
It is woven according to the twill technique under on 31, obtains the twills that the grammes per square metre of textile is 200 grams every square metre.
Above-mentioned fabrics are impregnated 30 seconds in the aqueous emulsion of a concentration of 20% polyflon, then pass through 150
DEG C drying, drying time be 10 minutes.Obtain the separator fabrics containing coating (weight percent 8%).
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, five layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Comparative example 2
20 kilograms of the 2D*51mm polyphenylene sulfide sulfone staple fiber and toray that Shanghai Qian Feng Fabritex S.r.l is produced
80 kilograms of the 2D*51mm polyphony thioether short fibers of company's production are sufficiently mixed by cotton blender machine, item are then carded to, using thick
The processes such as yarn, spun yarn, doubling and yarn steaming obtain 16 English count yarns.
Using the yarn, with the technique of inch 54 warp thread and 36 weft yarns of inch, in rapier loom, by according to or
Satin weave technique under 1 on 4 is woven, and the plain cloth that the grammes per square metre of textile is 600 grams every square metre is obtained.
Above-mentioned fabrics impregnate 30 seconds in polyphenylene sulfide sulfone/N pyrrole network alkanone solution of a concentration of 10% (weight percent),
Then pass through 250 DEG C of drying, drying time is 10 minutes, obtains the separator fabrics containing coating (weight percent 10%).
Above-mentioned electrolyte membrane is cut into growth * wide=100cm*100cm, two layers of electrolyte membrane are fixed on electrolytic hydrogen production and are set
It is used as diaphragm for middle.
Test case
By Accelarated aging test at high temperature, the heat resistance of electrolyte membrane is evaluated.By embodiment 1-6 and comparative example
The electrolyte membrane sample of 1-2 uses GB/T3923.1 (textile fabric tensile property part 1 ultimate strength and jackknifing elongation
Test galley proof method) method test the tensile strength of its textile, then these electrolyte membranes are placed on to 220 DEG C of hot wind
Quick thermal aging test is carried out in baking oven, the testing time continues 240 hours, after heat ageing, uses GB/T3923.1 again
Method test electrolyte membrane fabric tension strength, after heat ageing electrolyte membrane fabric tension strength can decline, if
The strength retention of electrolyte membrane after heat treatment is high, shows that the heat resistance of the electrolyte membrane is good.
The fabric strength (N) before fabric strength (N)/heat treatment after strength retention (%)=heat treatment
The electrolyte membrane obtained by Examples 1 to 6 and comparative example 1~2, in 93 DEG C of operating temperatures, 30% hydrogen of electrolyte
Potassium oxide works under the electrolysis hydrogen operating mode of DC voltage 3V, DC current 750A, investigates above-mentioned various electrolyte membranes and meets (1)
Bubble should not penetrate (300 millimeter of water pressure cannot have bubble generation)；(2) it can be soaked by electrolyte, make the ion in solution
Can smoothly it pass through；(3) there are enough mechanical strengths (being more than 50N)；(4) in the electrolytic solution not by alkali liquid corrosion (alkali vector
2%) etc. less than under the conditions of, can continue working time.
Heat ageing strength retention and continuous working period contrast table
Claims (10)
1. a kind of electrolyte membrane, it is characterised in that：Including fabric and the coating being overlying on fabric；
Textile includes the polyphony thioether short fiber of the polyphenylene sulfide sulfone staple fiber and 0-70 parts by weight of 30-100 parts by weight；
The coating is to contain polyphenylene sulfide sulfone resinous coat.
2. electrolyte membrane as described in claim 1, it is characterised in that：Textile further includes the polytetrafluoro of 10-20 parts by weight
Ethylene staple fiber.
3. the preparation method of electrolyte membrane described in claim 1, which is characterized in that include the following steps：
（1）By polyphenylene sulfide sulfone staple fiber and polyphony thioether short fiber, by cotton blender machine mixing, it is combed into item, spinning resultant yarn
Line；
（2）Fabric is made by loom in yarn；
（3）The fabric is impregnated in the N methyl pyrrole network alkanone solution containing polyphenylene sulfide sulphone resin, then pass through 200 ~
250 DEG C of drying.
4. preparation method as claimed in claim 3, it is characterised in that：Step（1）In manufactured yarn be 6-60 English branch.
5. preparation method as claimed in claim 3, it is characterised in that：Step（2）Described in fabric can be plain cloth, tiltedly
Pattern fabric or satin fabric.
6. preparation method as claimed in claim 3, it is characterised in that：Step（2）The grammes per square metre of the fabric is every square metre 100
Grams -1000 grams.
7. preparation method as claimed in claim 3, it is characterised in that：The weight percent that the coating of the fabric accounts for fabric is
0.1~10%。
8. preparation method as claimed in claim 3, it is characterised in that：Step（3）The N methyl pyrroles containing polyphenylene sulfide sulfone
The weight percent of polyphenylene sulfide sulfone is 1-10% in network alkanone solution, and the time that fabric impregnates in the solution is 3 ~ 30 seconds, so
It is dried afterwards by 200 ~ 250 DEG C, drying time is 1 ~ 10 minute.
9. purposes of the electrolyte membrane as claimed in claim 1 or 2 in water electrolysis hydrogen producing, water electrolytic oxygen generating or chlor-alkali electrolytic cells.
10. purposes as claimed in claim 9, it is characterised in that：After the electrolyte membrane is cut into, directly by single layer or more
Layer electrolyte membrane is fixed in partition board, and the diaphragm as water electrolysis hydrogen producing, water electrolytic oxygen generating or chlor-alkali electrolytic cells uses.
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| CN108053818B (en) * | 2018-01-25 | 2021-11-02 | 上海钱丰纺织品有限公司 | Loudspeaker positioning support sheet and preparation method thereof |
| CN111979627B (en) * | 2020-05-12 | 2021-07-20 | 江苏百护纺织科技有限公司 | Flame-retardant yarn, fabric, garment and flame-retardant work garment |
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