CN110339734A - A kind of bipolar membrane and its novel processing step - Google Patents
A kind of bipolar membrane and its novel processing step Download PDFInfo
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- CN110339734A CN110339734A CN201910607237.9A CN201910607237A CN110339734A CN 110339734 A CN110339734 A CN 110339734A CN 201910607237 A CN201910607237 A CN 201910607237A CN 110339734 A CN110339734 A CN 110339734A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J43/00—Amphoteric ion-exchange, i.e. using ion-exchangers having cationic and anionic groups; Use of material as amphoteric ion-exchangers; Treatment of material for improving their amphoteric ion-exchange properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/42—Ion-exchange membranes
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Abstract
The present invention provides a kind of bipolar membrane and its novel processing step, using unique bipolar membrane preparation process, prepare raw material and process, it is initially formed cation-exchange membrane by impregnation, polymerization, sulfonation, then single side chlorination and quaternized obtained bipolar membrane are successively carried out to cation-exchange membrane by thionyl chloride.The in-between product of the novel processing step bipolar membrane produced can be directly as cation-exchange membrane, bipolar membrane is generated by continuing chlorination and quaternization reaction on molding cation-exchange membrane, greatly reduce the cost of manufacture of bipolar membrane, shorten processing step, also avoid having virose methylation procedure simultaneously, simplify preparation process, reduce technologic complexity, preparation efficiency is improved, a kind of novel processing step of the bipolar membrane of environmentally friendly low-cost high-efficiency is formed.Meanwhile bipolar membrane made from the novel processing step is significantly better than traditional bipolar membrane in performance parameter.
Description
Technical field
The invention belongs to separation membrane technical fields, more particularly, to a kind of bipolar membrane and its novel processing step.
Background technique
As electroosmose process prepares drinking water in seawater and brackish water desalination, organic compound desalting and purifying, at industrial wastewater
Reason such as recycles to be widely used at the fields, research and innovation to amberplex be increasingly becoming this method development core and
Hot spot.
Existing well-known bipolar membrane preparation method is United States Patent (USP) US4, uses polyethylene disclosed in 024,043
Film is the preparation method of the bipolar membrane of counterdie.The method is using density polyethylene film with high, and ultra-high molecular weight polyethylene is thin
Film is basilar memebrane, immersion styrene, in the solution of divinylbenzene (crosslinking agent) and benzoyl peroxide (initiator) composition,
It impregnates 10 minutes to 1 hour, takes out under 70-90 DEG C of high temperature, two sides presss from both sides aluminium foil, is subsequently sandwiched between two blocks of plate glass, it pressurizes,
Heating polymerize to obtain basement membrane.Polystyrene content in basement membrane is in 15%-45% range.Then basement membrane two sides is subjected to sulphur respectively
Change, bipolar membrane is made in chloromethylation and amination.But bipolar membrane impregnation rate is made for this method and exchange capacity is not high, surface resistance
It is higher.
CN102061004B discloses a kind of preparation method of bipolar membrane, uses polyethylene and ethylene and octene copolymer
The alloy film or polyethylene and ethylene and octene copolymer elastomer and Oppanol tertiary blending that elastomer binary is blended
Alloy film do basilar memebrane；Basilar memebrane is immersed in styrene, in the solution of divinylbenzene and benzoyl peroxide, impregnation film is added
Pressure, heating polymerize to obtain basement membrane；Basement membrane is methylated to obtain chloromethane basement membrane in the chloromethyl ether Chlorine in Solution containing anhydrous stannic chloride, then
Chloromethane basement membrane is quaternized in trimethylamine aqueous solution, obtain bipolar membrane.This method compensates for US4, lacking in 024,043 method
It falls into, but two methods have used chloromethane ethereal solution to carry out methylation reaction, need to carry out respectively with basement membrane two sides during preparation
Reaction, not only step is many and diverse, but also preparation cost is high, and coefficient of injury is big, and bipolar membrane performance obtained, which there is no, obviously to be changed
It is kind.
Summary of the invention
The first purpose of this invention is, provides a kind of novel processing step of bipolar membrane, novel method production
At low cost, simple process, Operating Complexity and danger coefficient are low, and the bipolar membrane of preparation not only during the preparation process can be simultaneously
Output cation-exchange membrane, and have higher exchange capacity and more low areal resistance.
For this purpose, above-mentioned purpose of the invention is achieved through the following technical solutions:
A kind of novel processing step of bipolar membrane, the novel processing step of the bipolar membrane include:
By basilar memebrane containing being immersed in the solution of styrene, divinylbenzene and initiator, so that the monomer in solution immerses film
It is interior；
By after impregnation basilar memebrane pet film or sheet material covering step up, and heated
Pressure polymerization；
Basilar memebrane after polymerization is heated to sulfonation in the concentrated sulfuric acid or chlorosulfonic acid to get cation-exchange membrane is arrived；
By cation-exchange membrane when containing being immersed in the ion for carrying out chlorination when chlorination obtains in thionyl chloride
Film；
The one side of above-mentioned ionic membrane chlorination is contained to be immersed in amine aqueous solution and carries out quaternization reaction to get positive to having
The bipolar membrane of facial mask and back film.
The present invention by adopting the above technical scheme while, can also use or combine using following technical scheme:
As the preferred technical solution of the present invention, the basilar memebrane is polyvinyl chloride film or polypropylene phenylethylene bullet
Property body binary blend film.
As the preferred technical solution of the present invention, the polyvinyl chloride film is blended with plasticizer for Corvic and squeezes
Film out, plasticizer are o-phthalic acid dibutyl ester, and the mass ratio of Corvic and plasticizer is 100:20-45；
The polypropylene styrenic elastomer binary blend film is that PP GRANULES or powder and styrenic elastomer particle are total
It is mixed, and PP GRANULES or content of powder are 20-80%.
As the preferred technical solution of the present invention, in the solution of the styrene, divinylbenzene and initiator, styrene is used
The mass percent of amount is 60-95%, and the mass percent of divinylbenzene dosage is 4.5-35%.
As the preferred technical solution of the present invention, the initiator be benzoyl peroxide or dilauroyl peroxide, and
Mass percent is 0.5-5%.
As the preferred technical solution of the present invention, basilar memebrane, which contains, to be immersed in the solution of styrene, divinylbenzene and initiator
Temperature be 20-65 DEG C, impregnation the time be 0.5-10 hours.
As the preferred technical solution of the present invention, by after impregnation basilar memebrane pet film or
The heating pressure polymerization that carries out after sheet material covering steps up, polymerization temperature are 70-160 DEG C, polymerization pressure 0.1-5bar, when polymerization
Between be 4-16 hours.
As the preferred technical solution of the present invention, heat in sulfonating reaction: sulfonation temperature is 60-90 DEG C, time 4-14
Hour.
As the preferred technical solution of the present invention, the temperature of the chlorination is 25-70 DEG C, and the time is 2-8 hours.
As the preferred technical solution of the present invention, the amine aqueous solution is trimethylamine, dimethylamine, triethylamine, tripropyl amine (TPA)
Or the aqueous solution that one or more of triethylene diamine is combined, the mass concentration of the amine aqueous solution are 10-40%.
As the preferred technical solution of the present invention, the temperature of quaternary ammonium reaction is 40-120 DEG C, reaction time 0.5-12
Hour.
A further object of the invention is, is based on above-mentioned novel processing step, provides a kind of bipolar membrane.
For this purpose, above-mentioned purpose of the invention is achieved through the following technical solutions:
A kind of bipolar membrane, the bipolar membrane are obtained as prepared by the novel processing step of previously described bipolar membrane
It arrives.
The present invention provides a kind of bipolar membrane and its novel processing step, using unique bipolar membrane preparation process, system
Standby raw material and process are initially formed cation-exchange membrane by impregnation, polymerization, sulfonation, then are exchanged by thionyl chloride cation
Film successively carries out single side chlorination and quaternized obtained bipolar membrane.The novel processing step bipolar membrane produced is in-between
Product can be directly as cation-exchange membrane, by continuing chlorination and quaternization reaction on molding cation-exchange membrane
Bipolar membrane is generated, the cost of manufacture of bipolar membrane is greatly reduced, shortens processing step, while also avoiding that there is poison
The methylation procedure of property, simplifies preparation process, reduces technologic complexity, improve preparation efficiency, form a kind of ring
Protect the novel processing step of the bipolar membrane of low-cost high-efficiency.Meanwhile bipolar membrane made from the novel processing step is in property
Traditional bipolar membrane can be significantly better than in parameter.
Specific embodiment
The present invention is described in further detail referring to specific embodiment.
Embodiment 1
The preparation-obtained polyvinyl chloride basilar memebrane of rolling process for being 100:35 by Corvic and plasticizer proportions
Film contains the solution for being immersed in styrene, divinylbenzene and initiator, and wherein initiator is benzoyl peroxide；Styrene, divinyl
Benzene and benzoyl peroxide mass ratio are 85:10:2；Being impregnated with temperature is 40 DEG C, and the impregnation time is 2 hours.
It is put into air dry oven after basilar memebrane after impregnation is stepped up with the covering of polyethylene terephthalate sheet material
Heating polymerization, polymerization temperature are 90 DEG C, and polymerization time is 8 hours, take out, are washed with deionized after the reaction was completed；Then will
It is impregnated with carries out sulfonation in concentrated sulfuric acid, and sulfonation temperature is 70 DEG C, and sulfonation time is to obtain cation-exchange membrane in 6 hours, after taking-up
It will wherein be impregnated on one side in thionyl chloride liquid and carry out chlorination, reaction temperature is 50 DEG C, and the reaction time is to take out for 8 hours
Clean, and the face be placed in 40% trimethylamine aqueous solution, impregnation temperature is 80 DEG C, and the impregnation time is 1 hour, can obtain it is negative from
Sub- 0.8 milliequivalent of exchange capacity/gram dry film, 1.7 milliequivalent of cation exchange capacity/gram dry film, transmembrane voltage 1.5V's
Bipolar membrane.
Embodiment 2
The calendering basilar memebrane of polypropylene and styrenic elastomer mass ratio 70:30 are contained and are immersed in styrene, divinyl
The solution of benzene and initiator, wherein initiator is benzoyl peroxide；Styrene, divinylbenzene and benzoyl peroxide mass ratio
For 80:10:1；Being impregnated with temperature is 40 DEG C, and the impregnation time is 2 hours.
It is put into air dry oven after basilar memebrane after impregnation is stepped up with the covering of polyethylene terephthalate sheet material
Heating polymerization, polymerization temperature are 80 DEG C, and polymerization time is 10 hours, take out, are washed with deionized after the reaction was completed；Then will
It is impregnated with carries out sulfonation in concentrated sulfuric acid, and sulfonation temperature is 80 DEG C, and sulfonation time is to obtain cation-exchange membrane in 8 hours, after taking-up
It will wherein be impregnated on one side in thionyl chloride liquid and carry out chlorination, reaction temperature is 60 DEG C, and the reaction time is to take out for 4 hours
It cleans, and the face is placed in 30% trimethylamine and dimethylamine mixed aqueous solution, trimethylamine and dimethylamine mass ratio are 5:1,
Being impregnated with temperature is 70 DEG C, and the impregnation time is 3 hours, can obtain 1.1 milliequivalent of anion-exchange capacity/gram dry film, and cation is handed over
Change 2.0 milliequivalent of capacity/gram dry film, the bipolar membrane of transmembrane voltage 1.4V.
Embodiment 3
The rolling process polyvinyl chloride basilar memebrane film that Corvic and plasticizer proportions are 100:45 is contained and is immersed in benzene second
The solution of alkene, divinylbenzene and initiator, wherein initiator is benzoyl peroxide；Styrene, divinylbenzene and benzoyl peroxide
Formyl mass ratio is 100:10:1；Being impregnated with temperature is 40 DEG C, and the impregnation time is 2 hours.
It is put into air dry oven after basilar memebrane after impregnation is stepped up with the covering of polyethylene terephthalate sheet material
Heating polymerization, polymerization temperature are 110 DEG C, and polymerization time is 6 hours, take out, are washed with deionized after the reaction was completed；Then will
Wherein one side impregnation carries out sulfonation in concentrated sulfuric acid, and sulfonation temperature is 90 DEG C, and sulfonation time is to obtain cation-exchange membrane in 10 hours,
It will be wherein impregnated on one side in thionyl chloride liquid after taking-up and carry out chlorination, reaction temperature is 65 DEG C, and the reaction time is 2 small
When take out and clean, and the face is placed in 40% trimethylamine and dimethylamine mixed aqueous solution, trimethylamine and dimethylamine mass ratio
For 5:3, being impregnated with temperature is 60 DEG C, and the impregnation time is 6 hours, can obtain 0.9 milliequivalent of anion-exchange capacity/gram dry film, sun
1.9 milliequivalent of ion exchange capacity/gram dry film, the bipolar membrane of transmembrane voltage 1.7V.
Embodiment 4
For operating procedure with embodiment 2, the chlorination time is 6 hours, and other conditions are with embodiment 2 to get arriving
1.1 milliequivalent of anion-exchange capacity/gram dry film, 2.0 milliequivalent of cation exchange capacity/gram dry film, transmembrane voltage drop
The bipolar membrane of 1.4V.
Embodiment 5
For operating procedure with embodiment 2, the chlorination time is 8 hours, and other conditions are with embodiment 2 to get arriving
1.1 milliequivalent of anion-exchange capacity/gram dry film, 2.0 milliequivalent of cation exchange capacity/gram dry film, transmembrane voltage drop
The bipolar membrane of 1.4V.
Embodiment 6
One side of the cation-exchange membrane after chloro is contained with embodiment 2 and is immersed in 70 DEG C of amine aqueous solutions by operating procedure
In 1 hour, other conditions with embodiment 4 to get arrive 1.0 milliequivalent of anion-exchange capacity/gram dry film, cation exchange
The bipolar membrane of 1.4V drops in 1.8 milliequivalent of capacity/gram dry film, transmembrane voltage.
Embodiment 7
One side of the cation-exchange membrane after chloro is contained with embodiment 2 and is immersed in 35 DEG C of amine aqueous solutions by operating procedure
In 5 hours, other conditions with embodiment 4 to get arrive 0.9 milliequivalent of anion-exchange capacity/gram dry film, cation exchange
The bipolar membrane of 1.3V drops in 1.8 milliequivalent of capacity/gram dry film, transmembrane voltage.
Embodiment 8
Operating procedure with embodiment 2, by the basilar memebrane after impregnation in 80 DEG C of baking oven pressure polymerization 6 hours, other
With embodiment 2 to get 0.7 milliequivalent of anion-exchange capacity/gram dry film is arrived, 1.4 milligrams of cation exchange capacity are worked as part
The bipolar membrane of 1.8V drops in amount/gram dry film, transmembrane voltage.
Embodiment 9
Operating procedure with embodiment 2, by the basilar memebrane after impregnation in 80 DEG C of baking oven pressure polymerization 4 hours, other
With embodiment 2 to get 0.6 milliequivalent of anion-exchange capacity/gram dry film is arrived, 1.3 milligrams of cation exchange capacity are worked as part
The bipolar membrane of 1.9V drops in amount/gram dry film, transmembrane voltage.
Embodiment 10
Operating procedure with embodiment 6, by the basilar memebrane after impregnation in 90 DEG C of baking oven pressure polymerization 6 hours, other
With embodiment 6 to get 0.9 milliequivalent of anion-exchange capacity/gram dry film is arrived, 1.6 milligrams of cation exchange capacity are worked as part
The bipolar membrane of 1.3V drops in amount/gram dry film, transmembrane voltage.
Table 1 shows reference example and obtains to prepared by the major parameter of preparation method in embodiment 1-10 and corresponding embodiment
The characterization result of the film arrived.
Table 1
The data of reference example are derived from embodiment 5 in Chinese patent CN102061004B in table, compare reference example and embodiment
The characterization parameter that 1-10 can be seen that film prepared by embodiment 1-10 is superior to or is bordering on parameter shown in reference example.From above-mentioned
Embodiment 1-3, which can be seen that embodiment 2, can be obtained the relatively good bipolar membrane of effect, carry out single argument pair according to embodiment 2
Than experiment, detailed in Example 4-10.Referring to embodiment 2 and embodiment 4-5, it can be found that: the lengthening of chloro time is to film properties
Parameter influences smaller；Comparative example 4,6-7 can be seen that the quaternization reaction time shortens or reduce quaternized temperature, ionic membrane
Parameter has downward trend；Comparative example 2 and embodiment 8-10, it is found that polymerization time shortens, ion exchange capacity meeting
It reduces, transmembrane voltage drop will increase, and polymerization temperature increases, and ion exchange capacity and transmembrane voltage drop can all reduce.
Above-mentioned specific embodiment is used to illustrate the present invention, is merely a preferred embodiment of the present invention, rather than to this
Invention is limited, and within the spirit of the invention and the scope of protection of the claims, to any modification of the invention made, is equal
Replacement, improvement etc., both fall within protection scope of the present invention.
Claims (10)
1. a kind of novel processing step of bipolar membrane, it is characterised in that: the novel processing step of the bipolar membrane includes:
By basilar memebrane containing being immersed in the solution of styrene, divinylbenzene and initiator, so that the monomer in solution immerses in film；
By after impregnation basilar memebrane pet film or sheet material covering step up, and carry out heating pressurization
Polymerization；
Basilar memebrane after polymerization is heated to sulfonation in the concentrated sulfuric acid or chlorosulfonic acid to get cation-exchange membrane is arrived；
By cation-exchange membrane when containing being immersed in the ionic membrane for carrying out chlorination when chlorination obtains in thionyl chloride；
The one side of above-mentioned ionic membrane chlorination is contained to be immersed in amine aqueous solution and carries out quaternization reaction to get to sunny side film
With the bipolar membrane of back film.
2. the novel processing step of bipolar membrane according to claim 1, it is characterised in that: the basilar memebrane is polychlorostyrene second
Alkene film or polypropylene styrenic elastomer binary blend film.
3. the novel processing step of bipolar membrane according to claim 2, it is characterised in that: the polyvinyl chloride film is
The film of Corvic and plasticizer blending extrusion；The polypropylene styrenic elastomer binary blend film is poly- third
Alkene particle or powder are blended with styrenic elastomer particle, and PP GRANULES or content of powder are 20-80%.
4. the novel processing step of bipolar membrane according to claim 1, it is characterised in that: the styrene, divinyl
In the solution of benzene and initiator, the mass percent of styrene dosage is 60-95%, and the mass percent of divinylbenzene dosage is
4.5-35%.
5. the novel processing step of bipolar membrane according to claim 1 or 4, it is characterised in that: the initiator was
Benzoyl Oxide or dilauroyl peroxide, and mass percent is 0.5-5%.
6. the novel processing step of bipolar membrane according to claim 1, it is characterised in that: basilar memebrane, which contains, is immersed in benzene second
Temperature in the solution of alkene, divinylbenzene and initiator is 20-65 DEG C, and the impregnation time is 0.5-10 hours.
7. the novel processing step of bipolar membrane according to claim 1, it is characterised in that: use the basilar memebrane after impregnation
The heating pressure polymerization that pet film or sheet material covering carry out after stepping up, polymerization temperature 70-160
DEG C, polymerization pressure 0.1-5bar, polymerization time is 4-16 hours.
8. the novel processing step of bipolar membrane according to claim 1, it is characterised in that: the temperature of the chlorination
It is 25-70 DEG C, the time is 2-8 hours.
9. the novel processing step of bipolar membrane according to claim 1, it is characterised in that: the amine aqueous solution is three
The combined aqueous solution of one or more of methylamine, dimethylamine, triethylamine, tripropyl amine (TPA) or triethylene diamine, the amine water
The mass concentration of solution is 10-40%.
10. a kind of bipolar membrane, it is characterised in that: the bipolar membrane by bipolar membrane described in claim 1 novel system
It is obtained prepared by Preparation Method.
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Application publication date: 20191018 |