CN105664739A - Preparation method of highly hydrophilic polysulfone ultrafiltration membrane - Google Patents
Preparation method of highly hydrophilic polysulfone ultrafiltration membrane Download PDFInfo
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- CN105664739A CN105664739A CN201610040730.3A CN201610040730A CN105664739A CN 105664739 A CN105664739 A CN 105664739A CN 201610040730 A CN201610040730 A CN 201610040730A CN 105664739 A CN105664739 A CN 105664739A
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- graphene oxide
- ultrafiltration membrane
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
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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
- B01D2325/36—Hydrophilic membranes
Abstract
The invention discloses a preparation method of a highly hydrophilic polysulfone ultrafiltration membrane, comprising the following steps; evenly dispersing graphene oxide in a polar organic solvent by using ultrasound, adding polysulfone and an additive into an organic solution, dissolving and stirring to form uniform and stable casting solution, subjecting the casting solution to phase inversion on polyester nonwoven fabric through a wiping apparatus by using a phase inversion method to form a solid membrane, and finally preparing the highly hydrophilic polysulfone ultrafiltration membrane.The graphene oxide containing rich oxygen-containing functional groups such as carboxyl groups, hydroxyl groups and carbonyl groups are used as a modifying agent that is added into the polysulfone ultrafiltration membrane, thus changing inner pore structure of the polysulfone ultrafiltration membrane, reducing the angle of contact of the ultrafiltration membrane and significantly improving hydrophilicity of the modified polysulfone ultrafiltration membrane, the problems that the existing ultrafiltration membrane has poor hydrophilicity are overcome, and the preparation method has promising industrial application prospect.
Description
Technical field
The invention belongs to membrane for water treatment separation technology field, particularly to the preparation method of a kind of high-hydrophilic polysulphones hyperfiltration membrane.
Background technology
It is low that membrane separation technique has energy consumption, simple to operate, separation efficiency advantages of higher, as a kind of novel separation means, has been widely used in the industries such as medicine, food, biology, chemical industry, environmental protection. Membrane separation technique can be divided into microfiltration, ultrafiltration, nanofiltration and reverse osmosis according to aperture, and wherein hyperfiltration technique has concentration and purification efficiency is high, simple to operate and low power consumption and other advantages, is one of the focus of membrance separation area research both at home and abroad at present. The industrial application of ultrafiltration membrane technique is extensive, for instance, for field of biological pharmacy and the separation of food industry, concentration and purification, for wastewater treatment, for drinking water treatment etc.
The material category preparing ultrafilter membrane is various, can be divided into macromolecule member material and inorganic material film by character, wherein in the majority with macromolecule member material. The common used material preparing ultrafilter membrane has cellulose acetate, polysulfones, polyether sulfone, Kynoar, polyacrylonitrile etc. Polysulfones macromolecular material has rigidity and good toughness, creep-resistant property is excellent, heatproof, resistance to thermal oxide, inorganic acid resistance, alkali, saline solution corrosion, resistance to ionizing radiation, the advantage such as nontoxic, and polysulfones separating organic matters film has good water flux and cutoff performance, mechanical performance, chemical stability and heat stability, is widely used in the preparation of ultrafilter membrane. But, polysulphones hyperfiltration membrane hydrophilic in actual applications and anti-fouling performance are poor, it is easy to be contaminated, and cause water flux to decline, and reduce the service life of film. For this, it is possible to by improving masking technique, as added inorganic nanoparticles in material of preparing, it is intended to improve hydrophilicity and the antifouling property of polysulphones hyperfiltration membrane.
Graphene oxide is the oxide of Graphene, it it is powdered graphite product after chemical oxidation and stripping, include hydroxyl, carboxyl, carbonyl etc. containing abundant oxygen-containing functional group, there is excellent hydrophilicity, chemical stability and mechanical property, also have certain anti-microbial property. Therefore, select graphene oxide as polysulphones hyperfiltration membrane modifying agent, the polysulphones hyperfiltration membrane that a kind of graphene oxide of preparation is modified, addition due to graphene oxide, change the internal pore structure of polysulphones hyperfiltration membrane, reduce the contact angle of ultrafilter membrane, improve hydrophilicity and antifouling property.
Summary of the invention
It is an object of the invention to overcome the problem of existing ultrafilter membrane hydrophilicity difference, polysulphones hyperfiltration membrane is modified, it is provided that the preparation method of high-hydrophilic polysulphones hyperfiltration membrane, it is possible to well solve this problem. But work as the too large in size of graphene oxide, membrane aperture can be caused to block, cause that water flux declines, so the graphene oxide that should select suitable size is modifying agent.
The preparation method of a kind of high-hydrophilic polysulphones hyperfiltration membrane of the present invention. Specifically include following steps:
(1) graphene oxide ultrasound wave is scattered in polar organic solvent, form uniform and stable dispersion soln, then in dispersion soln, add polysulfones and additive, under 60-80 DEG C of condition, dissolve stirring, standing and defoaming, form uniform and stable casting solution, casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through pure water coagulation bath, occurs inversion of phases to generate solid film, the rinse bath that solid film sequentially passes through different water temperature subsequently cleans, and last rolling obtains high-hydrophilic polysulphones hyperfiltration membrane.
The thickness of above-mentioned graphene oxide is 0.5-5nm, and lateral dimension is 0.5-5 μm, and the number of plies is 1-10 layer.
Above-mentioned polar organic solvent is at least one in DMF, N,N-dimethylacetamide, dimethyl sulfoxide, N-Methyl pyrrolidone.
Above-mentioned additive is at least one in polyvinylpyrrolidone, Polyethylene Glycol, ethylene glycol monomethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether, diethylene glycol dimethyl ether.
The content of above-mentioned polysulfones is 10%-25%, and the content of graphene oxide is 0.01%-5%, and the content of additive is 5%-15%, and the content of polar organic solvent is 55%-84.99%.
The above-mentioned ultrasonic disperse time is 1-4h, and the stirring and dissolving time is 5-8h, and the standing and defoaming time is 12-24h.
The temperature of above-mentioned pure water coagulation bath is 5-25 DEG C, and rinse bath is 3, and rinse bath water temperature range is 10-75 DEG C.
The thickness of above-mentioned polyester non-woven fabric is 100 μm.
Beneficial effects of the present invention is as follows:
The present invention contains the feature of the oxygen-containing functional groups such as abundant carboxyl, hydroxyl, carbonyl by utilizing graphene oxide, add graphene oxide in polysulphones hyperfiltration membrane, to change the internal pore structure of polysulphones hyperfiltration membrane, reduce the contact angle of ultrafilter membrane, significantly improve the hydrophilicity of prepared polysulphones hyperfiltration membrane. The graphene oxide selecting suitable size joins in casting solution as modifying agent, improves the preparation technology of polysulphones hyperfiltration membrane, obtains the ultrafilter membrane with excellent hydrophilicity, be with a wide range of applications.
Accompanying drawing explanation
Fig. 1-4 respectively graphene oxide content is the contact angle figure of the high-hydrophilic polysulphones hyperfiltration membrane of 0%, 1%, 2% and 7%.
Detailed description of the invention
The specific embodiment of the present invention given below, is used for the present invention is further described, but is not limiting as the present invention.
The preparation method of a kind of high-hydrophilic polysulphones hyperfiltration membrane of the present invention, casting solution system is: membrane material selects polysulfones, material modified selection graphene oxide, and additive selects ethylene glycol monomethyl ether, and polar organic solvent selects DMF.
The preparation method of a kind of high-hydrophilic polysulphones hyperfiltration membrane of the present invention, casting solution system the ratio of each component is: the content of polysulfones is 10%-25%, the content of graphene oxide is 0.01%-5%, the content of ethylene glycol monomethyl ether is 5%-15%, N, the content of dinethylformamide is 55%-84.99%, and the content of above each component is all by weight percentage.
The preparation method of a kind of high-hydrophilic polysulphones hyperfiltration membrane of the present invention, its concrete preparation technology is:
Graphene oxide ultrasound wave is scattered in N, in dinethylformamide, ultrasonic dispersing time is 1-4h, form uniform and stable dispersion soln, ethylene glycol monomethyl ether is added in dispersion soln, it is uniformly mixed, polysulfones is slowly added in dispersion soln and forms feed liquid, then feed temperature is risen to 60-80 DEG C, continue stirring and dissolving 5-8h, standing and defoaming 12-24h subsequently, form uniform and stable casting solution, casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through the pure water coagulation bath of 5-25 DEG C, inversion of phases is occurred to generate solid film, solid film is sequentially passed through the rinse bath that water temperature is 10-70 DEG C, it is carried out, last rolling obtains high-hydrophilic polysulphones hyperfiltration membrane.
The contact angle of ultrafiltration diaphragm of the present invention adopts the test of contact angle tester, and the hydrophilicity of diaphragm can be reacted in film contact angle, and contact angle is more little, and hydrophilicity is more good.
The performance test methods of ultrafiltration diaphragm of the present invention is: diaphragm is placed under 0.15MPa pressure precompressed 30min, then measures the pure water flux of ultrafilter membrane under 0.1MPa pressure condition; Replace pure water as test fluid with the bovine serum albumin (BSA) of 0.1g/L, continue after precompressed 30min under 0.1MPa pressure, utilize ultraviolet spectrophotometer to measure the content of the BSA in now permeate, obtain the diaphragm rejection to BSA.
Embodiment 1
Graphene oxide (is selected Tangshan Jian Hua development in science and technology Co., Ltd, graphene oxide JH-, technical specification is: thickness is 0.5-4nm, lateral dimension is 0.5-3 μm, the number of plies is 1-10 layer) it is scattered in N with ultrasound wave, in dinethylformamide, ultrasound wave dispersion 2h, form uniform and stable dispersion soln, ethylene glycol monomethyl ether is added in dispersion soln, it is uniformly mixed, polysulfones is slowly added in dispersion soln and forms feed liquid, then feed temperature is risen to 80 DEG C, continue stirring and dissolving 6h, standing and defoaming 16h subsequently, form uniform and stable casting solution, the content of component described in casting solution is followed successively by: graphene oxide 1%, N, dinethylformamide 73%, ethylene glycol monomethyl ether 8%, polysulfones 18%.
Casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through the pure water coagulation bath of 18 DEG C, inversion of phases is occurred to generate solid film, solid film is sequentially passed through the rinse bath that water temperature is 25 DEG C and 60 DEG C, being carried out, last rolling obtains high-hydrophilic polysulphones hyperfiltration membrane. The contact angle of graphene oxide/polysulphones hyperfiltration membrane that the present embodiment provides is 63.175 ° after tested, and pure water flux is 320.4L/h m2, the rejection of BSA is maintained at more than 90%.
Embodiment 2
Graphene oxide (with embodiment 1) is scattered in N with ultrasound wave, in dinethylformamide, ultrasound wave dispersion 2h, form uniform and stable dispersion soln, ethylene glycol monomethyl ether is added in dispersion soln, it is uniformly mixed, polysulfones is slowly added in dispersion soln and forms feed liquid, then feed temperature is risen to 80 DEG C, continue stirring and dissolving 6h, standing and defoaming 16h subsequently, forms uniform and stable casting solution, and the content of component described in casting solution is followed successively by: graphene oxide 2%, N, dinethylformamide 72%, ethylene glycol monomethyl ether 8%, polysulfones 18%.
Casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through the pure water coagulation bath of 18 DEG C, inversion of phases is occurred to generate solid film, solid film is sequentially passed through the rinse bath that water temperature is 25 DEG C and 60 DEG C, being carried out, last rolling obtains high-hydrophilic polysulphones hyperfiltration membrane. The contact angle of graphene oxide/polysulphones hyperfiltration membrane that the present embodiment provides is 59.905 ° after tested, and pure water flux is 359.9L/h m2, the rejection of BSA is maintained at more than 90%.
Comparative example 1
Ethylene glycol monomethyl ether is joined N, in dinethylformamide, it is uniformly mixed, polysulfones is slowly added in dispersion soln and forms feed liquid, then feed temperature is risen to 80 DEG C, continue stirring and dissolving 6h, subsequently standing and defoaming 16h, form uniform and stable casting solution, the content of component described in casting solution is followed successively by: N, dinethylformamide 74%, ethylene glycol monomethyl ether 8%, polysulfones 18%.
Casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through the pure water coagulation bath of 18 DEG C, inversion of phases is occurred to generate solid film, solid film is sequentially passed through the rinse bath that water temperature is 25 DEG C and 60 DEG C, being carried out, last rolling obtains polysulphones hyperfiltration membrane. The contact angle of graphene oxide/polysulphones hyperfiltration membrane that the present embodiment provides is 71.24 ° after tested, and pure water flux is 224.0L/h m2, the rejection of BSA is maintained at more than 90%.
Comparative example 2
Graphene oxide (with embodiment 1) is scattered in N with ultrasound wave, in dinethylformamide, ultrasound wave dispersion 2h, form uniform and stable dispersion soln, ethylene glycol monomethyl ether is added in dispersion soln, it is uniformly mixed, polysulfones is slowly added in dispersion soln and forms feed liquid, then feed temperature is risen to 80 DEG C, continue stirring and dissolving 6h, standing and defoaming 16h subsequently, forms uniform and stable casting solution, and the content of component described in casting solution is followed successively by: graphene oxide 7%, N, dinethylformamide 67%, ethylene glycol monomethyl ether 8%, polysulfones 18%.
Casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through the pure water coagulation bath of 18 DEG C, inversion of phases is occurred to generate solid film, solid film is sequentially passed through the rinse bath that water temperature is 25 DEG C and 60 DEG C, being carried out, last rolling obtains polysulphones hyperfiltration membrane. The contact angle of graphene oxide/polysulphones hyperfiltration membrane that the present embodiment provides is 69.995 ° after tested, and pure water flux is 246.1L/h m2, the rejection of BSA is maintained at more than 90%.
Comparative example 3
The thickness selecting graphene oxide in this comparative example is 6-10nm, and lateral dimension is 6-10 μm, and the number of plies is 10-20 layer.
Graphene oxide ultrasound wave is scattered in N, in dinethylformamide, ultrasound wave dispersion 2h, form uniform and stable dispersion soln, ethylene glycol monomethyl ether is added in dispersion soln, it is uniformly mixed, polysulfones is slowly added in dispersion soln and forms feed liquid, then feed temperature is risen to 80 DEG C, continue stirring and dissolving 6h, standing and defoaming 16h subsequently, forms uniform and stable casting solution, and the content of component described in casting solution is followed successively by: graphene oxide 1%, N, dinethylformamide 73%, ethylene glycol monomethyl ether 8%, polysulfones 18%.
Casting solution is poured in the hopper scraping film device, casting solution forms liquid primary membrane through scraper on polyester non-woven fabric, through the pure water coagulation bath of 18 DEG C, inversion of phases is occurred to generate solid film, solid film is sequentially passed through the rinse bath that water temperature is 25 DEG C and 60 DEG C, being carried out, last rolling obtains polysulphones hyperfiltration membrane.Graphene oxide/polysulphones hyperfiltration membrane pure water flux that the present embodiment provides after tested is 227.5L/h m2, the rejection of BSA is maintained at more than 90%.
Form
By the comparison of the embodiment of the present application and comparative example it is apparent that pass through to add the graphene oxide of certain content scope, it is possible to be obviously improved the hydrophilicity of polysulphones hyperfiltration membrane. By above table it can be seen that when graphene oxide mass concentration is 1%-5%, the contact angle of modified polysulphone super-filter membrane is substantially less than 71.24 ° and 69.995 ° of comparative example, and pure water flux is significantly higher than the 224.0L/h m of comparative example2With 246.1L/h m2; By embodiment 1 and comparative example 3 it can be seen that when selecting graphene oxide larger in size, the ultrafilter membrane pure water flux of preparation is 227.5L/h m2, hence it is evident that lower than 320.4L/h m2。
Although the present invention has described that about exemplary, but the invention is not limited in described disclosed exemplary. Scope of the claims is consistent with the widest explanation to include this type of improvement all and equivalent structure and effect.
Claims (8)
1. the preparation method of a high-hydrophilic polysulphones hyperfiltration membrane, it is characterised in that be coated with one layer of polysulfones layer containing graphene oxide on polyester non-woven fabric, comprise the steps:
(1) graphene oxide ultrasound wave is scattered in polar organic solvent, forms dispersion soln;
(2) in the dispersion soln of step (1) gained, polysulfones and additive are added, after dissolving stirring, standing and defoaming, form uniform and stable casting solution;
(3) on polyester non-woven fabric surface, the casting solution of step (2) gained being formed liquid primary membrane through scraper, be then immersed in pure water coagulation bath, in coagulation bath tank, primary membrane generation inversion of phases generates solid film;
(4) rinse bath that the solid film of step (3) gained sequentially passes through 3 different temperatures cleans, and rolling obtains high-hydrophilic polysulphones hyperfiltration membrane.
2. method according to claim 1, it is characterised in that the thickness of described graphene oxide is 0.5-5nm, and lateral dimension is 0.5-5 μm, the number of plies is 1-10 layer.
3. method according to claim 1, it is characterised in that described polar organic solvent is at least one in DMF, N,N-dimethylacetamide, dimethyl sulfoxide and N-Methyl pyrrolidone.
4. method according to claim 1, it is characterised in that described additive is at least one in polyvinylpyrrolidone, Polyethylene Glycol, ethylene glycol monomethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether and diethylene glycol dimethyl ether.
5. method according to claim 1, it is characterized in that, the content of described graphene oxide is 0.01%-5%, the content of described polysulfones is 10%-25%, the content of described additive is 5%-15%, the content of described polar organic solvent is 55%-84.99%, and the gross weight of described graphene oxide, described polysulfones, described additive and described polar organic solvent is 100%.
6. method according to claim 1, it is characterised in that ultrasonic dispersing time is 1-4h, dissolved stirring time is 5-8h, and the standing and defoaming time is 12-24h.
7. method according to claim 1, it is characterised in that the temperature of described pure water coagulation bath is 5-25 DEG C, and the water temperature of described rinse bath ranges for 10-75 DEG C.
8. method according to claim 1, it is characterised in that described non-woven fabrics is polyester non-woven fabric, its thickness is 100 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108837716A (en) * | 2018-07-09 | 2018-11-20 | 广州暨环科技有限公司 | A kind of big flux modified polysulfone film and preparation method thereof |
| CN112638823A (en) * | 2018-08-24 | 2021-04-09 | 上海特瑞思材料科技有限公司 | Water filtration membrane device and method of making |
| CN112774468A (en) * | 2020-12-18 | 2021-05-11 | 任国峰 | Graphene polysulfone ultrafiltration membrane and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108837716A (en) * | 2018-07-09 | 2018-11-20 | 广州暨环科技有限公司 | A kind of big flux modified polysulfone film and preparation method thereof |
| CN112638823A (en) * | 2018-08-24 | 2021-04-09 | 上海特瑞思材料科技有限公司 | Water filtration membrane device and method of making |
| CN112638823B (en) * | 2018-08-24 | 2023-11-28 | 上海特瑞思材料科技有限公司 | Water filtration membrane device and preparation method |
| CN112774468A (en) * | 2020-12-18 | 2021-05-11 | 任国峰 | Graphene polysulfone ultrafiltration membrane and preparation method thereof |
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