CN105771704A - Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane - Google Patents
Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane Download PDFInfo
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- CN105771704A CN105771704A CN201610252921.6A CN201610252921A CN105771704A CN 105771704 A CN105771704 A CN 105771704A CN 201610252921 A CN201610252921 A CN 201610252921A CN 105771704 A CN105771704 A CN 105771704A
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- membrane
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- sulfonated polysulfone
- casting solution
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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
-
- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/22—Thermal or heat-resistance properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
-
- 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 novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane. The preparation method comprises the following steps: dissolving sulfonated polysulfone and tetrabutyl titanate into ethylene glycol monomethyl ether to prepare a membrane casting solution, coating the surface of a polysulfone ultrafiltration base membrane with the membrane casting solution, and then drying the surface under certain temperature to prepare the sulfonated polysulfone nanofiltration membrane. As sulfonated polysulfone serving as a membrane forming material contains a sulfonic acid group, the nanofiltration membrane is higher in anti-pollution property. The structure, the retention rate and the anti-pollution property of the membrane are adjusted according to the amounts of sulfonated polysulfone and tetrabutyl titanate which are added into the membrane casting solution and the drying temperature for membrane forming. The prepared sulfonated polysulfone nanofiltration membrane is higher in permeation selectivity and anti-pollution property; the membrane preparation method is simple and feasible, and has a good industrial application prospect.
Description
Technical field
The present invention relates to the preparation technology of NF membrane, specifically the preparation method of a kind of novel antipollution height selectivity SPSF NF membrane.
Background technology
Polysulfones is with its good chemical stability, resistance to water, thermostability, and good film property and mechanical strength, is widely used in membrance separation field.Polysulfone membrane has the advantages such as excellent permeability, higher mechanical strength, acid-proof alkaline, the close property of resistance to compression, stable chemical nature and pH be applied widely, but owing to polysulfone membrane itself belongs to hydrophobic material, the membrane aperture that film surface or fenestra internal adsorption, deposition cause diminishes or the fouling membrane phenomenon such as blocking, membrance separation ability is caused to decline, reduce membrane lifetime, constrain the film application in ultrafiltration field.Therefore, the performance of polysulfone material and polysulfone membrane has just been carried out big quantity research by people, and wherein the research of polysulfone membrane is concentrated mainly in the surface modification of film by people, and as blended, copolymerization and oxidation reaction etc. improve the hydrophilic of film, and then improve the resistance tocrocking of film.And the research of polysulfone material mainly through introducing hydrophilic group on polysulfones monomer, for instance sulfonic group, change the hydrophilic of film, and then affect structure and the resistance tocrocking of film.
SPSF is to introduce sulfonic group on polysulfones chain to be prepared from, therefore also just there is the premium properties of polysulfone material, such as chemically stable, resistance to water, excellent heat stability, and good film property and mechanical strength, simultaneously again due to sulfonic introducing, and there is good hydrophilic and resistance tocrocking.
Meanwhile, by improving rejection and the flux of SPSF NF membrane further at casting solution addition butyl titanate.Film adds nano-particle, it is possible to improve and optimize rejection and the flux of NF membrane, but directly add nano-particle and can make nanoparticle agglomerates, make the roughness on film surface and defect increase, make the antipollution of film reduce with rejection.And the butyl titanate added can slowly resolve into titania nanoparticles, it is possible to improve rejection and the flux of film, simultaneously because butyl titanate and solvent have good intermiscibility, it is possible to reduce agglomeration.
Summary of the invention
The preparation method that The present invention gives a kind of antipollution height selectivity SPSF NF membrane, the selectivity and the flux that are simultaneous for film improve further.
The present invention is achieved by the following technical programs:
The preparation method of a kind of novel antipollution height selectivity SPSF NF membrane, comprises the following steps:
Filmogen SPSF and butyl titanate are positioned in ethylene glycol monomethyl ether, stirring 2 hours at normal temperatures, form transparent casting solution, then casting solution is coated uniformly on polysulfones ultrafiltration counterdie, stand 10 minutes, then unnecessary casting solution is removed, then film is put into and baking oven is dried film forming under 30-60C.
Further, the mass fraction of SPSF is 0.05%-1.00%, and the mass fraction of butyl titanate is at 0.00%-0.70%.
This technique uses SPSF to be that filmogen prepares casting solution, and use butyl titanate is additive simultaneously, then adopts cladding process to prepare into antipollution height selectivity NF membrane at polysulfones ultrafiltration counterdie.SPSF is to introduce sulfonic group on the basis of polysulfone material to be prepared from, therefore polysulfone material premium properties is being inherited, such as high temperature resistant, resistance to oxidation, resistance to water and high film build, have again good clear water simultaneously, reduces the pollutant absorption on film surface, reduce fouling membrane, increase membrane lifetime.Butyl titanate can slowly resolve into titanium dioxide, therefore the selectivity that can improve film adding butyl titanate and permeation flux are changed, simultaneously because butyl titanate and solvent ethylene glycol monomethyl ether have the good compatibility, the agglomeration caused owing to being directly added into titania nanoparticles can be reduced, and then reduce film defect.
Detailed description of the invention
Below in conjunction with example, the present invention will be further described, but protection scope of the present invention is not limited to this:
Embodiment 1:
Being dissolved in glycol monoethyl ether by SPSF, mass fraction is 1.00%, stirs 2 hours with certain rotating speed at normal temperatures, make transparent casting solution, then being evenly coated at by casting solution on polysulfones ultrafiltration counterdie, room temperature staticly settles 10 minutes, then dries 10 minutes film forming under 50 degree.
Under the pressure of 1.2MPa, film is to magnesium chloride, magnesium sulfate, sodium chloride, and the rejection of sodium sulfate is as follows with permeation flux:
Embodiment 2:
Changing drying temperature during film forming, other steps are identical with embodiment 1.Under the pressure of 1.2MPa, film is to magnesium chloride, magnesium sulfate, sodium chloride, and the rejection of sodium sulfate is as follows with permeation flux:
Embodiment 3:
Changing the concentration of SPSF in casting solution, other steps are identical with embodiment 1.Under the pressure of 1.2MPa, film is to magnesium chloride, magnesium sulfate, sodium chloride, and the rejection of sodium sulfate is as follows with permeation flux:
Embodiment 4:
Changing over the casting solution sedimentation time in membrane process, other steps are identical with embodiment 1.Under the pressure of 1.2MPa, film is to magnesium sulfate, and sodium chloride rejection is as follows with permeation flux:
Embodiment 5
Changing over the drying time in membrane process, other steps are identical with embodiment 1.Under the pressure of 1.2MPa, film is to magnesium sulfate, and sodium chloride rejection is as follows with permeation flux:
Embodiment 6
SPSF and butyl titanate are dissolved in glycol monoethyl ether, their mass fraction respectively 0.70% and 0.35%, stir 2 hours with certain rotating speed at normal temperatures, make transparent casting solution, then casting solution is evenly coated on polysulfones ultrafiltration counterdie, room temperature staticly settles 10 minutes, then dries 10 minutes film forming under 50 degree.
Under the pressure of 1.2MPa, film is to magnesium chloride, magnesium sulfate, sodium chloride, and the rejection of sodium sulfate is as follows with permeation flux:
Embodiment 7
Changing the concentration of butyl titanate in casting solution, other steps are identical with embodiment 6, and under the pressure of 1.2MPa, film is to magnesium chloride, magnesium sulfate, sodium chloride, and the rejection of sodium sulfate is as follows with permeation flux:
Embodiment 8
Taking the concentration of SPSF in casting solution is 0.7%, butyl titanate respectively 0.0%, and it is as follows that the NF membrane of 0.35% and industry 270#, 90# finished film carry out antipollution experimental result:
Wherein the mass fraction of the SPSF of 161 and No. 153 samples is 0.70%, the mass fraction of butyl titanate respectively 0.00%, 0.35%, as seen from the above table, compare with finished industrial product film 270#, 90#, SPSF NF membrane has good resistance tocrocking, the stability of film is better, points out that butyl titanate is while increasing membrane flux, also can make the antifouling property of film have and slightly reduce simultaneously.
Claims (2)
1. a preparation method for novel antipollution height selectivity SPSF NF membrane, comprises the following steps:
Filmogen SPSF and butyl titanate are positioned in ethylene glycol monomethyl ether, stirring 2 hours at normal temperatures, form transparent casting solution, then casting solution is coated uniformly on polysulfones ultrafiltration counterdie, stand 10 minutes, then unnecessary casting solution is removed, then film is put into and baking oven is dried film forming under 30-60C.
2. the preparation method of a kind of novel antipollution height selectivity SPSF NF membrane as claimed in claim 1, it is characterised in that: the mass fraction of SPSF is 0.05%-1.00%, and the mass fraction of butyl titanate is at 0.00%-0.70%.
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| CN201610252921.6A CN105771704A (en) | 2016-04-22 | 2016-04-22 | Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane |
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| CN201610252921.6A CN105771704A (en) | 2016-04-22 | 2016-04-22 | Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106345316A (en) * | 2016-10-13 | 2017-01-25 | 潍坊学院 | Anti-sour corrosion micro-pore filter membrane |
| CN107158975A (en) * | 2017-06-01 | 2017-09-15 | 江苏天和制药有限公司 | A kind of positively charged nanofiltration membranes and preparation method thereof |
| CN109603207A (en) * | 2018-12-24 | 2019-04-12 | 广州中科检测技术服务有限公司 | A kind of wellability miillpore filter and the preparation method and application thereof for water-oil separating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103182252A (en) * | 2011-12-28 | 2013-07-03 | 中国科学院宁波材料技术与工程研究所 | Novel composite forward osmosis membrane and preparation method thereof |
| CN104258738A (en) * | 2014-09-28 | 2015-01-07 | 唐贵凤 | Forward osmosis organic-inorganic composite membrane and preparation method thereof |
| CN105038996A (en) * | 2015-07-24 | 2015-11-11 | 河南工程学院 | Nanofiber composite membrane reactor |
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2016
- 2016-04-22 CN CN201610252921.6A patent/CN105771704A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182252A (en) * | 2011-12-28 | 2013-07-03 | 中国科学院宁波材料技术与工程研究所 | Novel composite forward osmosis membrane and preparation method thereof |
| CN104258738A (en) * | 2014-09-28 | 2015-01-07 | 唐贵凤 | Forward osmosis organic-inorganic composite membrane and preparation method thereof |
| CN105038996A (en) * | 2015-07-24 | 2015-11-11 | 河南工程学院 | Nanofiber composite membrane reactor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106345316A (en) * | 2016-10-13 | 2017-01-25 | 潍坊学院 | Anti-sour corrosion micro-pore filter membrane |
| CN106345316B (en) * | 2016-10-13 | 2017-10-13 | 潍坊学院 | A kind of miillpore filter of acid-resisting corrosion |
| CN107158975A (en) * | 2017-06-01 | 2017-09-15 | 江苏天和制药有限公司 | A kind of positively charged nanofiltration membranes and preparation method thereof |
| CN109603207A (en) * | 2018-12-24 | 2019-04-12 | 广州中科检测技术服务有限公司 | A kind of wellability miillpore filter and the preparation method and application thereof for water-oil separating |
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Application publication date: 20160720 |