CN108043234A - The preparation method of ultrafiltration membrane - Google Patents
The preparation method of ultrafiltration membrane Download PDFInfo
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- CN108043234A CN108043234A CN201711363973.1A CN201711363973A CN108043234A CN 108043234 A CN108043234 A CN 108043234A CN 201711363973 A CN201711363973 A CN 201711363973A CN 108043234 A CN108043234 A CN 108043234A
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- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to material chemistry technical fields, and in particular to a kind of preparation method of ultrafiltration membrane.Include the raw material of following mass percent：10 25wt% of polyether sulfone, 15 30wt% of interworking perforating agent, 1 5wt% of inorganic additive, 50 70wt% of solvent；Ultrafiltration membrane acid and alkali-resistance produced by the present invention, high throughput.
Description
Technical field
The invention belongs to material chemistry technical fields, and in particular to a kind of preparation method of ultrafiltration membrane.
Background technology
Ultrafiltration is using pressure as one of membrane separation technique of motive force, has the characteristics that efficient, low energy consumption, is led in water process
Domain has a wide range of applications.Polyether sulfone is a kind of polymeric film material for being usually used in preparing ultrafiltration membrane, and glass transition temperature reaches
225 DEG C, there is excellent heat-resisting, acid and alkali-resistance, pressure-resistant performance.At present, due to being limited be subject to technology and raw material, in the market
Poly (ether-sulfone) ultrafiltration membrane largely limits its application industrially there are the defects of flux is low, acidproof alkaline error.
The content of the invention
It is an object of the invention to provide the preparation methods of a kind of acid and alkali-resistance, high-throughput ultrafiltration membrane.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of ultrafiltration membrane, includes the following steps：
(1) at 70-80 DEG C, polyether sulfone is added in into solvent, first stirring to solution is clarified；Then interworking pore is added in
Agent and inorganic additive at 50-60 DEG C, are again stirring for formation homogeneous phase solution；
(2) vacuum defoamation processing is carried out to homogeneous phase solution, obtains casting solution；
(3) membrane is made in casting solution and non-woven fabrics, membrane is successively by standing, deionized water solidification in air environment
Curing, deionized water impregnate and dry processing in bath, obtain ultrafiltration membrane；
The composition of above-mentioned each raw material is as follows：Polyether sulfone 10-25wt%, interworking perforating agent 15-30wt%, inorganic additive 1-
5wt%, solvent 50-70wt%.
In the above-mentioned technical solutions, resistance to acid and alkali can be increased using inorganic additive and improves membrane flux；Deionization water logging
Bubble is to guarantee to remove pore-foaming agent completely.Applicant of the present invention is shown by long-term experimental study and verification result：
Ultrafiltration membrane uniform pore diameter, flux height, the stability being prepared using more than raw material and method are good, suitable for high viscosity, Gao Gu
Contain, the system of pH=1-14.Preparation method provided by the invention is simple, and operation is easy, and environmental requirement is low, favorable repeatability, fits
For industrialized production.
The composition and content of interworking pore-foaming agent are very big on the flux influence of ultrafiltration membrane, preferably, the interworking pore-foaming agent
According to mass ratio it is 1-2 by polyvinylpyrrolidone and polyethylene glycol：2-1 is mixed.
Preferably, the molecular weight of the polyethylene glycol is 1000-10000.
Preferably, the molecular weight of the polyvinylpyrrolidone is 38000-600000.
For increase resistance to acid and alkali and improve membrane flux, the inorganic additive for silica, titanium dioxide, lithium chloride,
Any one in zinc chloride.
Preferably, the solvent is n,N-Dimethylformamide, n,N-dimethylacetamide, N-Methyl pyrrolidone, two
One or two kinds of compositions in methyl sulfoxide.
Preferably, first in the step (1) and be again stirring for rate as 300-500r/min, first mixing time is 2-
4h；The time is again stirring for as 1-3h.
Preferably, the polypropylene non-woven fabric or polyphenylene sulfide nonwoven that non-woven fabrics selects resistance to acid and alkali good in the step (3)
Cloth.
Specific embodiment
1-4 is further described technical solution disclosed by the invention with reference to embodiments.
Embodiment 1：The preparation of ultrafiltration membrane
(1) each raw material is weighed by following mass percent：Polyether sulfone 20wt%, n,N-dimethylacetamide 47wt%, point
Son amount is 38000 kollidon 15wt%, and molecular weight is 1000 polyethylene glycol 15wt%, zinc chloride 3wt%；
(2) at 75 DEG C, polyether sulfone is added in into n,N-dimethylacetamide, 3h is stirred under the rotating speed of 400r/min,
It is clarified to solution；Then kollidon, polyethylene glycol and zinc chloride are added in, 3h is stirred at 50 DEG C, until being formed homogeneous
Solution；
(3) at 40 DEG C, vacuum defoamation processing 1h is carried out to homogeneous phase solution, obtains casting solution；
(4) membrane is made in casting solution and polypropylene non-woven fabric on film applicator, membrane is placed on 25-30 DEG C of temperature, wet
It spends in the air of 70-80% and stands 2-3min, then be transferred in deionized water coagulating bath and cure, deionized water immersion, finally dry,
Obtain ultrafiltration membrane.
Embodiment 2：The preparation of ultrafiltration membrane
(1) each raw material is weighed by following mass percent：Polyether sulfone 10wt%, n,N-dimethylacetamide 31wt%, two
Methyl sulfoxide 31wt%, molecular weight are 21600 kollidon 12wt%, and molecular weight is 2000 polyethylene glycol
12wt%, silica 4wt%；
(2) at 80 DEG C, polyether sulfone is added in into the mixed liquor of n,N-dimethylacetamide and dimethyl sulfoxide (DMSO),
4h is stirred under the rotating speed of 300r/min, until solution is clarified；Then kollidon, polyethylene glycol and silica are added in,
3h is stirred at 60 DEG C, until forming homogeneous phase solution；
(3) at 50 DEG C, vacuum defoamation processing 2h is carried out to homogeneous phase solution, obtains casting solution；
(4) membrane is made in casting solution and polyphenylene sulfide non-woven fabrics on film applicator, by membrane be placed on 25-30 DEG C of temperature,
2-3min is stood in the air of humidity 70-80%, then is transferred in deionized water coagulating bath and cures, deionized water immersion, is finally dried in the air
It is dry, obtain ultrafiltration membrane.
Embodiment 3：The preparation of ultrafiltration membrane
(1) each raw material is weighed by following mass percent：Polyether sulfone 23wt%, n,N-dimethylacetamide 55wt%, point
Son amount is 21600 kollidon 10wt%, and molecular weight is 6000 polyethylene glycol 10wt%, titanium dioxide 2wt%；
(2) at 70 DEG C, polyether sulfone is added in into n,N-dimethylacetamide, 3h is stirred under the rotating speed of 400r/min,
It is clarified to solution；Then kollidon, polyethylene glycol and titanium dioxide are added in, 3h is stirred at 50 DEG C, until being formed equal
Phase solution；
(3) at 40 DEG C, vacuum defoamation processing 1h is carried out to homogeneous phase solution, obtains casting solution；
(4) membrane is made in casting solution and polypropylene non-woven fabric on film applicator, membrane is placed on 25-30 DEG C of temperature, wet
It spends in the air of 70-80% and stands 2-3min, then be transferred in deionized water coagulating bath and cure, deionized water immersion, finally dry,
Obtain ultrafiltration membrane.
Embodiment 4：The preparation of ultrafiltration membrane
(1) each raw material is weighed by following mass percent：Polyether sulfone 14wt%, n,N-dimethylacetamide 25.6wt%,
Dimethyl sulfoxide (DMSO) 38.4wt%, molecular weight are 600000 kollidon 8wt%, and molecular weight is 10000 poly- second two
Alcohol 8wt%, lithium chloride 6wt%；
(2) at 70 DEG C, polyether sulfone is added in into the mixed liquor of n,N-dimethylacetamide and dimethyl sulfoxide (DMSO),
3h is stirred under the rotating speed of 400r/min, until solution is clarified；Then kollidon, polyethylene glycol and lithium chloride are added in,
3h is stirred at 50 DEG C, until forming homogeneous phase solution；
(3) at 40 DEG C, vacuum defoamation processing 2h is carried out to homogeneous phase solution, obtains casting solution；
(4) membrane is made in casting solution and polyphenylene sulfide non-woven fabrics on film applicator, by membrane be placed on 25-30 DEG C of temperature,
2-3min is stood in the air of humidity 70-80%, then is transferred in deionized water coagulating bath and cures, deionized water immersion, is finally dried in the air
It is dry, obtain ultrafiltration membrane.
Ultrafiltration membrane product obtained by embodiment 1-4 and comparative example 1-2 is placed in test equipment and is tested, is used in test process
Feed liquid temperature be 50 DEG C, pH=14, feed liquid it is solid containing being 15%；The pipe produced using Anhui Plum Membrane Technology Co., Ltd.
Formula film complete set of equipments detects the service condition of film product, and test method is as follows：
The starting material flux of every film is tested first, is then taken the film out again water-soluble with pH=1 and pH=14 respectively
After liquid impregnates 200 days under temperature 50 C, throughput is tested again, and concrete numerical value is shown in Table 1.
The test parameter table of 1 film product of table
As can be seen from Table 1：Ultrafiltration membrane uniform pore diameter produced by the present invention, flux are high, stability is good, viscous suitable for height
Degree, large arch dam, the system of pH=1-14.
Claims (8)
1. a kind of preparation method of ultrafiltration membrane, which is characterized in that include the following steps：
(1) at 70-80 DEG C, polyether sulfone is added in into solvent, first stirring to solution is clarified；Then add in interworking pore-foaming agent and
Inorganic additive at 50-60 DEG C, is again stirring for formation homogeneous phase solution；
(2) vacuum defoamation processing is carried out to homogeneous phase solution, obtains casting solution；
(3) membrane is made in casting solution and non-woven fabrics, membrane in air environment successively by standing, in deionized water coagulating bath
Curing, deionized water impregnate and dry processing, obtain ultrafiltration membrane；
The composition of above-mentioned each raw material is as follows：Polyether sulfone 10-25wt%, interworking perforating agent 15-30wt%, inorganic additive 1-
5wt%, solvent 50-70wt%.
2. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that the interworking pore-foaming agent is by polyethylene pyrrole
Pyrrolidone and polyethylene glycol are 1-2 according to mass ratio：2-1 is mixed.
3. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that the molecular weight of the polyethylene glycol is
1000-10000。
4. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that the molecule of the polyvinylpyrrolidone
It measures as 38000-600000.
5. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that the inorganic additive is titanium dioxide
Any one in silicon, titanium dioxide, lithium chloride, zinc chloride.
6. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that the solvent be N, N- dimethyl formyls
One or two kinds of compositions in amine, n,N-dimethylacetamide, N-Methyl pyrrolidone, dimethyl sulfoxide (DMSO).
7. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that in the step (1) for the first time and again
Stir speed (S.S.) is 300-500r/min, and first mixing time is 2-4h；The time is again stirring for as 1-3h.
8. the preparation method of ultrafiltration membrane according to claim 1, which is characterized in that non-woven fabrics is poly- in the step (3)
Propylene non-woven fabrics or polyphenylene sulfide non-woven fabrics.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550412A (en) * | 2018-12-12 | 2019-04-02 | 湖南恒业城市环境科技有限公司 | A kind of acid resistance polyphenylsulfone ultrafiltration membrane and preparation method thereof |
| CN109758915A (en) * | 2019-03-19 | 2019-05-17 | 福建工程学院 | A kind of method that regenerating waste used polyester prepares ultrafiltration membrane |
| CN112370978A (en) * | 2020-11-24 | 2021-02-19 | 苏州富淼膜科技有限公司 | Polysulfone ultrafiltration membrane and preparation method thereof |
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| CN102728244A (en) * | 2011-04-02 | 2012-10-17 | 青岛华轩环保科技有限公司 | Ultrafiltration membrane material with high tensile strength and preparation method thereof |
| CN104258745A (en) * | 2014-10-24 | 2015-01-07 | 南京水思环保科技有限公司 | Preparation method of hydrophilic polyethersulfone microfiltration membrane |
| CN104474929A (en) * | 2014-12-18 | 2015-04-01 | 北京碧水源膜科技有限公司 | Production method of polyether sulfone hollow fiber membrane and structure regulation method of membrane |
| CN104492285A (en) * | 2014-11-20 | 2015-04-08 | 江苏凯米膜科技股份有限公司 | Anti-pollution and high-flux ultrafiltration membrane, preparation method thereof and membrane casting solution |
| CN105833745A (en) * | 2016-05-04 | 2016-08-10 | 浙江理工大学 | Method for preparing hydrophilic polyethersulfone ultrafiltration membrane by taking polyethylene glycol as additive |
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2017
- 2017-12-18 CN CN201711363973.1A patent/CN108043234A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102728244A (en) * | 2011-04-02 | 2012-10-17 | 青岛华轩环保科技有限公司 | Ultrafiltration membrane material with high tensile strength and preparation method thereof |
| CN104258745A (en) * | 2014-10-24 | 2015-01-07 | 南京水思环保科技有限公司 | Preparation method of hydrophilic polyethersulfone microfiltration membrane |
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| CN105833745A (en) * | 2016-05-04 | 2016-08-10 | 浙江理工大学 | Method for preparing hydrophilic polyethersulfone ultrafiltration membrane by taking polyethylene glycol as additive |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550412A (en) * | 2018-12-12 | 2019-04-02 | 湖南恒业城市环境科技有限公司 | A kind of acid resistance polyphenylsulfone ultrafiltration membrane and preparation method thereof |
| CN109758915A (en) * | 2019-03-19 | 2019-05-17 | 福建工程学院 | A kind of method that regenerating waste used polyester prepares ultrafiltration membrane |
| CN112370978A (en) * | 2020-11-24 | 2021-02-19 | 苏州富淼膜科技有限公司 | Polysulfone ultrafiltration membrane and preparation method thereof |
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