CN102343219A - Polysulfone membrane with supporting materials and preparation method thereof - Google Patents
Polysulfone membrane with supporting materials and preparation method thereof Download PDFInfo
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- CN102343219A CN102343219A CN2011102920476A CN201110292047A CN102343219A CN 102343219 A CN102343219 A CN 102343219A CN 2011102920476 A CN2011102920476 A CN 2011102920476A CN 201110292047 A CN201110292047 A CN 201110292047A CN 102343219 A CN102343219 A CN 102343219A
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Abstract
The invention discloses a polysulfone hollow fibrous membrane with supporting materials and a preparation method thereof. The polysulfone hollow fibrous composite membrane with the supporting materials is prepared a method comprising the following steps: preparing the polysulfone hollow fibrous membrane by a dry-wet method by taking Tween 20 or polyethylene glycol as an additive and N,N-dimethylacetamide or N-methylpyrrolidone as a solvent, ensuring monofilaments to enter into a spinneret from other inlets and blending the polysulfone hollow fibrous membrane with the monofilaments, wherein the monofilament fibrous materials are spandex, nylon 6 or polyurethane and have diameter of 0.01-2mm. According to the invention, the defect that the hollow fibrous membranes without supports have insufficient physical tensile strength and are easy to suffer from filament break is overcome; the physical tensile strength of the membrane disclosed by the invention is improved by more than several times compared with that of the hollow fibrous membranes without supports; support and membrane stripping can be avoided; the water flux and manufacturing cost of the membrane disclosed by the invention are equivalent to those of the hollow fibers without supports; and the membrane has technical and economic breakthroughs, can replace the existing hollow fiber products and has great economic and social benefits.
Description
Technical field
The present invention relates to composite, relate in particular to a kind of ps hollow fiber uf membrane with backing material and preparation method thereof.
Background technology
Ultrafiltration is to be motive force with pressure, utilize the aperture, material surface chemical characteristic etc. of film to make solvent, little molecule solute see through film, and macromolecular substances such as colloid, protein, bacterium, virus is trapped concentrated screening process.Milipore filter material commonly used has polysulfones, polyether sulfone, Kynoar, polyacrylonitrile etc., and poor like: hydrophily, be prone to pollution, intensity difference or the like in order to overcome some shortcoming of membrane material itself, people usually use some physics or chemical method that it is carried out modification.In recent years, some scholars attempt utilizing Al
2O
3, SiO
2, TiO
2Deng inorganic nano-particle the milipore filter material is carried out study on the modification, prepare inorganic nano-particle filled polymer composite film material, and show excellent serviceability.But the manufacturing cost higher price of these milipore filters is expensive, and preparation process is complicated, is not beneficial to large-scale promotion application very much.Thereby preparation intensity is big, the PVC hollow fiber membrane of good toughness, high flux, high rejection has important theory and realistic meaning.
Summary of the invention
The objective of the invention is deficiency, a kind of ps hollow fiber uf membrane with backing material and preparation method thereof is provided to existing ps hollow fiber uf membrane technology.
The poly (ether sulfone) film of band backing material is: with the filter membrane of polyether sulfone materials and 3 parallel blending formation of above monfil; Monfil is evenly distributed on the rete center after the film forming; Monfil is spandex, nylon 6 or polyurethane, and the diameter of monfil is the 0.01-2 millimeter.
The preparation method's of the PS membrane of band backing material step is following:
1) concentration is that polyether sulfone, the concentration of 16-18 wt/v % are that 5-15 wt/v % additive, concentration are that the solvent of 50-80 wt/v % adds successively and dissolves in the material still; Open the shaft sealing of dissolving the material still and press the hurdle; Through fully stirring 8-24h, obtain casting solution under 60-100 ℃;
2) casting solution is clamp-oned tubular type doughnut spinning nozzle; Under the spinning speed of 15-40m/min; Casting solution is extruded by air pressure, gets into the spinning head casting solution through strainer filtering and measuring pump and gets into the hole, and gets into the hole from monfil and gets into the monfil of spinning head and get into deionized water the hole film-forming that after entering coagulating bath after the spinning head generation composite molding, is separated with core liquid; The coagulating bath gel media is the water of steady temperature, and coolant-temperature gage is controlled at 18-45 ℃.Spinning temperature 20-80 ℃, interior coagulating bath is a deionized water, and temperature is 5-60 ℃.
Described additive is: polysorbas20 or polyethylene glycol.Described solvent is: N, N-dimethylacetylamide or N-methyl pyrrolidone.
The present invention's beneficial effect compared with prior art is:
1) the physics hot strength is high: because the monfil booster action as reinforcing bar is arranged, the physics hot strength of this product is minimum can be increased more than the several times, and can increase the next doughnut film strength that further increases of quantity of monfil.Usually 3-4 root monfil longitudinal tensile strength can reach more than 1 kgf;
2) membrane material can not peel off: adopt the blending hollow-fibre membrane of kernmantle, coating and kernmantle easy separation are peeled off, and lose filtering function; And adopt this product, because monfil and bulk material have certain compatibility, and, can not take place to separate and peel off, the service life of the film that increases greatly fully by PVC bulk material parcel;
3) cost is lower than the blending hollow-fibre membrane of kernmantle: in the blending hollow-fibre membrane material cost of kernmantle the kernmantle cost to account for over half, so cost will double above than this product;
4) loading density is higher than the blending hollow-fibre membrane of kernmantle, reduces volume, reduces the filter plant cost.The blending hollow-fibre membrane of kernmantle is owing to receive the external diameter size restriction of kernmantle, and often thicker, external diameter is generally more than 2 millimeters; And this product does not have this restriction; External diameter can be accomplished 1.2 millimeters, and the membrane area of unit volume can increase like this, reduces the filter plant volume;
5) because the monofilament of introducing has certain intermiscibility with membrane material, and the volume that is embedded in the film is little, only accounts for the 3-5% of membrane material volume, and is very little to the film forming structure influence, so the water flux of film can reach 180-300L/m
2H, 0.1MPa, 25 ℃ is more than 2 times of kernmantle structural membrane, suitable with no support hollow tunica fibrosa.
Description of drawings
Fig. 1 is the PS membrane preparation method schematic flow sheet of band backing material;
Fig. 2 is novel blending ps hollow fiber uf membrane generalized section and existing two types of PES hollow-fibre membrane generalized sections.
The specific embodiment
The preparation method's of the PS membrane of band backing material step is following:
1) concentration is that polyether sulfone, the concentration of 16-18 wt/v % are that 5-15 wt/v % additive, concentration are that the solvent of 50-80 wt/v % adds successively and dissolves in the material still; Open the shaft sealing of dissolving the material still and press the hurdle; Through fully stirring 8-24h, obtain casting solution under 60-100 ℃;
2) casting solution is clamp-oned tubular type doughnut spinning nozzle; Under the spinning speed of 15-40m/min; Casting solution is extruded by air pressure, gets into the spinning head casting solution through strainer filtering and measuring pump and gets into the hole, and gets into the hole from monfil and gets into the monfil of spinning head and get into deionized water the hole film-forming that after entering coagulating bath after the spinning head generation composite molding, is separated with core liquid; The coagulating bath gel media is the water of steady temperature, and coolant-temperature gage is controlled at 18-45 ℃.Spinning temperature 20-80 ℃, interior coagulating bath is a deionized water, and temperature is 5-60 ℃.
Described additive is: polysorbas20 or polyethylene glycol.Described solvent is: N, N-dimethylacetylamide or N-methyl pyrrolidone.
Embodiment 1
1) concentration is that polyether sulfone, the concentration of 16 wt/v % are that 5 wt/v % polysorbas20s, concentration are the N of 50 wt/v %, and the N-dimethylacetylamide adds successively and dissolves in the material still, opens the shaft sealing of dissolving the material still and presses the hurdle, and 60 ℃ down through fully stirring 8h, obtains casting solution;
2) casting solution is clamp-oned tubular type doughnut spinning nozzle; Under the spinning speed of 15m/min; Casting solution is extruded by air pressure, gets into the spinning head casting solution through strainer filtering and measuring pump and gets into the hole, and gets into the hole from monfil and gets into the monfil of spinning head and get into deionized water the hole film-forming that after entering coagulating bath after the spinning head generation composite molding, is separated with core liquid; The coagulating bath gel media is the water of steady temperature, and coolant-temperature gage is controlled at 18 ℃.20 ℃ of spinning temperatures, interior coagulating bath are deionized water, and temperature is 5 ℃.
Obtained PS membrane pore-creating character is better, and fenestra is evenly distributed, and pore size distribution range is narrower, and hydrophilicity is better.In the 1g/L bovine serum albumin cushioning liquid retention experiments, flux can maintain 200L/ (m
2H), rejection is 99%.
Embodiment 2
1) concentration is that polyether sulfone, the concentration of 18 wt/v % are that 15 wt/v % polyethylene glycol, concentration are that the N-methyl pyrrolidone of 80 wt/v % adds successively and dissolves in the material still; Open the shaft sealing of dissolving the material still and press the hurdle; Through fully stirring 24h, obtain casting solution under 100 ℃;
2) casting solution is clamp-oned tubular type doughnut spinning nozzle; Under the spinning speed of 40m/min; Casting solution is extruded by air pressure, gets into the spinning head casting solution through strainer filtering and measuring pump and gets into the hole, and gets into the hole from monfil and gets into the monfil of spinning head and get into deionized water the hole film-forming that after entering coagulating bath after the spinning head generation composite molding, is separated with core liquid; The coagulating bath gel media is the water of steady temperature, and coolant-temperature gage is controlled at 45 ℃.80 ℃ of spinning temperatures, interior coagulating bath are deionized water, and temperature is 60 ℃.
Obtained PS membrane pore-creating character is better, and fenestra is evenly distributed, and pore size distribution range is narrower, and hydrophilicity is better.In the 1g/L bovine serum albumin cushioning liquid retention experiments, flux can maintain 215L/ (m
2H), rejection is 98%.
Embodiment 3
Polysulfones 16 wt/v %, additives polyethylene glycol 10 wt/v %, solvent is N, N-dimethylacetylamide 80 wt/v %.Casting solution was stirred 12 hours through abundant down for 85 ℃ in temperature, mix.Under hot state, filter the uniform casting solution of dissolving removing insoluble impurity, and under 25 ℃ of conditions, carry out vacuum outgas.Open and dissolve material still baiting valve; Casting solution is extruded by air pressure; Get into the spinning head casting solution through strainer filtering and measuring pump and get into the hole, with get into from monfil the hole get into spinning head monfil and with core liquid entering hole deionized water in spinning head generation composite molding, behind the 25cm that in air, walks vertically downward; Get into coagulating bath, the phase-splitting film forming.The outer gel media of coagulating bath is the water of steady temperature, and temperature is controlled at 25 ℃, and the inner gel medium is a deionized water, and temperature is controlled at 25 ℃.Spinning temperature is 65 ℃, and spinning speed is 40m/min.Core liquid is the aqueous solution that contains 10% solvent, and temperature is 25 ℃.Preparation gained film soaks the back test through rinsing and 60 wt/v % glycerine.
Obtained PS membrane pore size distribution is even, narrow pore size distribution range.Be used to separate concentrating 1g/L bovine serum albumin cushioning liquid, flux can maintain 200L/ (m
2H), rejection is 96.7%.
Adopt the Hollow Fiber Ultrafiltration assembly or the MBR membrane bioreactor of this production to compare for the kernmantle hollow-fibre membrane with supporter, volume is little, and film can not peel off damage, long service life, and cost of investment and use cost can significantly reduce.
Embodiment 4
Polyether sulfone 18 wt/v %, additive are tween 10 wt/v %, and solvent is N-methyl pyrrolidone 75 wt/v %.Casting solution was stirred 12 hours through abundant down for 85 ℃ in temperature, mix and remove insoluble impurity, under 25 ℃ of conditions, carry out vacuum outgas.Open and dissolve material still baiting valve; Casting solution is extruded by air pressure; Get into the spinning head casting solution through strainer filtering and measuring pump and get into the hole, with get into from monfil the hole get into spinning head monfil and with core liquid entering hole deionized water in spinning head generation composite molding, behind the 35cm that in air, walks vertically downward; Get into coagulating bath, the phase-splitting film forming.The outer gel media of coagulating bath is the water of steady temperature, and temperature is controlled at 25 ℃, and the inner gel medium is the mixed liquor of water and solvent, and temperature is controlled at 25 ℃.Wherein spinning temperature is 65 ℃, and spinning speed is 35m/min.Core liquid is deionized water, and temperature is 25 ℃.Preparation gained film soaks the back test through rinsing and 60% glycerine.
Obtained PS membrane pore-creating character is better, and fenestra is evenly distributed, and pore size distribution range is narrower, and hydrophilicity is better.In the 1g/L bovine serum albumin cushioning liquid retention experiments, flux can maintain 220L/ (m
2H), rejection is 99%.
Embodiment 5:
Polyether sulfone 16 wt/v %, additive is a polyethylene glycol, 10 wt/v %, solvent are N-methyl pyrrolidone 75 wt/v %.Casting solution was stirred 12 hours through abundant down for 85 ℃ in temperature, mix and remove insoluble impurity, under 25 ℃ of conditions, carry out vacuum outgas.Open and dissolve material still baiting valve; Casting solution is extruded by air pressure; Get into the spinning head casting solution through strainer filtering and measuring pump and get into the hole, with get into from monfil the hole get into spinning head monfil and with core liquid entering hole deionized water in spinning head generation composite molding, behind the 30cm that in air, walks vertically downward; Get into coagulating bath, the phase-splitting film forming.The outer gel media of coagulating bath is the water of steady temperature, and temperature is controlled at 25 ℃, and the inner gel medium is a deionized water, and temperature is controlled at 25 ℃.Wherein spinning temperature is 60 ℃, and spinning speed is 40m/min.Core liquid is the aqueous solution that contains 10% solvent, and temperature is 25 ℃.Preparation gained film soaks the back test through rinsing and 60% glycerine.
To this complex system of wastewater from regenerating paper production of certain papermaking enterprise, the PS film of choosing novel band backing material carries out advanced treating to it, and system thinking film service condition is to the influence of effluent quality and membrane separating property.
COD clearance and film silk stability result such as following table
At last, what need particularly point out is that what more than to enumerate only is practical implementation case of the present invention.Obviously, the invention is not restricted to above-mentioned case study on implementation, can also many combinations.The all scenario that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (4)
1. poly (ether sulfone) film with backing material; It is characterized in that filter membrane with polyether sulfone materials and 3 parallel blending formation of above monfil; Monfil is evenly distributed on the rete center after the film forming, and monfil is spandex, nylon 6 or polyurethane, and the diameter of monfil is the 0.01-2 millimeter.
2. the preparation method of an a kind of PS membrane with backing material as claimed in claim 1 is characterized in that its step is following:
1) concentration is that polyether sulfone, the concentration of 16-18 wt/v % are that 5-15 wt/v % additive, concentration are that the solvent of 50-80 wt/v % adds successively and dissolves in the material still; Open the shaft sealing of dissolving the material still and press the hurdle; Through fully stirring 8-24h, obtain casting solution under 60-100 ℃;
2) casting solution is clamp-oned tubular type doughnut spinning nozzle; Under the spinning speed of 15-40m/min, casting solution is extruded by air pressure, gets into spinning head casting solution entering hole through strainer filtering and measuring pump; With get into the hole from monfil and get into the monfil of spinning head and get into deionized water the hole film-forming that after getting into coagulating bath after the spinning head generation composite molding, is separated with core liquid; The coagulating bath gel media is the water of steady temperature, and coolant-temperature gage is controlled at 18-45 ℃, spinning temperature 20-80 ℃; Interior coagulating bath is a deionized water, and temperature is 5-60 ℃.
3. the preparation method of a kind of polysulfones with backing material according to claim 2 is characterized in that described additive is: polysorbas20 or polyethylene glycol.
4. the preparation method of a kind of PS membrane with backing material according to claim 2 is characterized in that described solvent is: N, N-dimethylacetylamide or N-methyl pyrrolidone.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102343221A (en) * | 2011-09-29 | 2012-02-08 | 浙江开创环保科技有限公司 | Polyethersulfone membrane with supporting materials and preparation method thereof |
| CN103721573A (en) * | 2014-01-08 | 2014-04-16 | 宁波恺谱瑞膜科技有限公司 | High-strength hollow fiber film and preparation method thereof |
| CN114797491A (en) * | 2022-06-23 | 2022-07-29 | 杭州科百特过滤器材有限公司 | Filtering membrane package and preparation method thereof |
| CN115400616A (en) * | 2022-11-01 | 2022-11-29 | 富海(东营)新材料科技有限公司 | Preparation process and system of continuous integrated polysulfone hollow fiber membrane |
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| CN102019150A (en) * | 2010-12-21 | 2011-04-20 | 惠州七芯膜净化环保有限公司 | Polyether sulfone-polyurethane blend hollow fiber membrane and preparation method thereof |
| CN102151489A (en) * | 2011-03-21 | 2011-08-17 | 凌雪萍 | Multi-core hollow fiber porous membrane and preparation method thereof |
| CN102343221A (en) * | 2011-09-29 | 2012-02-08 | 浙江开创环保科技有限公司 | Polyethersulfone membrane with supporting materials and preparation method thereof |
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2011
- 2011-09-29 CN CN2011102920476A patent/CN102343219A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019150A (en) * | 2010-12-21 | 2011-04-20 | 惠州七芯膜净化环保有限公司 | Polyether sulfone-polyurethane blend hollow fiber membrane and preparation method thereof |
| CN102151489A (en) * | 2011-03-21 | 2011-08-17 | 凌雪萍 | Multi-core hollow fiber porous membrane and preparation method thereof |
| CN102343221A (en) * | 2011-09-29 | 2012-02-08 | 浙江开创环保科技有限公司 | Polyethersulfone membrane with supporting materials and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102343221A (en) * | 2011-09-29 | 2012-02-08 | 浙江开创环保科技有限公司 | Polyethersulfone membrane with supporting materials and preparation method thereof |
| CN103721573A (en) * | 2014-01-08 | 2014-04-16 | 宁波恺谱瑞膜科技有限公司 | High-strength hollow fiber film and preparation method thereof |
| CN103721573B (en) * | 2014-01-08 | 2016-02-03 | 宁波恺谱瑞膜科技有限公司 | A kind of High-strength hollow fiber film and preparation method thereof |
| CN114797491A (en) * | 2022-06-23 | 2022-07-29 | 杭州科百特过滤器材有限公司 | Filtering membrane package and preparation method thereof |
| CN115400616A (en) * | 2022-11-01 | 2022-11-29 | 富海(东营)新材料科技有限公司 | Preparation process and system of continuous integrated polysulfone hollow fiber membrane |
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Application publication date: 20120208 |