CN105233712A - Preparation method for water-purifying polyether sulfone hollow fiber membrane - Google Patents

Preparation method for water-purifying polyether sulfone hollow fiber membrane Download PDF

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Publication number
CN105233712A
CN105233712A CN201510731184.3A CN201510731184A CN105233712A CN 105233712 A CN105233712 A CN 105233712A CN 201510731184 A CN201510731184 A CN 201510731184A CN 105233712 A CN105233712 A CN 105233712A
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China
Prior art keywords
spinning
preparation
stirred tank
water
hollow fibre
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CN201510731184.3A
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Chinese (zh)
Inventor
陆祖红
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Ningbo Ouvan Sanitaryware Co Ltd
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Ningbo Ouvan Sanitaryware Co Ltd
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Priority to CN201510731184.3A priority Critical patent/CN105233712A/en
Publication of CN105233712A publication Critical patent/CN105233712A/en
Pending legal-status Critical Current

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Abstract

The invention relates to the technical field of water-purifying hydrophilic films, in particular to a preparation method for a water-purifying polyether sulfone hollow fiber membrane. The preparation method comprises the following steps: a first step, respectively preparing a spinning membrane liquid, a bore liquid and a coagulating bath solution; a second step, regulating pressure of a spinning membrane liquid pump to 0.2Mp-0.35Mp, controlling pressure of a bore liquid pump to 0.015Mp-0.035Mp, controlling an air gap between a spinning jet and a coagulating bath solution surface to 5CM-50CM, controlling a coagulating bath temperature to 15-60 DEG C, and carrying out spinning at a speed of 10-20 M per minute. The membrane prepared by adopting the preparation method and the formula provided by the invention is uniform in silk membrane holes, high in retention rate and high in hydrophilicity, and has a better antifouling property.

Description

A kind of preparation method of Water warfare polyether sulphone hollow fibre film
Technical field
The present invention relates to Water warfare hydrophilic film technical field, particularly a kind of preparation method of Water warfare polyether sulphone hollow fibre film.
Background technology
Membrane separation technique be a kind of be widely used in material in liquid or gas medium separation, the concentrated and isolation technics of purifying.Gather extremely trickle micropore on the membranous wall of fluid separation applications, and when stoste passes through the side of film under stress, solvent and low molecule solute become permeate through membranous wall, and larger molecule solute tunicle retains, thus reach the object of separating substances or purifying.Membrane technology is the isolation technics of a kind of advanced person, has many advantages.Such as separation accuracy is high, by force selective, operation at normal temperatures without phase-state change, energy consumption is low, automaticity is high, it is little etc. to pollute.Doughnut is a kind of important form of diffusion barrier.Compared with other form membrane modules, in unit volume, filling film area doughnut is maximum.Hollow-fibre membrane has that high, the easy cleaning of separative efficiency, structure are simple, easy to operate, cost performance high, is thus widely used.Membrane filtration technique develops than faster more a kind of membrane process, and milipore filter and microfiltration membranes are the diffusion barriers be most widely used.Membrane filtration technique development is had higher requirement with the performance of extensive use to diffusion barrier, possesses antipollution, and the diffusion barrier research and development of the property such as heatproof and solvent resistant just become the emphasis problem of current research.Wherein, diffusion barrier pollution problem in use remains the bottleneck of the development of restriction membrane filtration technique and extensive use, and research anti-pollution separation membrane is the key fundamentally solving this problem.There is many pollution problems in existing membrane separation technique has to be solved.
Summary of the invention
The object of the invention is to the defect for prior art and deficiency, a kind of preparation method of Water warfare polyether sulphone hollow fibre film is provided.
A preparation method for Water warfare polyether sulphone hollow fibre film, comprises the steps:
The first step, respectively obtained spinning film liquid, core liquid and coagulating bath solution;
Second step, regulate spinning film liquid pump pressure at 0.2MP-0.35Mp, core liquid pump pressure is at 0.015Mp-0.035Mp, and the air gap of spinning head distance coagulating bath liquid level is at 5CM-50CM, coagulation bath temperature controls, at 15 DEG C-60 DEG C, to carry out spinning with the speed of 10-20M per minute.
The preparation method of described spinning film liquid is is the polyethersulfone resin of 15%-25% by weight ratio, stirred tank is put in the mixing of the dimethylacetylamide of the polyvinylpyrrolidone of 1%-10%, the Macrogol 4000 of 1%-10% and 65%-75%, make to keep vacuum state in stirred tank, heating temperatures is to 50 DEG C-120 DEG C, stir after 5-12 hour, then enter spinning still wait spinning through deaeration.
The preparation method of described core liquid is that stirred tank is put in the water of 50%-70% and the dimethylacetylamide mixing of 30%-50% by weight ratio, make to keep vacuum state in stirred tank, heating temperatures, to 50 DEG C-120 DEG C, stirs after 5-12 hour, then enters spinning still wait spinning through deaeration.
The preparation method of described coagulating bath solution is is the water of 50%-70% by weight ratio, stirred tank is put in the acetic acid mixing of the dimethylacetylamide of 30%-50% and 1%-5%, make to keep vacuum state in stirred tank, heating temperatures, to 50 DEG C-120 DEG C, stirs after 5-12 hour, leaves standstill and waits for spinning.
The K value of described polyvinylpyrrolidone is 30.
Vacuum in described stirred tank is-90Kp.
Beneficial effect of the present invention: the film cortina hole adopting preparation method of the present invention and formula to obtain is even, and rejection is high, hydrophily is high, have good antifouling property.
Detailed description of the invention
Embodiment 1
The invention provides a kind of preparation method of Water warfare polyether sulphone hollow fibre film, comprise the steps:
The first step, respectively obtained spinning film liquid, core liquid and coagulating bath solution;
Second step, regulates spinning film liquid pump pressure at 0.2MPMp, and core liquid pump pressure is at 0.015Mp, and the air gap of spinning head distance coagulating bath liquid level is at 5CM, and coagulation bath temperature controls, at 15 DEG C, to carry out spinning with the speed of 10M per minute.
The preparation method of spinning film liquid be by weight ratio be 15% polyethersulfone resin, the polyvinylpyrrolidone of 1%, the Macrogol 4000 of 9% and 75% dimethylacetylamide mixing put into stirred tank, make to keep vacuum state in stirred tank, heating temperatures is to 50 DEG C, stir after 5 hours, then enter spinning still wait spinning through deaeration.
The preparation method of core liquid is that stirred tank is put in the water of 50% and the dimethylacetylamide mixing of 50% by weight ratio, and make to keep vacuum state in stirred tank, heating temperatures, to 50 DEG C, stirs after 5 hours, then enters spinning still wait spinning through deaeration.
The preparation method of coagulating bath solution is is the water of 50% by weight ratio, the dimethylacetylamide of 49% and 1% acetic acid mixing put into stirred tank, make to keep vacuum state in stirred tank, heating temperatures, to 50 DEG C, stirs after 5 hours, leaves standstill wait spinning.
Preferably, the K value of polyvinylpyrrolidone is 30.
Preferably, the vacuum in stirred tank is-90Kp.
Embodiment 2
A preparation method for Water warfare polyether sulphone hollow fibre film, comprises the steps:
The first step, respectively obtained spinning film liquid, core liquid and coagulating bath solution;
Second step, regulates spinning film liquid pump pressure at 0.3MP, and core liquid pump pressure is at 0.03Mp, and the air gap of spinning head distance coagulating bath liquid level is at 20CM, and coagulation bath temperature controls, at 30 DEG C, to carry out spinning with the speed of 15M per minute.
The preparation method of spinning film liquid be by weight ratio be 20% polyethersulfone resin, the polyvinylpyrrolidone of 5%, the Macrogol 4000 of 5% and 70% dimethylacetylamide mixing put into stirred tank, make to keep vacuum state in stirred tank, heating temperatures is to 80 DEG C, stir after 9 hours, then enter spinning still wait spinning through deaeration.
The preparation method of core liquid is that stirred tank is put in the water of 60% and the dimethylacetylamide mixing of 40% by weight ratio, and make to keep vacuum state in stirred tank, heating temperatures, to 80 DEG C, stirs after 9 hours, then enters spinning still wait spinning through deaeration.
The preparation method of coagulating bath solution is is the water of 60% by weight ratio, the dimethylacetylamide of 37% and 3% acetic acid mixing put into stirred tank, make to keep vacuum state in stirred tank, heating temperatures, to 80 DEG C, stirs after 9 hours, leaves standstill wait spinning.
Preferably, the K value of polyvinylpyrrolidone is 30.
Preferably, the vacuum in stirred tank is-90Kp.
Embodiment 3
A preparation method for Water warfare polyether sulphone hollow fibre film, comprises the steps:
The first step, respectively obtained spinning film liquid, core liquid and coagulating bath solution;
Second step, regulates spinning film liquid pump pressure at 0.35Mp, and core liquid pump pressure is at 0.035Mp, and the air gap of spinning head distance coagulating bath liquid level is at 50CM, and coagulation bath temperature controls, at 60 DEG C, to carry out spinning with the speed of 20M per minute.
The preparation method of spinning film liquid be by weight ratio be 25% polyethersulfone resin, the polyvinylpyrrolidone of 9%, the Macrogol 4000 of 1% and 65% dimethylacetylamide mixing put into stirred tank, make to keep vacuum state in stirred tank, heating temperatures is to 120 DEG C, stir after 12 hours, then enter spinning still wait spinning through deaeration.
The preparation method of core liquid is that stirred tank is put in the water of 70% and the dimethylacetylamide mixing of 30% by weight ratio, and make to keep vacuum state in stirred tank, heating temperatures, to 120 DEG C, stirs after 12 hours, then enters spinning still wait spinning through deaeration.
The preparation method of coagulating bath solution is is the water of 65% by weight ratio, the dimethylacetylamide of 30% and 5% acetic acid mixing put into stirred tank, make to keep vacuum state in stirred tank, heating temperatures, to 120 DEG C, stirs after 12 hours, leaves standstill wait spinning.
Preferably, the K value of polyvinylpyrrolidone is 30.
Preferably, the vacuum in stirred tank is-90Kp.
The above is only better embodiment of the present invention, therefore all equivalences done according to structure, feature and the principle described in patent claim of the present invention change or modify, and are included in patent claim of the present invention.

Claims (6)

1. a preparation method for Water warfare polyether sulphone hollow fibre film, comprises the steps:
The first step, respectively obtained spinning film liquid, core liquid and coagulating bath solution;
Second step, regulate spinning film liquid pump pressure at 0.2MP-0.35Mp, core liquid pump pressure is at 0.015Mp-0.035Mp, and the air gap of spinning head distance coagulating bath liquid level is at 5CM-50CM, coagulation bath temperature controls, at 15 DEG C-60 DEG C, to carry out spinning with the speed of 10-20M per minute.
2. the preparation method of a kind of Water warfare polyether sulphone hollow fibre film according to claim 1, it is characterized in that: the preparation method of described spinning film liquid is is the polyethersulfone resin of 15%-25% by weight ratio, stirred tank is put in the mixing of the dimethylacetylamide of the polyvinylpyrrolidone of 1%-10%, the Macrogol 4000 of 1%-10% and 65%-75%, make to keep vacuum state in stirred tank, heating temperatures is to 50 DEG C-120 DEG C, stir after 5-12 hour, then enter spinning still wait spinning through deaeration.
3. the preparation method of a kind of Water warfare polyether sulphone hollow fibre film according to claim 1, it is characterized in that: the preparation method of described core liquid is that stirred tank is put in the water of 50%-70% and the dimethylacetylamide mixing of 30%-50% by weight ratio, make to keep vacuum state in stirred tank, heating temperatures is to 50 DEG C-120 DEG C, stir after 5-12 hour, then enter spinning still wait spinning through deaeration.
4. the preparation method of a kind of Water warfare polyether sulphone hollow fibre film according to claim 1, it is characterized in that: the preparation method of described coagulating bath solution is is the water of 50%-70% by weight ratio, stirred tank is put in the acetic acid mixing of the dimethylacetylamide of 30%-50% and 1%-5%, make to keep vacuum state in stirred tank, heating temperatures is to 50 DEG C-120 DEG C, stir after 5-12 hour, leave standstill and wait for spinning.
5. the preparation method of a kind of Water warfare polyether sulphone hollow fibre film according to claim 2, is characterized in that: the K value of described polyvinylpyrrolidone is 30.
6. the preparation method of a kind of Water warfare polyether sulphone hollow fibre film according to claim 2 to 5 any one, is characterized in that: the vacuum in described stirred tank is-90Kp.
CN201510731184.3A 2015-10-31 2015-10-31 Preparation method for water-purifying polyether sulfone hollow fiber membrane Pending CN105233712A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115463550A (en) * 2022-08-28 2022-12-13 天津汉晴环保科技有限公司 Polyether sulfone humidifying membrane with symmetrical structure and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1375351A (en) * 2001-12-28 2002-10-23 上海益尔康医用设备有限公司 Production process of hollow blended polyether sulphone fiber dialysis membrane
CN1631501A (en) * 2004-11-11 2005-06-29 东华大学 Hollow cellulous dialyzing and ultra filtrating membrane of cross blend polyethersulfone, its manufacturing method and usage
WO2008046779A1 (en) * 2006-10-18 2008-04-24 Gambro Lundia Ab Hollow fiber membrane and method for manufacturing thereof
CN101543731A (en) * 2009-03-23 2009-09-30 杭州洁弗膜技术有限公司 Method for preparing fiber braided tube embedded enhanced type polymer hollow fiber microporous membrane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1375351A (en) * 2001-12-28 2002-10-23 上海益尔康医用设备有限公司 Production process of hollow blended polyether sulphone fiber dialysis membrane
CN1631501A (en) * 2004-11-11 2005-06-29 东华大学 Hollow cellulous dialyzing and ultra filtrating membrane of cross blend polyethersulfone, its manufacturing method and usage
WO2008046779A1 (en) * 2006-10-18 2008-04-24 Gambro Lundia Ab Hollow fiber membrane and method for manufacturing thereof
CN101543731A (en) * 2009-03-23 2009-09-30 杭州洁弗膜技术有限公司 Method for preparing fiber braided tube embedded enhanced type polymer hollow fiber microporous membrane

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115463550A (en) * 2022-08-28 2022-12-13 天津汉晴环保科技有限公司 Polyether sulfone humidifying membrane with symmetrical structure and preparation method thereof

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