CN100393397C - Method for preparing reticular fiber reinforced hollow fiber membrane of polyvinylidene fluoride - Google Patents
Method for preparing reticular fiber reinforced hollow fiber membrane of polyvinylidene fluoride Download PDFInfo
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- CN100393397C CN100393397C CNB2006100135589A CN200610013558A CN100393397C CN 100393397 C CN100393397 C CN 100393397C CN B2006100135589 A CNB2006100135589 A CN B2006100135589A CN 200610013558 A CN200610013558 A CN 200610013558A CN 100393397 C CN100393397 C CN 100393397C
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Abstract
The present invention discloses a method for preparing a reticular fiber reinforced hollow fiber membrane of polyvinylidene fluoride, which belongs to a preparative technique of a hollow fiber membrane. The method comprises the preparing processes that polyvinylidene fluoride is used as membrane materials, N and N-dimethyl formamide, etc. are used as solvent, polyvinylpyrrolidone, etc. are used as additives, and membrane making liquid is formulated by the membrane materials, the solvent and the additives according to certain proportion; a hollow fiber membrane is made of the membrane making liquid under certain temperature, pressure and pulling speed; synthetic fibers are braided into a net on the outer part of the hollow fiber membrane, the hollow fiber membrane which is reinforced by fibers is orderly soaked in the membrane making liquid and solidifying liquid, coated and solidified under certain temperature, pressure and pulling speed, and thus, a reticular fiber reinforced hollow fiber membrane of polyvinylidene fluoride is produced. The present invention has the advantages that fiber blocking phenomena do not exist in flow passages of the hollow fiber membrane, and the flow resistance is little; the stretching intensity reaches 10 to 50MPa, the bursting strength is from 0.5 to 1MPa, and the pore diameter of the hollow fiber membrane is easy to control; the preparing process can be operated continuously, and the present invention is convenient for industrialization.
Description
Technical field
The present invention relates to the preparation method that a kind of reticular fibre strengthens the Kynoar hollow-fibre membrane.The technology of preparing that belongs to the high strength hollow-fibre membrane.
Background technology
Kynoar is increasingly extensive with its good corrosion-resistant, anti-solvent, weatherability and mechanical performance is applied to membrane separation technique, utilizes its hollow-fibre membrane as the membrane material preparation in wastewater treatment, sewage reuse and counter-infiltration application preferably to be arranged with water pretreatment aspect.In these processing procedures, doughnut continues to stand to use and the water impact when cleaning, so need higher intensity to guarantee its normal operation, this point is particularly outstanding in the submerged membrane assembly.And the Kynoar hollow-fibre membrane of conventional method preparation, its strength character concentrates on film body simultaneously with separating through performance, and both are difficult to take into account, and material itself makes that also the Kynoar doughnut film-strength of preparation is lower, is difficult to meet the demands simultaneously.And be that reinforcing material joins among the doughnut with synthetic fibers, utilize synthetic fibers to bear stressed effect, then be a kind of outstanding effect method.As the fiber reinforcement type Kynoar hollow-fibre membrane that patent CN1695777A discloses, its hot strength can reach 10-15MPa, burst strength 0.5-1MPa.
Summary of the invention
The object of the invention is to provide a kind of reticular fibre to strengthen the preparation method of Kynoar hollow-fibre membrane, and this method is simple, is convenient to industrial realization.
The present invention is realized that by following technical proposals a kind of reticular fibre strengthens the preparation method of Kynoar hollow-fibre membrane, and its method feature comprises following process:
1. with the Kynoar membrane material, with N, dinethylformamide, N, N-dimethylacetylamide, dimethyl sulfoxide (DMSO), N-methyl pyrrolidone, trimethyl phosphate, triethyl phosphate, hexamethyl phosphoric acid ammonium or tetramethylurea are solvent, with polyvinylpyrrolidone, polyethylene glycol, lithia, sodium nitrate or ethanol are additive, press Kynoar, solvent, additive mass ratio are (5-30): (55-95): (1-15) preparation preparation liquid.
2. with the part preparation liquid in the step 1, in temperature 20-90 ℃, pressure 0.1-0.6MPa, core flow quantity 1-8ml/min, spinning and through one-level coagulating bath submergence gel, coagulation bath temperature 10-50 ℃ under the hauling speed 0.5-10ml/min condition.Spin to such an extent that external diameter is the doughnut of 1-3mm.
3. the outside with synthetic fibers gained hollow-fibre membrane in step 2 is woven into net, make the doughnut that the outside is surrounded by plastic wire, it is immersed the remaining another part preparation liquid of step 1, at temperature 20-90 ℃, pressure 0-0.5MPa, with the outside doughnut that is surrounded by plastic wire of speed 0.2-5m/min traction, be 10-50 ℃ coagulating bath through excess temperature, make reticular fibre and strengthen the Kynoar hollow-fibre membrane.
Above-mentioned solvent is N, dinethylformamide, N, N-dimethylacetylamide, dimethyl sulfoxide (DMSO) or N-methyl pyrrolidone; Above-mentioned additive is polyvinylpyrrolidone, polyethylene glycol or lithium chloride.
The invention has the advantages that: the hollow-fibre membrane post forming guarantees that fortifying fibre is arranged in membranous wall, and can control the radial position of fortifying fibre at the doughnut membranous wall according to different instructions for uses, thereby reaches the purpose of the serviceability of controlling diaphragm; The doughnut inner flow passage does not have the fiber clogging, can guarantee less flow resistance; The hot strength height, the anti-burst ability is strong; And the hollow-fibre membrane pore size is easily controlled; Industrial realization is convenient in the preparation process continued operation.
The specific embodiment
Embodiment one
1. get Kynoar 75g, N, N-dimethylacetylamide 385g, polyvinylpyrrolidone 40g adds in the molten batch can, is stirring 8 hours dissolving back standing and defoaming down at 60 ℃.In 30 ℃ of temperature, pressure 0.25MPa, core flow quantity 3ml/min, spinning and through solidifying for the coagulating bath submergence under the hauling speed 2ml/min condition with water, 30 ℃ of coagulation bath temperatures spin doughnut.Its aperture is 0.1 μ m, external diameter 1.46mm, wall thickness 0.28mm, pure water flux 454.5L/m under the 0.1MPa
2H, burst strength 0.6MPa, hot strength 0.98MPa, porosity 70%.
2. get Kynoar 40g, N, N-dimethylacetylamide 440g, polyvinylpyrrolidone 8g add in the molten batch can, stir 8 hours dissolving back standing and defoaming down at 60 ℃.
3. the obtained hollow-fibre membrane of step 1 is carried out netting by braiding apparatus in this doughnut outside.The synthetic fibers that netting is adopted are the 100D/48F polyester filament, fiber number of spindles 16, braiding speed 0.68m/min.Then with the coating liquid of the hollow-fibre membrane after the gained netting by step 2,15 ℃ of temperature, hauling speed 0.68m/min applies, and enters the coagulating bath pure water, 20 ℃ of coagulation bath temperatures after 0.25m does journey.Make reticular fiber reinforced Kynoar hollow-fibre membrane.
4. the gained hollow-fibre membrane was soaked in water 4 hours, soaked in absolute ethyl alcohol was tested after 2 hours.Making reticular fiber reinforced Kynoar doughnut membrane aperture is 0.13 μ m, external diameter 1.8mm, wall thickness 0.45mm, pure water flux 265L/m under the 0.1MPa
2H, burst strength 0.68MPa, hot strength 40.1MPa, porosity 67.5%.
Embodiment two
1. prepare the doughnut basement membrane with raw material quality and the operating condition that step 1 is identical among the embodiment one.
2. get Kynoar 50g, N, N-dimethylacetylamide 425g, polyvinylpyrrolidone 25g add in the molten batch can, stir 8 hours dissolving back standing and defoaming down at 60 ℃.
3. step 1 gained hollow-fibre membrane is externally carried out netting by braiding apparatus.Synthetic fibers adopt the 100D/48F polyester filament, fiber number of spindles 16, braiding speed 0.68m/min.Then with the coating liquid of the hollow-fibre membrane after the gained netting by step 2,15 ℃ of temperature, hauling speed 0.68m/min applies, and enters the coagulating bath pure water, 10 ℃ of coagulation bath temperatures after 0.25m does journey.Make reticular fiber reinforced Kynoar hollow-fibre membrane.
4. the gained hollow-fibre membrane was soaked in water 4 hours, soaked in absolute ethyl alcohol was tested after 2 hours.Making reticular fiber reinforced Kynoar doughnut membrane aperture is 0.14 μ m, external diameter 1.76mm, wall thickness 0.41mm, pure water flux 223.9L/m under the 0.1MPa
2H, burst strength 0.62MPa, hot strength 46.93MPa, porosity 64.7%.
Embodiment three
1. prepare the doughnut basement membrane with raw material quality and the operating condition that step 1 is identical among the embodiment one.
2. with Kynoar 75g, N, N-dimethylacetylamide 400g, polyvinylpyrrolidone 25g add in the molten batch can, stir 8 hours dissolving back standing and defoaming down at 60 ℃.
3. step 1 gained hollow-fibre membrane is externally carried out netting by braiding apparatus.Synthetic fibers adopt the 100D/48F polyester filament, fiber number of spindles 16, braiding speed 0.68m/min.Then with the coating liquid of the hollow-fibre membrane after the gained netting by step 2,15 ℃ of temperature, hauling speed 0.68m/min applies, and enters the coagulating bath pure water, 10 ℃ of coagulation bath temperatures after 0.25m does journey.Make reticular fiber reinforced Kynoar hollow-fibre membrane
4. the gained hollow-fibre membrane was soaked in water 4 hours, soaked in absolute ethyl alcohol was tested after 2 hours.Making reticular fiber reinforced Kynoar doughnut membrane aperture is 0.158 μ m, external diameter 1.79mm, wall thickness 0.47mm, pure water flux 165.4L/m under the 0.1MPa
2H, burst strength 0.67MPa, hot strength 43.5MPa, porosity 61.7%.
Claims (2)
1. a reticular fibre strengthens the preparation method of Kynoar hollow-fibre membrane, and its feature comprises following process:
1). with the Kynoar is membrane material, with N, dinethylformamide, N, N-dimethylacetylamide, dimethyl sulfoxide (DMSO), N-methyl pyrrolidone, trimethyl phosphate, triethyl phosphate, hexamethyl phosphoric acid ammonium or tetramethylurea are solvent, with polyvinylpyrrolidone, polyethylene glycol, lithium chloride, sodium nitrate or ethanol is additive, press Kynoar, solvent, additive mass ratio are (5-30): (55-95): (1-15) preparation preparation liquid;
2). with the part preparation liquid in the step 1), in temperature 20-90 ℃, pressure 0.1-0.6MPa, core flow quantity 1-8ml/min, spinning and process one-level coagulating bath submergence gel, spin to such an extent that external diameter is the doughnut of 1-3mm by coagulation bath temperature 10-50 ℃ under the hauling speed 0.5-10ml/min condition;
3). with synthetic fibers in step 2) in the outside of gained hollow-fibre membrane be woven into net, make the doughnut that the outside is surrounded by plastic wire, it is immersed the remaining another part preparation liquid of step 1), at temperature 20-90 ℃, pressure 0-0.5MPa, with the outside doughnut that is surrounded by plastic wire of speed 0.2-5m/min traction, be 10-50 ℃ coagulating bath through excess temperature, make reticular fibre and strengthen the Kynoar hollow-fibre membrane.
2. strengthen the preparation method of Kynoar hollow-fibre membrane by the described reticular fibre of claim 1, it is characterized in that: the solvent of employing is N, dinethylformamide, N, N-dimethylacetylamide, dimethyl sulfoxide (DMSO) or N-methyl pyrrolidone; The additive that adopts is polyvinylpyrrolidone, polyethylene glycol or lithium chloride.
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| CNB2006100135589A CN100393397C (en) | 2006-04-28 | 2006-04-28 | Method for preparing reticular fiber reinforced hollow fiber membrane of polyvinylidene fluoride |
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| CNB2006100135589A CN100393397C (en) | 2006-04-28 | 2006-04-28 | Method for preparing reticular fiber reinforced hollow fiber membrane of polyvinylidene fluoride |
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| CN100450598C (en) * | 2007-03-06 | 2009-01-14 | 天津大学 | Method for preparing PVDF super-fine fiber film with good mechanics-performance |
| CN101185848B (en) * | 2007-08-29 | 2010-12-01 | 江南大学 | Unsymmetrical network shape pore structure hollow fiber film and preparation method thereof |
| CN101357303B (en) * | 2008-09-25 | 2011-06-01 | 杭州洁弗膜技术有限公司 | Preparation method of polyvinylidene fluoride hollow fiber composite microporous film with strong interface binding power |
| CN101422707B (en) * | 2008-11-26 | 2011-08-31 | 北京碧水源膜科技有限公司 | Recovery method of tape liner type polyvinylidene fluoride hollow fiber membrane |
| CN101422708B (en) * | 2008-11-26 | 2011-08-31 | 北京碧水源膜科技有限公司 | Recovery method of polyvinylidene fluoride hollow fiber membrane |
| CN101439268B (en) * | 2008-12-09 | 2011-06-29 | 南京龙源环保有限公司 | Method for preparing high-intensity high-throughput polyvinylidene fluoride hollow fiber membrane |
| CN101791525B (en) * | 2009-12-24 | 2011-11-09 | 北京碧水源膜科技有限公司 | Polyvinylidene fluoride hollow fiber membrane with base material and production method thereof |
| CN101837248B (en) * | 2010-06-24 | 2013-04-10 | 厦门绿邦膜技术有限公司 | Production method of cellosilk enhanced compound hollow fiber membrane |
| CN101961611B (en) * | 2010-10-27 | 2012-11-07 | 江南大学 | Hollow polyester fiber microporous membrane and preparation method thereof |
| CN102500249B (en) * | 2011-11-07 | 2013-07-17 | 北京碧水源科技股份有限公司 | Preparation method for liner type hollow fiber composite membrane and product |
| CN102489181B (en) * | 2011-12-09 | 2013-07-03 | 北京碧水源科技股份有限公司 | Method for preparing hetero-structured hollow fiber membranes |
| US9022229B2 (en) * | 2012-03-09 | 2015-05-05 | General Electric Company | Composite membrane with compatible support filaments |
| CN102600733B (en) * | 2012-03-28 | 2014-03-19 | 天津工业大学 | Preparation method for homogeneously-enhanced polyvinylidene fluoride hollow fiber membrane |
| CN102921308B (en) * | 2012-11-21 | 2014-08-13 | 北京碧水源膜科技有限公司 | Membrane with flocculent reinforced hollow fibers and preparation method therefor |
| CN103028330B (en) * | 2012-12-20 | 2015-08-19 | 北京碧水源膜科技有限公司 | Cotton-shaped enhancing hollow-fibre membrane of a kind of band and preparation method thereof |
| CN103949166B (en) * | 2014-04-30 | 2016-07-06 | 刘必前 | Inner pressed fiber reinforcement filter membrane and preparation method thereof |
| CN104801205B (en) | 2015-04-20 | 2017-06-06 | 天津工业大学 | A kind of preparation method of the enhanced PPTA hollow-fibre membranes of homogeneity |
| CN107308825A (en) * | 2016-04-27 | 2017-11-03 | 李月玲 | A kind of manufacture method of internal pressure tubular multilayer composite separation membrane |
| CN106311170B (en) * | 2016-08-30 | 2019-12-13 | 中山朗清膜业有限公司 | Hollow porous adsorption material for removing inorganic phosphorus and preparation method thereof |
| CN107596928B (en) | 2017-10-12 | 2020-12-15 | 天津工业大学 | Homogeneous fiber reinforced PVDF hollow fiber membrane and preparation method thereof |
| CN108079795A (en) * | 2017-12-13 | 2018-05-29 | 浙江长兴求是膜技术有限公司 | A kind of classifying porous polyvinylidene fluoride hollow fiber composite membrane and its manufacturing method |
| CN108211815A (en) * | 2017-12-29 | 2018-06-29 | 盐城海普润膜科技有限公司 | A kind of composite enhanced hollow-fibre membrane and its preparation method and application |
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