CN102580553A - Method for manufacturing environmental-friendly hollow-fibre membrane - Google Patents
Method for manufacturing environmental-friendly hollow-fibre membrane Download PDFInfo
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- CN102580553A CN102580553A CN2012100896922A CN201210089692A CN102580553A CN 102580553 A CN102580553 A CN 102580553A CN 2012100896922 A CN2012100896922 A CN 2012100896922A CN 201210089692 A CN201210089692 A CN 201210089692A CN 102580553 A CN102580553 A CN 102580553A
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Abstract
The invention discloses a method for manufacturing environmental-friendly hollow-fibre membrane. The method is characterized by comprising the following steps: step 1, polylactic acid, polyvinylidene fluoride or polyether sulfone, solvent and pore-forming agent are mixed according to the following weight ratio: 2 to 20% of polylactic acid, 2 to 20 of polyvinylidene fluoride or polyether sulfone, 50 to 86% of solvent and 0.5 to 25% of pore-forming agent; and step 2, the solution obtained in step 1 is stirred, heated and resolved uniformly to obtain casting solution, and the casting solution is extruded together with core liquid in central pipe hole of a spinning head by the spinning head of a hollow fiber spinning machine, solvent and pore-forming agent in spinning solution are in solidified liquid phase, and polymer blend settles to form polymer hollow-fibre membrane due to phase transfer. The method can be used for the development of various high-function ultrafiltration membrane, nanofiltration membrane, micro-filtration membrane, gas separation membrane and the like.
Description
Technical field
The present invention relates to the film separation field, particularly a kind of manufacturing approach of environmentally friendly hollow-fibre membrane.
Background technology
Hollow-fibre membrane is widely used in the filtration or the dialysis in the various fields such as processing, drink water purifying, middle water reuse, food processing and biological medicine of industry and municipal wastewater.Adopt the design of corn polylactic acid blend film; Can study respectively and select different blend macromolecules; Be easy to obtain high-hydrophilic, high flux, antibiotic property, eco-friendly diffusion barrier; Therefore, corn polylactic acid blend doughnut membrane technology has become an important development direction in the high functional membrane technology of preparing.
In use mainly there is following problem in hollow-fibre membrane at present: (1) is difficult for degraded, is prone to cause environmental pollution; (2) antibiotic property is poor, and face is prone to the growth bacterium, is prone to pollute, and is difficult for cleaning; (3) raw material is petroleum chemicals, is difficult for regeneration.Application number is that disclosed a kind of hydrophilic PVB blended hollow-fibre membrane of Chinese invention patent application of 200810031016 and preparation method thereof is: with PVB and other high molecular polymer blend, adding solvent, pore former etc. are made into the casting solution spinning and process hollow-fibre membrane." zein fiber " in " Guangxi textile technology " (2007 the 36th the 1st phases of volume) also introduced with the spinning of corn polymer and made zein fiber; Having good antibacterial property, water imbibition (hydrophily) and high strength, is a kind of environment-friendly materials that have development prospect.U.S. HANZSCH BERND etc. on August 21st, 2003 U.S. Patent No. US2003158260 reported that a kind of fermentation starch based agricultural product (corn) make PLA (corn PLA).Chinese biological technical information net was introduced the new lining of du pont company corn polymer (PLA) weaving and has been appeared on the market on September 12nd, 2004, and the corn polymer derives from corn, and safety and environmental protection helps resource regeneration.At present, the corn PLA is used to prepare hollow-fibre membrane and also rarely has report.
Summary of the invention
The object of the invention be exactly through preparation corn polylactic acid blend hollow-fibre membrane be prone to pollute to solve film, difficult cleaning and environmental pollution, non-renewable problem.
For achieving the above object, technical scheme proposed by the invention is: a kind of manufacturing approach of environmentally friendly hollow-fibre membrane is characterized in that: comprise the steps:
Step 1: PLA and Kynoar or polyether sulfone, solvent, pore former are mixed by following part by weight:
PLA 2-20%;
Kynoar or polyether sulfone 2-20%;
Solvent 50-86%;
Pore former 0.5-25%;
Step 2: the casting solution that above-mentioned solution stirring, heating for dissolving are evenly made; The core liquid of pore extrudes simultaneously through the spinneret of doughnut spinning-drawing machine with at the spinneret center; Get in the outer solidification liquid then; Solvent in the spinning solution and pore former get into and solidify liquid phase, and polymer blend is because phase transfer and precipitating becomes blend hollow fiber membrane.
Further, the preferred intensive polar solvent of described solvent can be thought the mixture of following one or more solvents: dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone, trichloroethanes, acetone or toluene etc.
Further, described core liquid can be the mixed liquor of water or water and spin solvent.
Further, described solidification liquid is the mixed solution of pure water and organic solvent, and wherein hundred parts of specific concentrations of weight of organic solvent are 0-30%, described organic solvent preferred alcohol or isopropyl alcohol.
Further, described pore former is inorganic pore former or organic polymer pore former or is the mixture of the two.
Preferably; Described inorganic pore former is following one or more mixture: lithium chloride, lithium nitrate, sodium chloride, calcium chloride, calcium nitrate, titanium dioxide, silica, alundum (Al etc.; The content of inorganic pore former in casting solution is 0.5-20wt%; Be preferably 1-10 wt%, the granularity of inorganic pore former is preferably nanoscale less than 5 microns.
Further, when adopting inorganic pore former, can after spinning, use alkali, acid, water or organic solvent etc. again with inorganic pore former stripping.
Further; Described organic polymer pore former is following one or more mixture: high molecular weight water soluble polymers such as polyethylene glycol, ethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol; Wherein the molecular weight of polyethylene glycol is preferably 200-30000 dalton, and the molecular weight of polyvinylpyrrolidone is preferably 200-30000 dalton.The content of organic polymer pore former in casting solution is 1-25wt%, is preferably 3-10wt%.
Adopt the preparation method of corn polylactic acid blend hollow-fibre membrane of the present invention, the hollow-fibre membrane that makes, its external diameter are 0.5-3.5mm, and internal diameter is 0.2-2.5mm, and porosity is 50-85%.It is the 0.001-1 micron that film separates the aperture, and at 0.1MPa, under 25 ℃ the test condition, the pure water water-flowing amount is 100-8000L/m2*hr.
This method can be used to develop various high function milipore filters, NF membrane, micro-filtration membrane and gas separation membrane etc., and compared with prior art, beneficial effect of the present invention is following:
1) be one of main material through adopting the corn PLA, raw material sources are abundant and renewable, and have biodegradability, and are environmentally friendly;
2) the corn PLA has good hydrophily, can improve the water-flowing amount and the stain resistance of product;
3) the corn PLA also has antibiotic property, can avoid the growth of bacterium on the film surface, and the pollution resistance and the Geng Yi that have also just improved product clean, and keep more stable water-flowing amount;
4) through with the adjustment of various polymerization thing or different proportion, can more easily produce the various performance products that are fit to demands of different.
The specific embodiment
Below in conjunction with the specific embodiment, the present invention is further specified.
The present invention adopts solution phase transfer doughnut spinning technique commonly used in the prior art (wet method or dried-wet method) condition system film.
Performance measurement of the present invention: water-flowing amount adopts the outer press filtering device of the homemade dead end in laboratory to measure, and the wet film after promptly cleaning is earlier in 0.15MPa precompressed half an hour, then its external pressure water-flowing amount of mensuration under 0.1MPa pressure.
Embodiment 1: with 7 kilograms of dimethylacetylamides, and 0.2 kilogram of corn PLA, 2.0 kilograms of polyvinylidene fluoride polymer; 0.5 the kilogram polyethylene glycol, 200 gram lithium nitrates, the heated and stirred dissolving is evenly; Process the casting solution of corn polylactic acid blend hollow-fibre membrane; Adopt and do-wet method doughnut spinning technique, casting solution and core liquid (core liquid is pure water) are extruded through spinneret, through coagulating bath water tank (coagulating agent is a pure water); Solvent in the casting solution (containing pore former, pore-creating agent) is dissolved in the solidification liquid, the polymer precipitation film forming, makes corn polylactic acid blend hollow-fibre membrane.External diameter 1.5mm, internal diameter 0.9mm, porosity is 66%, and it is 0.1 micron that film separates the aperture, and at 0.1MPa, under 25 ℃ the test condition, the pure water water-flowing amount is 820L/m2*hr.
Embodiment 2: with 7 kilograms of dimethylacetylamides, and 1.0 kilograms of corn PLAs, 0.8 kilogram of polyvinylidene fluoride polymer; 0.2 the kilogram polyethylene glycol, 200 gram polyvinyl alcohol, 500 gram lithium nitrates; The heated and stirred dissolving is evenly processed the casting solution of corn polylactic acid blend hollow-fibre membrane, adopts and does-wet method doughnut spinning technique; Casting solution and core liquid (core liquid is pure water) are extruded through spinneret; Through outer coagulating bath water tank (coagulating agent is a pure water), the solvent in the casting solution (containing pore former, pore-creating agent) is dissolved in the solidification liquid, the polymer precipitation film forming, makes corn polylactic acid blend hollow-fibre membrane.External diameter 1.5mm, internal diameter 0.9mm, porosity is 63%, and it is 0.05 micron that film separates the aperture, and at 0.1MPa, under 25 ℃ the test condition, the pure water water-flowing amount is 730L/m2*hr.
Embodiment 3: with 7 kilograms of dimethylacetylamides, and 1.0 kilograms of corn PLAs, 1.0 kilograms of polyether sulfone polymer; 0.5 the kilogram polyvinylpyrrolidone, 200 grams lithium chlorides, the heated and stirred dissolving is evenly; Process the casting solution of corn polylactic acid blend hollow-fibre membrane; Adopt and do-wet method doughnut spinning technique, casting solution and core liquid (core liquid is pure water) are extruded through spinneret, through coagulating bath water tank (coagulating agent is a pure water); Solvent in the casting solution (containing pore former, pore-creating agent) is dissolved in the solidification liquid, the polymer precipitation film forming, makes corn polylactic acid blend hollow-fibre membrane.External diameter 1.5mm, internal diameter 0.9mm, porosity is 66%, and it is 0.02 micron that film separates the aperture, and at 0.1MPa, under 25 ℃ the test condition, the pure water water-flowing amount is 550L/m2*hr.
Embodiment 4: with 5 kilograms of dimethylacetylamides, and 2 kilograms of N-methyl pyrrolidones, 1.0 kilograms of corn PLAs; 1.2 the kilogram polyvinylidene fluoride polymer, 1.0 kilograms of polyethylene glycol, 200 gram polyvinyl alcohol; 500 gram lithium nitrates, 300 gram silica, the heated and stirred dissolving is evenly; Process the casting solution of corn polylactic acid blend hollow-fibre membrane, adopt and do-wet method doughnut spinning technique, casting solution and core liquid (core liquid is pure water) are extruded through spinneret; Through outer coagulating bath water tank (coagulating agent is a pure water), the solvent in the casting solution (containing pore former, pore-creating agent) is dissolved in the solidification liquid, the polymer precipitation film forming, makes corn polylactic acid blend hollow-fibre membrane.External diameter 1.5mm, internal diameter 0.9mm, porosity is 63%, and it is 0.1 micron that film separates the aperture, and at 0.1MPa, under 25 ℃ the test condition, the pure water water-flowing amount is 930L/m2*hr.
Embodiment 5: with 4 kilograms of dimethylacetylamides, and 3 kilograms of N-methyl pyrrolidones, 1.2 kilograms of corn PLAs; 1.0 the kilogram polyvinylidene fluoride polymer, 1.0 kilograms of polyethylene glycol, 200 gram polyvinyl alcohol; 500 grams lithium chlorides, 500 gram silica, the heated and stirred dissolving is evenly; Process the casting solution of corn polylactic acid blend hollow-fibre membrane, adopt and do-wet method doughnut spinning technique, casting solution and core liquid (core liquid is pure water) are extruded through spinneret; Through outer coagulating bath water tank (coagulating agent is a pure water), the solvent in the casting solution (containing pore former, pore-creating agent) is dissolved in the solidification liquid, the polymer precipitation film forming, makes corn polylactic acid blend hollow-fibre membrane.External diameter 1.5mm, internal diameter 0.9mm, porosity is 65%, and it is 0.1 micron that film separates the aperture, and at 0.1MPa, under 25 ℃ the test condition, the pure water water-flowing amount is 950L/m2*hr.
Total various embodiment; The present invention is mainly through having adopted corn PLA and other polyblend to improve the antibiotic property and the hydrophily of hollow-fibre membrane; And prepare environmentally friendly corn polylactic acid blend hollow-fibre membrane through the solution phase inversion; This film has big flux, hydrophily, antipollution, be prone to superior function such as cleanings, and processing, drink water purifying, middle water reuse, the food that can be applicable to industrial and municipal wastewater is capable, electronics, biological medicine industry be with many fields such as high purity water, feed separation.
Although specifically show and introduced the present invention in conjunction with preferred embodiment; But the those skilled in the art should be understood that; In the spirit and scope of the present invention that do not break away from appended claims and limited; In form with on the details the present invention is made various variations, be protection scope of the present invention.
Claims (10)
1. the manufacturing approach of an environmentally friendly hollow-fibre membrane is characterized in that: comprise the steps:
Step 1: PLA and Kynoar or polyether sulfone, solvent, pore former are mixed by following part by weight:
PLA 2-20%;
Kynoar or polyether sulfone 2-20%;
Solvent 50-86%;
Pore former 0.5-25%;
Step 2: the casting solution that above-mentioned solution stirring, heating for dissolving are evenly made; The core liquid of pore extrudes simultaneously through the spinneret of doughnut spinning-drawing machine with at the spinneret center; Get in the outer solidification liquid then; Solvent in the spinning solution and pore former get into and solidify liquid phase, and polymer blend is because phase transfer and precipitating becomes blend hollow fiber membrane.
2. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: described solvent is an intensive polar solvent; Described intensive polar solvent is the mixture of following one or more solvents: dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone, trichloroethanes, acetone or toluene.
3. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: described core liquid is the mixed liquor of water or water and spin solvent.
4. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: described solidification liquid is the mixed solution of pure water and organic solvent, wherein hundred parts of specific concentrations of weight of organic solvent are 0-30%; Described organic solvent is ethanol or isopropyl alcohol.
5. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1 is characterized in that: described pore former is inorganic pore former or organic polymer pore former or is the two mixture; Described inorganic pore former is following one or more mixture: lithium chloride, lithium nitrate, sodium chloride, calcium chloride, calcium nitrate, titanium dioxide, silica, alundum (Al.
6. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: the content of described inorganic pore former in casting solution is 0.5-20wt%, preferred 1-10 wt%.
7. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1 is characterized in that: the granularity of described inorganic pore former is less than 5 microns, preferred nanoscale.
8. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: described organic polymer pore former is a high molecular weight water soluble polymer; Described high molecular weight water soluble polymer is following one or more mixture: polyethylene glycol, ethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol.
9. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: the molecular weight of described polyethylene glycol is 200-30000 dalton, the molecular weight of polyvinylpyrrolidone is 200-30000 dalton.
10. the manufacturing approach of a kind of environmentally friendly hollow-fibre membrane according to claim 1, it is characterized in that: the content of described organic polymer pore former in casting solution is 1-25wt%, preferred 3-10wt%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961977A (en) * | 2012-12-17 | 2013-03-13 | 中国科学院宁波材料技术与工程研究所 | Preparation method of polylactic-acid hollow fiber dialysis membrane |
| CN103657452A (en) * | 2014-01-02 | 2014-03-26 | 厦门绿邦膜技术有限公司 | Hollow fiber membrane formed by coating corn polylactic onto corn fibermesh tube and preparation method of hollow fiber membrane |
| CN103831019A (en) * | 2014-03-25 | 2014-06-04 | 厦门绿邦膜技术有限公司 | Hollow fiber nanofiltration membrane and preparation method thereof |
| CN104162369A (en) * | 2014-07-31 | 2014-11-26 | 宿迁嵘锦信息科技有限公司 | Antibacterial self-cleaning filtration membrane |
| JP2015188778A (en) * | 2014-03-27 | 2015-11-02 | 株式会社ダイセル | Nf membrane and production method of the same |
| CN107335344A (en) * | 2017-08-22 | 2017-11-10 | 天津工业大学 | Preparation method for the hollow-fibre membrane of dye desalination |
| CN108816048A (en) * | 2018-06-30 | 2018-11-16 | 福州华博立乐新材料科技有限公司 | A kind of preparation method of novel ultrafiltration membrane |
| CN109455995A (en) * | 2016-06-02 | 2019-03-12 | 耿云花 | A kind of antibacterial building concrete manufacture craft |
| CN111530286A (en) * | 2020-04-28 | 2020-08-14 | 南京工业大学 | Hollow fiber nanofiltration membrane and preparation method thereof |
| CN112044279A (en) * | 2020-09-17 | 2020-12-08 | 苏州关怀新材料技术研究有限公司 | Film making liquid for processing vaccine separation membrane and preparation method thereof |
| CN116103774A (en) * | 2023-02-23 | 2023-05-12 | 青岛大学 | Preparation method and application of polylactic acid hollow fiber aerogel |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961977A (en) * | 2012-12-17 | 2013-03-13 | 中国科学院宁波材料技术与工程研究所 | Preparation method of polylactic-acid hollow fiber dialysis membrane |
| CN103657452A (en) * | 2014-01-02 | 2014-03-26 | 厦门绿邦膜技术有限公司 | Hollow fiber membrane formed by coating corn polylactic onto corn fibermesh tube and preparation method of hollow fiber membrane |
| CN103831019A (en) * | 2014-03-25 | 2014-06-04 | 厦门绿邦膜技术有限公司 | Hollow fiber nanofiltration membrane and preparation method thereof |
| JP2015188778A (en) * | 2014-03-27 | 2015-11-02 | 株式会社ダイセル | Nf membrane and production method of the same |
| CN104162369A (en) * | 2014-07-31 | 2014-11-26 | 宿迁嵘锦信息科技有限公司 | Antibacterial self-cleaning filtration membrane |
| CN109455995A (en) * | 2016-06-02 | 2019-03-12 | 耿云花 | A kind of antibacterial building concrete manufacture craft |
| CN107335344B (en) * | 2017-08-22 | 2020-11-03 | 天津工业大学 | Preparation method of hollow fiber membrane for dye desalination |
| CN107335344A (en) * | 2017-08-22 | 2017-11-10 | 天津工业大学 | Preparation method for the hollow-fibre membrane of dye desalination |
| CN108816048A (en) * | 2018-06-30 | 2018-11-16 | 福州华博立乐新材料科技有限公司 | A kind of preparation method of novel ultrafiltration membrane |
| CN111530286A (en) * | 2020-04-28 | 2020-08-14 | 南京工业大学 | Hollow fiber nanofiltration membrane and preparation method thereof |
| CN111530286B (en) * | 2020-04-28 | 2022-02-11 | 南京工业大学 | Hollow fiber nanofiltration membrane and preparation method thereof |
| CN112044279A (en) * | 2020-09-17 | 2020-12-08 | 苏州关怀新材料技术研究有限公司 | Film making liquid for processing vaccine separation membrane and preparation method thereof |
| CN116103774A (en) * | 2023-02-23 | 2023-05-12 | 青岛大学 | Preparation method and application of polylactic acid hollow fiber aerogel |
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Application publication date: 20120718 |