CN105289329A - Preparation method of PVDF/nanometer TiO2 blending modified flat sheet membrane module - Google Patents
Preparation method of PVDF/nanometer TiO2 blending modified flat sheet membrane module Download PDFInfo
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- CN105289329A CN105289329A CN201510781329.0A CN201510781329A CN105289329A CN 105289329 A CN105289329 A CN 105289329A CN 201510781329 A CN201510781329 A CN 201510781329A CN 105289329 A CN105289329 A CN 105289329A
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Abstract
The invention relates to a preparation method of a PVDF/nanometer TiO2 blending modified flat sheet membrane module, and belongs to the field of a flat sheet membrane establishment and production. Polyvinylidene fluoride is placed in a sodium hydroxide solution, the solution is stirred for mixing and permitted to stand, isopropyl acrylamide is added in to the solution, and a polymerization reaction is carried out with the protection of nitrogen and irradiation by ultraviolet light. A mixed liquor is prepared and is used as a solvent, TiO2 is added, a high speed stirring is carried out, a defoaming is carried out, after heating and insulation, a bovine serum albumin solution is added, after cooling, the solution is uniformly smeared on a piece of non-woven fabric, the fabric is scraped into a membrane, and an immersion is carried out to obtain the module. The invention has the beneficial effects that the bad hydrophilicity of the membrane is improved, the transmembrane pressure is reduced, the flat sheet membrane module is not easy to be polluted by organic matters and microorganisms, the preparation step is simple, and the cost is low.
Description
Technical field
The present invention relates to a kind of PVDF/ nano-TiO
2blending and modifying plate film assembly preparation method, belongs to Flat Membrane and sets up production field.
Background technology
At present, China's major part sewage treatment plant adopts conventional activated sludge process and biomembrane process.Traditional waste water treatment process exist major defect be: floor space is large, effluent quality is poor, sludge bulking, a large amount of excess sludge of generation and energy consumption high.In order to overcome the difficult problem existing for traditional waste water treatment process, various high-efficiency sewage treatment technology that is novel, improvement arises at the historic moment in recent years, membrane separation technique wherein, particularly the application in the treatment of waste water of membrane bioreactor (MembraneBio-Reactor, MBR) technology causes extensive concern both domestic and external.This technique, compared with traditional waste water treatment process, has that effluent quality is good, occupation area of equipment is little, sludge concentration is high, excess sludge production is low, be convenient to the advantages such as Automated condtrol.This technology demonstrates its advantage at reusing sewage and organic wastewater with difficult degradation thereby process field, and is widely applied in Practical Project.But fouling membrane can affect process stabilizing to be run, and determines the replacement frequency of film, the more wide popularization and application of yoke membrane bioreactor.Treatment scale is in the Sewage Reuse System of 240m3/d, and power cost accounts for 21% of operating cost; For lessening membrane fouling, membrane biological reactor process gas-water ratio is usually about 40: 1, and the energy consumption of aeration accounts for more than 96% of power cost.Effective membrane fouling control technology can increase membrane flux, reduces energy consumption, strengthens the stability of a system, extends the service life of film, reduce operating cost, and therefore, the research of control membrane fouling technology is very necessary.
Fouling membrane refers to that particulate, colloidal particle or solute transportation in processed material is owing to existing physics, chemistry or biological interaction with film, cause absorption in film surface or fenestra, deposited particles, colloidal particle or solute transportation, cause membrane aperture to diminish and even directly block fenestra, make film produce the phenomenon of the reversible or irreversible change of flux and stalling characteristic, one of current Main Bottleneck affecting application of membrane is exactly fouling membrane.
Summary of the invention
The technical problem that the present invention mainly solves: membrane aperture can be caused to diminish for current fouling membrane and even directly block fenestra, makes film produce the phenomenon of the reversible or irreversible change of flux and stalling characteristic, provides a kind of PVDF/ nano-TiO
2blending and modifying plate film assembly preparation method, the method is mainly poor by the hydrophily improving film, reduces transmembrane pressure, makes plate film assembly not be vulnerable to the pollution of organic matter and microorganism, and operating procedure is simple, economical and efficient.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) Kynoar of 1 ~ 2kg is placed in the sodium hydroxide solution that mass concentration is 80%, after being uniformly mixed 20 ~ 25min, after leaving standstill 10 ~ 15min, the N-isopropylacrylamide that mass concentration is 10% is added again to it, under the protection of nitrogen, utilize the irradiation of ultraviolet light, make it be polymerized 20 ~ 30min;
(2) with above-mentioned obtained mixed liquor for solvent, add TiO to it
2, the amount added and the mass ratio of mixed liquor are 1:2, and high-speed stirred makes uniform solution, control rate is 300 ~ 450r/min, to be mixed evenly after, be 15 ~ 30 DEG C in temperature, under 0.1 ~ 0.5 atmospheric pressure after deaeration 10 ~ 12h, then be warming up to 40 ~ 45 DEG C, insulation 1 ~ 2h;
(3) after insulation terminates, add bovine serum albumen solution to it, the volume ratio of the mixed solution of wherein bovine serum albumen solution and insulation is 1:1, after being uniformly mixed, with the speed of 2 DEG C/min, programmed cooling is carried out to it, is cooled to 20 ~ 30 DEG C, leave standstill 15 ~ 20min, take out, it be applied in uniformly on non-woven fabrics, spread to 300 ~ 450 μm of films, the water film made being placed in 10 ~ 15 DEG C soaks 20 ~ 40min, take out, in plate film assembly.
The preparation of the bovine serum albumen solution in above-mentioned steps (2): bovine serum albumin is solute, solvent to be pH be 7 ~ 7.5 phosphate buffer, wherein phosphatic concentration is 0.025mol/L.
The invention has the beneficial effects as follows:
(1) hydrophily improving film is poor, reduces transmembrane pressure, makes plate film assembly not be vulnerable to the pollution of organic matter and microorganism;
(2) preparation process is simple, and cost is low.
Detailed description of the invention
First the Kynoar of 1 ~ 2kg is placed in the sodium hydroxide solution that mass concentration is 80%, after being uniformly mixed 20 ~ 25min, after leaving standstill 10 ~ 15min, the N-isopropylacrylamide that mass concentration is 10% is added again to it, under the protection of nitrogen, utilize the irradiation of ultraviolet light, make it be polymerized 20 ~ 30min; With above-mentioned obtained mixed liquor for solvent, add TiO to it
2, the amount added and the mass ratio of mixed liquor are 1:2, and high-speed stirred makes uniform solution, control rate is 300 ~ 450r/min, to be mixed evenly after, be 15 ~ 30 DEG C in temperature, under 0.1 ~ 0.5 atmospheric pressure after deaeration 10 ~ 12h, then be warming up to 40 ~ 45 DEG C, insulation 1 ~ 2h; After insulation terminates, add bovine serum albumen solution to it, the volume ratio of the mixed solution of wherein bovine serum albumen solution and insulation is 1:1, after being uniformly mixed, with the speed of 2 DEG C/min, programmed cooling is carried out to it, is cooled to 20 ~ 30 DEG C, leave standstill 15 ~ 20min, take out, it be applied in uniformly on non-woven fabrics, spread to 300 ~ 450 μm of films, the water film made being placed in 10 ~ 15 DEG C soaks 20 ~ 40min, take out, in plate film assembly.Wherein bovine serum albumin is solute, solvent to be pH be 7 ~ 7.5 phosphate buffer, wherein phosphatic concentration is 0.025mol/L.
Example 1
First the Kynoar of 2kg is placed in the sodium hydroxide solution that mass concentration is 80%, after being uniformly mixed 20min, after leaving standstill 10min, the N-isopropylacrylamide that mass concentration is 10% is added again to it, under the protection of nitrogen, utilize the irradiation of ultraviolet light, make its polyase 13 0min; With above-mentioned obtained mixed liquor for solvent, add TiO to it
2, the amount added and the mass ratio of mixed liquor are 1:2, and high-speed stirred makes uniform solution, and control rate is 450r/min, to be mixed evenly after, be 30 DEG C in temperature, under 0.5 atmospheric pressure after deaeration 12h, then be warming up to 45 DEG C, insulation 2h; After insulation terminates, add bovine serum albumen solution to it, the volume ratio of the mixed solution of wherein bovine serum albumen solution and insulation is 1:1, after being uniformly mixed, with the speed of 2 DEG C/min, programmed cooling is carried out to it, is cooled to 30 DEG C, leave standstill 20min, take out, it is applied on non-woven fabrics uniformly, spreads to 450 μm of films, the water that the film made is placed in 15 DEG C is soaked 40min, take out, in plate film assembly.Wherein bovine serum albumin is solute, solvent to be pH be 7.5 phosphate buffer, wherein phosphatic concentration is 0.025mol/L.The hydrophily improving film is poor, reduces transmembrane pressure, makes plate film assembly not be vulnerable to the pollution of organic matter and microorganism, and operating procedure is simple, economical and efficient.
Example 2
First the Kynoar of 1kg is placed in the sodium hydroxide solution that mass concentration is 80%, after being uniformly mixed 20min, after leaving standstill 10min, the N-isopropylacrylamide that mass concentration is 10% is added again to it, under the protection of nitrogen, utilize the irradiation of ultraviolet light, make it be polymerized 20min; With above-mentioned obtained mixed liquor for solvent, add TiO to it
2, the amount added and the mass ratio of mixed liquor are 1:2, and high-speed stirred makes uniform solution, and control rate is 300r/min, to be mixed evenly after, be 15 DEG C in temperature, under 0.1 atmospheric pressure after deaeration 10h, then be warming up to 40 DEG C, insulation 1h; After insulation terminates, add bovine serum albumen solution to it, the volume ratio of the mixed solution of wherein bovine serum albumen solution and insulation is 1:1, after being uniformly mixed, with the speed of 2 DEG C/min, programmed cooling is carried out to it, be cooled to 30 DEG C, leave standstill 20min and take out, it is applied on non-woven fabrics uniformly, spread to 450 μm of films, the water that the film made is placed in 15 DEG C is soaked 40min, takes out, in plate film assembly.Wherein bovine serum albumin is solute, solvent to be pH be 7.5 phosphate buffer, wherein phosphatic concentration is 0.025mol/L.The hydrophily improving film is poor, reduces transmembrane pressure, makes plate film assembly not be vulnerable to the pollution of organic matter and microorganism, and operating procedure is simple, economical and efficient.
Example 3
First the Kynoar of 1.5kg is placed in the sodium hydroxide solution that mass concentration is 80%, after being uniformly mixed 22min, after leaving standstill 12min, the N-isopropylacrylamide that mass concentration is 10% is added again to it, under the protection of nitrogen, utilize the irradiation of ultraviolet light, make it be polymerized 25min; With above-mentioned obtained mixed liquor for solvent, add TiO to it
2, the amount added and the mass ratio of mixed liquor are 1:2, and high-speed stirred makes uniform solution, and control rate is 450r/min, to be mixed evenly after, be 30 DEG C in temperature, under 0.5 atmospheric pressure after deaeration 12h, then be warming up to 45 DEG C, insulation 2h; After insulation terminates, add bovine serum albumen solution to it, the volume ratio of the mixed solution of wherein bovine serum albumen solution and insulation is 1:1, after being uniformly mixed, with the speed of 2 DEG C/min, programmed cooling is carried out to it, is cooled to 30 DEG C, leave standstill 20min, take out, it is applied on non-woven fabrics uniformly, spreads to 300 μm of films, the water that the film made is placed in 12 DEG C is soaked 30min, take out, in plate film assembly.Wherein bovine serum albumin is solute, solvent to be pH be 7 phosphate buffer, wherein phosphatic concentration is 0.025mol/L.The hydrophily improving film is poor, reduces transmembrane pressure, makes plate film assembly not be vulnerable to the pollution of organic matter and microorganism, and operating procedure is simple, economical and efficient.
Claims (2)
1. a PVDF/ nano-TiO
2blending and modifying plate film assembly preparation method, is characterized in that concrete preparation process is:
(1) Kynoar of 1 ~ 2kg is placed in the sodium hydroxide solution that mass concentration is 80%, after being uniformly mixed 20 ~ 25min, after leaving standstill 10 ~ 15min, the N-isopropylacrylamide that mass concentration is 10% is added again to it, under the protection of nitrogen, utilize the irradiation of ultraviolet light, make it be polymerized 20 ~ 30min;
(2) with above-mentioned obtained mixed liquor for solvent, add TiO to it
2, the amount added and the mass ratio of mixed liquor are 1:2, and high-speed stirred makes uniform solution, control rate is 300 ~ 450r/min, to be mixed evenly after, be 15 ~ 30 DEG C in temperature, under 0.1 ~ 0.5 atmospheric pressure after deaeration 10 ~ 12h, then be warming up to 40 ~ 45 DEG C, insulation 1 ~ 2h;
(3) after insulation terminates, add bovine serum albumen solution to it, the volume ratio of the mixed solution of wherein bovine serum albumen solution and insulation is 1:1, after being uniformly mixed, with the speed of 2 DEG C/min, programmed cooling is carried out to it, is cooled to 20 ~ 30 DEG C, leave standstill 15 ~ 20min, take out, it be applied in uniformly on non-woven fabrics, spread to 300 ~ 450 μm of films, the water film made being placed in 10 ~ 15 DEG C soaks 20 ~ 40min, take out, in plate film assembly.
2. a kind of PVDF/ nano-TiO according to claim 2
2blending and modifying plate film assembly preparation method, it is characterized in that: the preparation of the bovine serum albumen solution in above-mentioned steps (2): bovine serum albumin is solute, solvent to be pH be 7 ~ 7.5 phosphate buffer, wherein phosphatic concentration is 0.025mol/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112023724A (en) * | 2020-08-25 | 2020-12-04 | 广州大学 | Modified polyvinylidene fluoride ultrafiltration membrane and preparation method thereof |
| CN112023723A (en) * | 2019-07-01 | 2020-12-04 | 江苏久吾高科技股份有限公司 | Hollow fiber membrane and manufacturing method thereof |
| CN115445453A (en) * | 2022-09-05 | 2022-12-09 | 大连理工大学 | Method for preparing ultra-high flux super-hydrophobic PVDF membrane by utilizing solute solvent co-crystallization |
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| CN101711950A (en) * | 2009-11-23 | 2010-05-26 | 天津工业大学 | Flat separation membrane |
| CN101905123A (en) * | 2009-06-03 | 2010-12-08 | 中国科学院大连化学物理研究所 | Blending modification method of polyvinylidene fluoride ultrafiltration membrane |
| CN102512973A (en) * | 2011-12-14 | 2012-06-27 | 东华大学 | Preparation method of low temperature plasma grafted protein modified polyvinylidene fluoride film |
| CN102728240A (en) * | 2012-07-05 | 2012-10-17 | 常州大学 | Novel polyvinylidene fluoride film as well as preparation method and application thereof |
| CN103182257A (en) * | 2013-04-07 | 2013-07-03 | 福州大学 | Temperature-sensitive self-cleaning polyvinylidene fluoride film and preparation method thereof |
| CN103394294A (en) * | 2013-08-08 | 2013-11-20 | 哈尔滨工业大学 | Preparation method of high-performance PVDF composite ultrafiltration membrane with surface loaded with TiO2 thin membrane |
| US20140076797A1 (en) * | 2012-09-20 | 2014-03-20 | Korea Institute Of Science And Technology | Fiber-based filter with nanonet layer and preparation method thereof |
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- 2015-11-14 CN CN201510781329.0A patent/CN105289329A/en active Pending
Patent Citations (7)
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| CN101905123A (en) * | 2009-06-03 | 2010-12-08 | 中国科学院大连化学物理研究所 | Blending modification method of polyvinylidene fluoride ultrafiltration membrane |
| CN101711950A (en) * | 2009-11-23 | 2010-05-26 | 天津工业大学 | Flat separation membrane |
| CN102512973A (en) * | 2011-12-14 | 2012-06-27 | 东华大学 | Preparation method of low temperature plasma grafted protein modified polyvinylidene fluoride film |
| CN102728240A (en) * | 2012-07-05 | 2012-10-17 | 常州大学 | Novel polyvinylidene fluoride film as well as preparation method and application thereof |
| US20140076797A1 (en) * | 2012-09-20 | 2014-03-20 | Korea Institute Of Science And Technology | Fiber-based filter with nanonet layer and preparation method thereof |
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| CN103394294A (en) * | 2013-08-08 | 2013-11-20 | 哈尔滨工业大学 | Preparation method of high-performance PVDF composite ultrafiltration membrane with surface loaded with TiO2 thin membrane |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112023723A (en) * | 2019-07-01 | 2020-12-04 | 江苏久吾高科技股份有限公司 | Hollow fiber membrane and manufacturing method thereof |
| CN112023724A (en) * | 2020-08-25 | 2020-12-04 | 广州大学 | Modified polyvinylidene fluoride ultrafiltration membrane and preparation method thereof |
| CN115445453A (en) * | 2022-09-05 | 2022-12-09 | 大连理工大学 | Method for preparing ultra-high flux super-hydrophobic PVDF membrane by utilizing solute solvent co-crystallization |
| CN115445453B (en) * | 2022-09-05 | 2023-07-25 | 大连理工大学 | Method for preparing superhigh flux superhydrophobic PVDF membrane by solute solvent co-crystallization |
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