CN102198371A - Blend membrane of polyvinyl butyral (PVB) and polyvinylidene fluoride (PVDF) and preparation method thereof - Google Patents
Blend membrane of polyvinyl butyral (PVB) and polyvinylidene fluoride (PVDF) and preparation method thereof Download PDFInfo
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- CN102198371A CN102198371A CN2011101358689A CN201110135868A CN102198371A CN 102198371 A CN102198371 A CN 102198371A CN 2011101358689 A CN2011101358689 A CN 2011101358689A CN 201110135868 A CN201110135868 A CN 201110135868A CN 102198371 A CN102198371 A CN 102198371A
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- butyral resin
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Abstract
The invention relates to a blend membrane of polyvinyl butyral (PVB) and polyvinylidene fluoride (PVDF) and a preparation method thereof. The blend membrane is composed of PVB and PVDF based on the mass ratio of 1-9:1-9. The preparation method comprises the following steps: (1) dissolving the PVB and the PVDF in a solvent, stirring at the temperature of 90 DEG C until the PVB and the PVDF are dissolved, standing still and defoaming to obtain casting solution; and (2) pouring the casting solution onto one end of a glass sheet and scraping to form a liquid-state membrane, placing the liquid-state membrane in a water bath, taking out the formed membrane from the water bath after the thin membrane falls off, washing the formed membrane with distilled water, soaking the washed membrane in glycerol aqueous solution with concentration of 50vol%, and finally naturally drying to obtain the blend membrane. The preparation method provided by the invention has the advantages of simple process and low cost and is easy for industrial production; and the obtained blend membrane has the advantages of good permeability, high water flux, high strength, better damage resistance and good application prospect.
Description
Technical field
The invention belongs to the polyvinylidene fluoride film field, particularly a kind of polyvinyl butyral resin and polyvinylidene fluoride blending film and preparation method thereof.
Background technology
Kynoar (PVDF) is a kind of semicrystalline polymer, C-F bond distance is short, bond energy reaches 486kJ/mol by force, so PVDF has favorable mechanical performance and stable chemical property, be a kind of new polymers membrane material of function admirable, can be prepared into that a class is heat-resisting, wear-resisting, the novel high-performance diffusion barrier of acid and alkali-resistance, organic solvent-resistant.In addition, the PVDF material price is cheap, and therefore, pvdf membrane has very big market value.20th century the mid-80, U.S. Millipore company at first develops Durepore type microporous barrier with it, and introduces to the market.But because the PVDF surface can be low, hydrophobicity is strong, and the pvdf membrane that makes is easy to generate absorption and pollutes at aspects such as sewage disposal, water-oil separating, protein medicaments separation, and the flux decay of film is very fast, the service life of having reduced film.Therefore, the improvement of the hydrophily of polyvinylidene fluoride film has great importance.
Adopt Kynoar to report as existing many documents of material of preparing and patent.People such as He Chunju have reported to have the preparation method's (application number: 200810202882) that improves hydrophilic blend polyvinylidene fluoride hollow-fibre membrane, its technology of preparing is that the casting solution that adopts Kynoar, polyether sulfone, cellulose derivative, pore former and solvent to be mixed with is made spun filament, spun filament again through the above biaxial tension in four roads and appropriateness retraction, washing, protect the hole and handle after, reel the blend polyvinylidene fluoride hollow-fibre membrane; People such as Ma Jun have reported that (application number: 200710072442.7), it is to be made according to percentage by weight by Kynoar, molysite and dimethylacetylamide for a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane and preparation method thereof; People such as Ruan Wenxiang have reported preparation method's (application number: CN200910155288.9) of dry high-hydrophilic polyvinylidene fluoride hollow-fibre membrane; People such as Xiao Changfa have reported that (application number: 200710058333), it is to be made according to percentage by weight by Kynoar, polyvinyl alcohol and dimethyl sulfoxide (DMSO) to a kind of polyvinylidene fluoride film hydrophilically modified method.Also do not seen relevant document and patent report up to now to polyvinyl butyral resin (PVB), Kynoar (PVDF) blend system film.
Polyvinyl butyral resin (PVB) hydrophily is strong, and physical and chemical performance and filming performance are good, but the carbonated drink flux is low, and film is hard and crisp.Mainly contain about research: PVB/PVC, PVB/PES PVB and other macromolecular material blend development of new membrane material.These researchs mainly are to utilize the hydrophily of PVB that PVC film, PES film are carried out hydrophilic modifying.Patent about the PVB film is not appeared in the newspapers.
Summary of the invention
Technical problem to be solved by this invention provides a kind of polyvinyl butyral resin and polyvinylidene fluoride blending film and preparation method thereof, and this method technology is simple, and cost is low, is easy to industrialization; The blend film transparent performance of preparation is good, the water flux height, and the intensity height has anti-damage performance preferably, and good prospects for application is arranged.
A kind of polyvinyl butyral resin of the present invention and polyvinylidene fluoride blending film is characterized in that: blend film is that 1～9: 1～9 polyvinyl butyral resin and Kynoar are formed by mass ratio.
Described blend film is a flat sheet membrane.
Described blend film thickness is 50～200 μ m, and pure water flux is 18.54～430.64Lm under the 0.18MPa pressure
-2H
-1, hot strength is 417.5～786Ncm
-2
The preparation method of a kind of polyvinyl butyral resin of the present invention and polyvinylidene fluoride blending film comprises:
(1) with polyvinyl butyral resin and Kynoar by mass ratio 1～9: 1～9 is dissolved in the solvent, stir down until dissolving at 90 ℃, leave standstill, deaeration gets casting solution, wherein, polyvinyl butyral resin and Kynoar gross mass percent concentration are 22～26%, and the solvent quality percent concentration is 74～78%;
(2) environment temperature be room temperature, ambient humidity be 55% and the casting solution temperature be under 90 ℃ the condition, above-mentioned casting solution is poured over an end of glass plate, scrape and make liquid film, put into 10～25 ℃ water-bath then, treat to take out from water-bath after film comes off, with the distilled water washing, the glycerine water solution with 50vol% soaks again, air dry, promptly.
Solvent in the described step (1) is one or more in dimethyl formamide, dimethylacetylamide, the N-N-methyl-2-2-pyrrolidone N-.
Liquid film thickness in the described step (2) is 0.2mm.
Beneficial effect
(1) technology of the present invention is simple, and cost is low, is easy to industrialization;
(2) the blend film transparent performance of the present invention's preparation is good, the water flux height, and the intensity height has anti-damage performance preferably, and good prospects for application is arranged.
Description of drawings
Fig. 1 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, when the casting solution temperature is 90 ℃, and the section structure electron-microscope scanning figure of pure PVB film;
Fig. 2 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, when the casting solution temperature is 90 ℃, and the section structure electron-microscope scanning figure of pure pvdf membrane;
Fig. 3 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 9: 1 PVB/PVDF blend film;
Fig. 4 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 8: 2 PVB/PVDF blend film;
Fig. 5 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 7: 3 PVB/PVDF blend film;
Fig. 6 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 6: 4 PVB/PVDF blend film;
Fig. 7 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 5: 5 PVB/PVDF blend film;
Fig. 8 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 4: 6 PVB/PVDF blend film;
Fig. 9 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 3: 7 PVB/PVDF blend film;
Figure 10 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 2: 8 PVB/PVDF blend film;
Figure 11 is 23wt% for polymer content, and the coagulation bath temperature is 5 ℃, and when the casting solution temperature was 90 ℃, mass ratio was the section structure electron-microscope scanning figure of 1: 9 PVB/PVDF blend film.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
With total mass concentration is that to join mass concentration be 77wt% solvent N for 23wt% polyvinyl butyral resin and Kynoar, in the N-dimethylacetylamide, be placed in the water-bath constant temperature and stir down until dissolving fully for 90 ℃, leave standstill again, deaeration, get casting solution, standby; Environment temperature be room temperature, ambient humidity be 55% and the casting solution temperature be under 90 ℃ the condition, the temperature of clean glass plate, glass bar and casting solution is consistent, the casting solution for preparing is poured over an end of glass plate, scrape the liquid film of making 0.2mm with glass bar, put into the water-bath film forming immediately, treat from water-bath, to take out after film comes off, fully wash, soak and remove the solvent that remains in the film with distilled water, glycerine water solution with 50vol% soaks 24h again, takes out in air at last and dries naturally.
The mass ratio of the described polyvinyl butyral resin/Kynoar of said method is respectively 10/0,9/1,8/2,7/3,6/4,5/5,4/6,3/7,2/8,1/9,0/10, and the flat sheet membrane of institute's striking is measured its pure water flux, the pure water flux (Lm of gained under 0.18MPa pressure
-2H
-1) analog value is respectively 5.00,18.54,153.44,259.53,282.48,306.70,78.29,39.87,28.43,22.35,17.87; Hot strength (Ncm
-2) analog value is respectively 963.5,786,673.5,603.5.The result shows, the mass ratio of polyvinyl butyral resin/Kynoar is that 7/3 flat sheet membrane combination property is best.
The mass ratio of further measuring polyvinyl butyral resin/Kynoar respectively is 10/0,9/1,8/2,7/3, the contact angle on 0/10 flat sheet membrane surface, and the contact angle data of gained are 61.06 °, 69.31 °, 69.71 °, 69.90 °, 78.33 °.The result shows that the hydrophily of blend film is than the good hydrophilic property of pvdf membrane, and the adding of PVB has improved the hydrophily of pvdf membrane.
Embodiment 2
Polyvinyl butyral resin and Kynoar are joined solvent N by mass ratio at 7: 3, and in the N-dimethylacetylamide, polyvinyl butyral resin and Kynoar total mass concentration are 22wt%, 23wt%, 24wt%, 25wt%, 26wt%.Environment temperature be room temperature, ambient humidity be 55% and the casting solution temperature be under 90 ℃ the condition, the temperature of clean glass plate, glass bar and casting solution is consistent, the casting solution for preparing is poured over an end of glass plate, scrape the liquid film of making 0.2mm with glass bar, put into the water-bath film forming immediately, treat from water-bath, to take out after film comes off, fully wash, soak and remove the solvent that remains in the film with distilled water, glycerine water solution with 50vol% soaks 24h again, takes out in air at last and dries naturally.The flat sheet membrane of institute's striking is measured its pure water flux, the pure water flux (Lm of gained under 0.18MPa pressure
-2H
-1) analog value is respectively 430.64,418.36,259.53,214.03,205.84; Hot strength (Ncm
-2) analog value is respectively 417.5,491.5,603.5,728.5,817.The result shows that the concentration of polyvinyl butyral resin and Kynoar is that the flat sheet membrane combination property of 23wt% is best.
Claims (6)
1. polyvinyl butyral resin and polyvinylidene fluoride blending film is characterized in that: blend film is that 1～9: 1～9 polyvinyl butyral resin and Kynoar are formed by mass ratio.
2. a kind of polyvinyl butyral resin according to claim 1 and polyvinylidene fluoride blending film is characterized in that: described blend film is a flat sheet membrane.
3. a kind of polyvinyl butyral resin according to claim 1 and polyvinylidene fluoride blending film is characterized in that: described blend film thickness is 50～200 μ m, and pure water flux is 18.54～430.64Lm under the 0.18MPa pressure
-2H
-1, hot strength is 417.5～786Ncm
-2
4. the preparation method of polyvinyl butyral resin and polyvinylidene fluoride blending film comprises:
(1) with polyvinyl butyral resin and Kynoar by mass ratio 1～9: 1～9 is dissolved in the solvent, stir down until dissolving at 90 ℃, leave standstill, deaeration gets casting solution, wherein, polyvinyl butyral resin and Kynoar gross mass percent concentration are 22～26%, and the solvent quality percent concentration is 74～78%;
(2) environment temperature be room temperature, ambient humidity be 55% and the casting solution temperature be under 90 ℃ the condition, above-mentioned casting solution is poured over an end of glass plate, scrape and make liquid film, put into 10～25 ℃ water-bath then, treat to take out from water-bath after film comes off, with the distilled water washing, the glycerine water solution with 50vol% soaks again, air dry, promptly.
5. the preparation method of a kind of polyvinyl butyral resin according to claim 4 and polyvinylidene fluoride blending film is characterized in that: the solvent in the described step (1) is one or more in dimethyl formamide, dimethylacetylamide, the N-N-methyl-2-2-pyrrolidone N-.
6. the preparation method of a kind of polyvinyl butyral resin according to claim 4 and polyvinylidene fluoride blending film is characterized in that: the liquid film thickness in the described step (2) is 0.2mm.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614785A (en) * | 2012-04-12 | 2012-08-01 | 东华大学 | Polrvinyl chloride and cellulose acetate blend membrane and preparation method thereof |
| CN103861481A (en) * | 2014-04-03 | 2014-06-18 | 陕西科技大学 | Method for preparing polyvinylidene-fluoride porous membrane |
| CN105854648A (en) * | 2016-05-12 | 2016-08-17 | 中国石油集团东北炼化工程有限公司葫芦岛设计院 | Preparation method of high-throughput, long-period and anti-pollution ultrafiltration membrane |
| CN108310988A (en) * | 2018-01-31 | 2018-07-24 | 天津科技大学 | High-performance PU/PVB/FF filter membranes |
| CN108483613A (en) * | 2018-04-19 | 2018-09-04 | 昆明理工大学 | Water wetted material doping and blending film carries nano zero valence iron composite material and preparation method and application |
| CN110526412A (en) * | 2019-09-18 | 2019-12-03 | 浙江海洋大学 | The processing method of chromate waste water based on microdisk electrode |
| CN111992059A (en) * | 2020-09-01 | 2020-11-27 | 安徽美邦树脂科技有限公司 | PVB-based ultrafiltration membrane and preparation method thereof |
| CN114588786A (en) * | 2021-12-14 | 2022-06-07 | 宁波水艺膜科技发展有限公司 | Microporous membrane containing cross-linked hydrophilic polymer and preparation method thereof |
| CN114588792A (en) * | 2021-11-18 | 2022-06-07 | 宁波水艺膜科技发展有限公司 | Polyvinyl butyral blending enhanced polyvinylidene chloride film and preparation method thereof |
| CN114891250A (en) * | 2022-05-05 | 2022-08-12 | 中海油天津化工研究设计院有限公司 | Method for preparing blend membrane by non-solvent phase separation method |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614785A (en) * | 2012-04-12 | 2012-08-01 | 东华大学 | Polrvinyl chloride and cellulose acetate blend membrane and preparation method thereof |
| CN103861481A (en) * | 2014-04-03 | 2014-06-18 | 陕西科技大学 | Method for preparing polyvinylidene-fluoride porous membrane |
| CN105854648A (en) * | 2016-05-12 | 2016-08-17 | 中国石油集团东北炼化工程有限公司葫芦岛设计院 | Preparation method of high-throughput, long-period and anti-pollution ultrafiltration membrane |
| CN108310988B (en) * | 2018-01-31 | 2021-01-26 | 天津科技大学 | High-performance PU/PVB/FF filtering membrane |
| CN108310988A (en) * | 2018-01-31 | 2018-07-24 | 天津科技大学 | High-performance PU/PVB/FF filter membranes |
| CN108483613A (en) * | 2018-04-19 | 2018-09-04 | 昆明理工大学 | Water wetted material doping and blending film carries nano zero valence iron composite material and preparation method and application |
| CN108483613B (en) * | 2018-04-19 | 2021-05-14 | 昆明理工大学 | Hydrophilic material doped blending membrane loaded nano zero-valent iron composite material and preparation method and application thereof |
| CN110526412B (en) * | 2019-09-18 | 2022-03-18 | 浙江海洋大学 | Treatment method of chromium-containing wastewater based on microalgae culture |
| CN110526412A (en) * | 2019-09-18 | 2019-12-03 | 浙江海洋大学 | The processing method of chromate waste water based on microdisk electrode |
| CN111992059A (en) * | 2020-09-01 | 2020-11-27 | 安徽美邦树脂科技有限公司 | PVB-based ultrafiltration membrane and preparation method thereof |
| CN114588792A (en) * | 2021-11-18 | 2022-06-07 | 宁波水艺膜科技发展有限公司 | Polyvinyl butyral blending enhanced polyvinylidene chloride film and preparation method thereof |
| CN114588792B (en) * | 2021-11-18 | 2023-09-05 | 宁波水艺膜科技发展有限公司 | Polyvinyl butyral blending reinforced polyvinylidene chloride ultrafiltration membrane and preparation method thereof |
| CN114588786A (en) * | 2021-12-14 | 2022-06-07 | 宁波水艺膜科技发展有限公司 | Microporous membrane containing cross-linked hydrophilic polymer and preparation method thereof |
| CN114891250A (en) * | 2022-05-05 | 2022-08-12 | 中海油天津化工研究设计院有限公司 | Method for preparing blend membrane by non-solvent phase separation method |
| CN114891250B (en) * | 2022-05-05 | 2023-09-15 | 中海油天津化工研究设计院有限公司 | Method for preparing blend membrane by non-solvent phase separation method |
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Application publication date: 20110928 |