CN100534595C - Temperature-sensitive separating film and preparation method thereof - Google Patents
Temperature-sensitive separating film and preparation method thereof Download PDFInfo
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- CN100534595C CN100534595C CNB2007100472731A CN200710047273A CN100534595C CN 100534595 C CN100534595 C CN 100534595C CN B2007100472731 A CNB2007100472731 A CN B2007100472731A CN 200710047273 A CN200710047273 A CN 200710047273A CN 100534595 C CN100534595 C CN 100534595C
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Abstract
The invention relates to a thermo-sensitive separating membrane, consisting of hydroxypropyl cellulose and polyacrylonitrile. The molecular weight of the membrane is 80000 to 100000, and the thickness of the membrane layer is 50 to 200 microns. The preparation process is as the following: (1) the hydroxypropyl cellulose and polyacrylonitrile are weighted and prepared, and then are dried and dissolved into a solvent to obtain a mixed solution; (2) a membrane preparation plate is pre-heated, and the membrane is shaved through a salivation membrane preparation method; (3) the obtained membrane is pre-vaporized and is dipped into the mixed solution and is curdled; (4) the membrane is taken out and the surface solution is removed, and then the membrane is dried to obtain the thermo-sensitive separating membrane. The membrane has the thermo-sensitivity, and then the water flux and the space ratio, etc. separation capability of the membrane may change suddenly when the temperature of the membrane passes some point and the membrane has reversibility; so the invention can be applied to big molecule separation, medicine release, etc. biological medicine fields.
Description
Technical field
The invention belongs to the Thermosensitive macromolecular membranes field, particularly relate to blend polymeric membrane and preparation method thereof.
Background technology
In phase later 1970s, intellectual material only is included in embedding Fibre Optical Sensor in the composite.And now, intellectual material is various in style, generally comprises metal intellectual material, nonmetal intellectual material and polymer intelligent material.It has been widely used in fields such as building, dam, bridge, pipeline, steamer and ground traffic tools, life science, bionics, electronics, numerology, ocean engineering and even space flight and aviation.
The wide range of polymer intelligent material is as high-molecular gel, intelligent macromolecule film material, intelligent macromolecule adhesive, intellectual drug delivery systme and the intelligent macromolecule composite as intellectual material.
Thermosensitive macromolecular membranes is when the residing environment temperature of polymeric membrane changes, and sharp response, the i.e. diffusion barrier of hop variation take place thereupon for the shape of film, infiltration rate etc.The water absorption (or solvent regain) that shows film has sudden variation in a certain temperature, the swelling ratio (absorb water or the ratio of the amount of solvent and dry film quality) that is film can change suddenly in a certain temperature, and this temperature is called sensitive temperature or lowest critical solution temperature (LCST).It can be widely used in the fields such as separation purification, artificial organs, medicine control release and bionical science of biochemical substances.The method for preparing Thermosensitive macromolecular membranes has physics and chemical method, physical method such as implantation, complex coacervation, blending method etc., and chemical method has solution polymerization process, radiation polymerization etc.Both at home and abroad particularly in Japan, the research of Thermosensitive macromolecular membranes and application have obtained bigger progress in many aspects in recent years.
Summary of the invention
The purpose of this invention is to provide a kind of temperature-sensitive separating film and preparation method thereof, this film has thermal sensitivity, residing temperature is through certain when a bit, separation performances such as the water flux of film, voidage can be undergone mutation, and have invertibity, thereby can be applicable to biomedicine fields such as big molecular separation, medicine release.
Temperature-sensitive separating film of the present invention is made up of hydroxypropyl cellulose and polyacrylonitrile, and the molecular weight of film is 80 000-100 000, and the thickness of rete is the 50-200 micron.
Described hydroxypropyl cellulose and polyacrylonitrile mass ratio 80-50: 20-50, preferred 50: 50.
The preparation method of temperature-sensitive separating film of the present invention comprises the following steps:
(1) take by weighing hydroxypropyl cellulose and polyacrylonitrile, drying is dissolved in the solvent, the preparation blend solution;
(2) will make the lamina membranacea preheating, with the method knifing of hydrostomia film forming;
(3) scrape the film prevapourising, immerse in the mixed liquor, solidify;
(4) take out film, remove surface solution, oven dry promptly gets temperature-sensitive separating film.
Drying in the described step (1) is 45-60 ℃ of dry 20-30 hour;
Solvent in the described step (1) is dimethyl sulfoxide (DMSO), dimethyl formamide or dimethylacetylamide, preferred dimethyl sulfoxide (DMSO);
Described blend solution is that hydroxypropyl cellulose and polyacrylonitrile are dissolved in respectively in the solvent, reaches identical solid content respectively, again with two solution blendings, stir or these two kinds of powder are mixed by identical quality, be dissolved in the solvent, obtain solution, solid content are 0-17%;
Described system lamina membranacea is glass plate, corrosion resistant plate or polyfluortetraethylene plate;
Described preheating is 25 ℃, 30 ℃ or 35 ℃ of preheatings;
Described knifing speed is the 50-80 cm per minute;
Described prevapourising is prevapourising 5-60 second under the room temperature;
Described immersion mixed liquor is immersion glycerine and water mixed liquor 5-15 minute, and wherein the mass ratio of glycerine and water is 50: 50;
Oven dry in the described step (4) is oven dry 10-16 hour in 45-60 ℃ the vacuum drying oven.
Beneficial effect of the present invention:
(1) its temperature sensitive property of temperature-sensitive separating film of the present invention has invertibity;
(2) the better Thermosensitive macromolecular membranes temperature adjusting of the present invention's preparation changes between 35～40 ℃;
(3) the present invention can prepare the film at different temperatures control point, and by changing the content of hydroxypropyl cellulose in the blend, temperature control point will change, and along with the increase of hydroxy propyl cellulose cellulose content, temperature control point raises.
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
Take by weighing and mix according to hydroxypropyl cellulose/ratio of 80: 20 of polyacrylonitrile mass ratio, be placed on then in the baking oven in 50 ℃ dry 24 hours down, be dissolved in the dimethylsulfoxide solvent.The dissolving fully of hydroxypropyl cellulose and polyacrylonitrile mixture needs the time about a week at least, needs repeatedly reinforced and constantly stirring at a slow speed, and the maximum solid content of gained blended liquid reaches 15%.Polyfluortetraethylene plate is preheated to 30 ℃, with the method for hydrostomia film forming knifing speed knifing with 50 cm per minute.To on polyfluortetraethylene plate, scrape hydroxypropyl cellulose/polyacrylonitrile blended film, prevapourising 15 seconds at room temperature more all immersed film in the mixed liquor of glycerin/water 15 minutes then, wherein the mass ratio of glycerine and water is 50: 50, as coagulating bath.Film is taken out, with absorbent filter Wiping film surface gently, then film is put into 50 ℃ vacuum drying oven oven dry 12 hours, the thicknesses of layers of gained is 50 microns.
Embodiment 2
Take by weighing and mix according to hydroxypropyl cellulose/ratio of 65: 35 of polyacrylonitrile mass ratio, be placed on then in the baking oven in 50 ℃ dry 24 hours down, be dissolved in the solvent dimethylformamide.The dissolving fully of hydroxypropyl cellulose and polyacrylonitrile mixture needs the time about a week at least, needs repeatedly reinforced and constantly stirring at a slow speed, and the maximum solid content of gained blended liquid reaches 15%.Polyfluortetraethylene plate is preheated to 30 ℃, with the method for hydrostomia film forming knifing speed knifing with 50 cm per minute.To on polyfluortetraethylene plate, scrape hydroxypropyl cellulose/polyacrylonitrile blended film, prevapourising 40 seconds at room temperature again, then film was all immersed in the mixed liquor of glycerin/water 10 minutes, wherein the mass ratio of glycerine and water is 50: 50, as coagulating bath film is taken out, with absorbent filter Wiping film surface gently, then film is put into 50 ℃ vacuum drying oven oven dry 12 hours, the thicknesses of layers of gained is 150 microns.
Embodiment 3
Take by weighing and mix according to hydroxypropyl cellulose/ratio of 50: 50 of polyacrylonitrile mass ratio, be placed on then in the baking oven in 50 ℃ dry 24 hours down, be dissolved in the dimethylacetamide solvent.The dissolving fully of hydroxypropyl cellulose and polyacrylonitrile mixture needs the time about a week at least, needs repeatedly reinforced and constantly stirring at a slow speed, and the maximum solid content of gained blended liquid reaches 15%.Polyfluortetraethylene plate is preheated to 35 ℃, with the method for hydrostomia film forming knifing speed knifing with 50 cm per minute.To on polyfluortetraethylene plate, scrape hydroxypropyl cellulose/polyacrylonitrile blended film, prevapourising 60 seconds at room temperature more all immersed film in the mixed liquor of glycerin/water 10 minutes then, wherein the mass ratio of glycerine and water is 50: 50, as coagulating bath.Film is taken out, with absorbent filter Wiping film surface gently, then film is put into 50 ℃ vacuum drying oven oven dry 12 hours, the thicknesses of layers of gained is 100 microns.
Embodiment 4
Take by weighing and mix according to hydroxypropyl cellulose/ratio of 65: 35 of polyacrylonitrile mass ratio, be placed on then in the baking oven in 50 ℃ dry 24 hours down, be dissolved in the dimethylsulfoxide solvent.The dissolving fully of hydroxypropyl cellulose and polyacrylonitrile mixture needs the time about a week at least, needs repeatedly reinforced and constantly stirring at a slow speed, and the maximum solid content of gained blended liquid reaches 17%.Polyfluortetraethylene plate is preheated to 30 ℃, with the method for hydrostomia film forming knifing speed knifing with 80 cm per minute.To on polyfluortetraethylene plate, scrape hydroxypropyl cellulose/polyacrylonitrile blended film, prevapourising 30 seconds at room temperature again, then film was all immersed in the mixed liquor of glycerin/water 15 minutes, wherein the mass ratio of glycerine and water is 50: 50, as coagulating bath film is taken out, with absorbent filter Wiping film surface gently, then film is put into 50 ℃ vacuum drying oven oven dry 12 hours, the thicknesses of layers of gained is 200 microns.
Embodiment 5
Take by weighing and mix according to hydroxypropyl cellulose/ratio of 50: 50 of polyacrylonitrile mass ratio, be placed on then in the baking oven in 50 ℃ dry 24 hours down, be dissolved in the dimethylsulfoxide solvent.The dissolving fully of hydroxypropyl cellulose and polyacrylonitrile mixture needs the time about a week at least, needs repeatedly reinforced and constantly stirring at a slow speed, and the maximum solid content of gained blended liquid reaches 15%.Polyfluortetraethylene plate is preheated to 35 ℃, with the method for hydrostomia film forming knifing speed knifing with 80 cm per minute.To on polyfluortetraethylene plate, scrape hydroxypropyl cellulose/polyacrylonitrile blended film, prevapourising 45 seconds at room temperature more all immersed film in the mixed liquor of glycerin/water 15 minutes then, wherein the mass ratio of glycerine and water is 50: 50, as coagulating bath.Film is taken out, with absorbent filter Wiping film surface gently, then film is put into 50 ℃ vacuum drying oven oven dry 12 hours, the thicknesses of layers of gained is 100 microns.
Claims (13)
1. temperature-sensitive separating film, it is characterized in that: this film is made up of hydroxypropyl cellulose and polyacrylonitrile, and the molecular weight of film is 80 000-100 000, and the thickness of rete is the 50-200 micron.
2. temperature-sensitive separating film according to claim 1 is characterized in that: described hydroxypropyl cellulose and polyacrylonitrile mass ratio 80-50: 20-50.
3. temperature-sensitive separating film according to claim 2 is characterized in that: described hydroxypropyl cellulose and polyacrylonitrile mass ratio 50: 50.
4. the preparation method of temperature-sensitive separating film comprises the following steps:
(1) take by weighing hydroxypropyl cellulose and polyacrylonitrile, drying is dissolved in the solvent, the preparation blend solution;
(2) will make the lamina membranacea preheating, with the method knifing of hydrostomia film forming;
(3) scrape the film prevapourising, immerse in the mixed liquor, solidify;
(4) take out film, remove surface solution, oven dry promptly gets temperature-sensitive separating film;
Described immersion mixed liquor is immersion glycerine and water mixed liquor 5-15 minute, and wherein the mass ratio of glycerine and water is 50: 50.
5. the preparation method of temperature-sensitive separating film according to claim 4 is characterized in that: the baking temperature 45-60 in the described step (1) ℃, and time 20-30 hour.
6. the preparation method of temperature-sensitive separating film according to claim 4, it is characterized in that: the solvent in the described step (1) is dimethyl sulfoxide (DMSO), dimethyl formamide or dimethylacetylamide.
7. the preparation method of temperature-sensitive separating film according to claim 6, it is characterized in that: the solvent in the described step (1) is a dimethyl sulfoxide (DMSO).
8. the preparation method of temperature-sensitive separating film according to claim 7, it is characterized in that: described blend solution is that hydroxypropyl cellulose and polyacrylonitrile are dissolved in the solvent respectively, reach identical solid content respectively, again with two solution blendings, stir or these two kinds of powder are mixed by identical quality, be dissolved in the solvent, obtain solution, solid content are 0-17%.
9. the preparation method of temperature-sensitive separating film according to claim 4, it is characterized in that: described system lamina membranacea is glass plate, corrosion resistant plate or polyfluortetraethylene plate.
10. the preparation method of temperature-sensitive separating film according to claim 4, it is characterized in that: described preheating is 25 ℃, 30 ℃ or 35 ℃ of preheatings.
11. the preparation method of temperature-sensitive separating film according to claim 4 is characterized in that: described knifing speed is the 50-80 cm per minute.
12. the preparation method of temperature-sensitive separating film according to claim 4 is characterized in that: described prevapourising is prevapourising 5-60 second under the room temperature.
13. the preparation method of temperature-sensitive separating film according to claim 4 is characterized in that: the oven dry in the described step (4) is oven dry 10-16 hour in 45-60 ℃ the vacuum drying oven.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100472731A CN100534595C (en) | 2007-10-19 | 2007-10-19 | Temperature-sensitive separating film and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100472731A CN100534595C (en) | 2007-10-19 | 2007-10-19 | Temperature-sensitive separating film and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101224395A CN101224395A (en) | 2008-07-23 |
| CN100534595C true CN100534595C (en) | 2009-09-02 |
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| CNB2007100472731A Expired - Fee Related CN100534595C (en) | 2007-10-19 | 2007-10-19 | Temperature-sensitive separating film and preparation method thereof |
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| CN106711401A (en) * | 2016-12-15 | 2017-05-24 | 安徽大学 | Lithium-ion flexible-cell substrate-free positive plate and preparation method |
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Non-Patent Citations (2)
| Title |
|---|
| 聚丙烯腈与羟乙基纤维素共混膜的研制. 刘永建，王庆瑞，陈雪英，沈新元.中国纺织大学学报，第23卷第3期. 1997 |
| 聚丙烯腈与羟乙基纤维素共混膜的研制. 刘永建，王庆瑞，陈雪英，沈新元.中国纺织大学学报，第23卷第3期. 1997 * |
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| CN101224395A (en) | 2008-07-23 |
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Assignee: Jiangsu Langsheng Life Science and Technology Co., Ltd. Assignor: Donghua University Contract record no.: 2010320000489 Denomination of invention: Temperature-sensitive separating film and preparing method thereof Granted publication date: 20090902 License type: Exclusive License Open date: 20080723 Record date: 20100429 |
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