CN105482012A - Preparation method of polyvinylidene fluoride porous hollow fiber membrane - Google Patents
Preparation method of polyvinylidene fluoride porous hollow fiber membrane Download PDFInfo
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- CN105482012A CN105482012A CN201510963103.2A CN201510963103A CN105482012A CN 105482012 A CN105482012 A CN 105482012A CN 201510963103 A CN201510963103 A CN 201510963103A CN 105482012 A CN105482012 A CN 105482012A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/18—Monomers containing fluorine
- C08F114/22—Vinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a polyvinylidene fluoride porous hollow fiber membrane. Polyvinylidene fluoride is taken as a raw material of the membrane and prepared through the following steps that 1, 1-2 parts by weight of polypropylene glycol, 0.8 part by weight of hydrogen peroxide and 1.6 parts by weight of an inorganic alkali solution are put into a reaction kettle and mixed evenly, 2.2 parts by weight of maleic anhydride, 18.5 parts by weight of dichlorofluoroethane solvent and 0.8 part by weight of a benzoyl chloride solution are put into the reaction kettle, reacting under stirring is performed for 45 minutes at minus 6 DEG C; 2, 1.4 parts by weight of polyalkoxy carboxylate, 6.2 parts by weight of a sodium tripolyphosphate solution, 69 parts by weight of vinylidene fluoride monomers, 1.9 parts by weight of n-butyl cyclopentane are put into the reaction kettle, reacting under stirring is performed at 16 DEG C, and reacting is stopped when the pressure is lowered to 0.23 MPa or below; 3, filtering, washing and drying are performed, and the powder-like polyvinylidene fluoride is obtained. The prepared membrane has the corrosion resistance, heat resistance, cold resistance, oxidation resistance and weather resistance.
Description
Technical field
The present invention relates to the preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane.
Background technology
Corrosion-resistant, heat-resisting, cold-resistant, resistance to oxidation, the weather resistance of existing ultra-filtration membrane, separatory membrane, hollow-fibre membrane all have much room for improvement.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, and the film of preparation has excellent corrosion-resistant, heat-resisting, cold-resistant, resistance to oxidation, weather resistance.
For achieving the above object, technical scheme of the present invention designs a kind of preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, and take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 ~ 2 weight part polypropylene glycol, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Preferably, the preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 weight part polypropylene glycol, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Preferably, the preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 2 weight part polypropylene glycols, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Advantage of the present invention and beneficial effect are: the preparation method providing a kind of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, and the film of preparation has excellent corrosion-resistant, heat-resisting, cold-resistant, resistance to oxidation, weather resistance.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The technical scheme that the present invention specifically implements is:
Embodiment 1
A preparation method for polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 ~ 2 weight part polypropylene glycol, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Embodiment 2
The preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 weight part polypropylene glycol, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Embodiment 3
The preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 2 weight part polypropylene glycols, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. the preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane, is characterized in that, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 ~ 2 weight part polypropylene glycol, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
2. the preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane according to claim 1, is characterized in that, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 weight part polypropylene glycol, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
3. the preparation method of polyvinylidene difluoride (PVDF) porous hollow fiber membrane according to claim 1, is characterized in that, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 2 weight part polypropylene glycols, 0.8 weight part hydrogen peroxide, 1.6 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 2.2 parts by weight maleic anhydride, 18.5 weight part one fluorine dichloroethane solvent, 0.8 weight part Benzoyl chloride solution again ,-6 DEG C of stirring reactions 45 minutes;
2) drop into 1.4 weight parts again and gather alkoxycarboxylates, 6.2 weight part sodium tripolyphosphate solutions, 69 weight part vinylidene fluoride monomers, 1.9 weight part normal-butyl pentamethylene, at 16 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
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| CN201510963103.2A CN105482012A (en) | 2015-12-18 | 2015-12-18 | Preparation method of polyvinylidene fluoride porous hollow fiber membrane |
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| CN201510963103.2A CN105482012A (en) | 2015-12-18 | 2015-12-18 | Preparation method of polyvinylidene fluoride porous hollow fiber membrane |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657447A (en) * | 2013-12-17 | 2014-03-26 | 常熟丽源膜科技有限公司 | Polyvinylidene fluoride porous hollow-fiber membrane |
| CN104403034A (en) * | 2014-12-06 | 2015-03-11 | 常熟丽源膜科技有限公司 | Preparation method of polyvinylidene fluoride with heat stability |
| CN104497179A (en) * | 2014-12-06 | 2015-04-08 | 常熟丽源膜科技有限公司 | Production method of polyvinylidene fluoride with thermal stability |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657447A (en) * | 2013-12-17 | 2014-03-26 | 常熟丽源膜科技有限公司 | Polyvinylidene fluoride porous hollow-fiber membrane |
| CN104403034A (en) * | 2014-12-06 | 2015-03-11 | 常熟丽源膜科技有限公司 | Preparation method of polyvinylidene fluoride with heat stability |
| CN104497179A (en) * | 2014-12-06 | 2015-04-08 | 常熟丽源膜科技有限公司 | Production method of polyvinylidene fluoride with thermal stability |
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Application publication date: 20160413 |