CN105461837A - Preparation method of polyvinylidene fluoride ultrafiltration membrane - Google Patents
Preparation method of polyvinylidene fluoride ultrafiltration membrane Download PDFInfo
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- CN105461837A CN105461837A CN201510963185.0A CN201510963185A CN105461837A CN 105461837 A CN105461837 A CN 105461837A CN 201510963185 A CN201510963185 A CN 201510963185A CN 105461837 A CN105461837 A CN 105461837A
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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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- Chemical Kinetics & Catalysis (AREA)
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- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a preparation method of a polyvinylidene fluoride ultrafiltration membrane. Polyvinylidene fluoride is taken as a raw material of the membrane and is prepared by the following steps: (1) putting 1 to 2 parts by weight of sodium tripolyphosphate, 2.3 parts by weight of hydrogen peroxide, 1.4 parts by weight of inorganic aqueous alkali into a reaction still, uniformly mixing, then putting 1.4 parts by weight of benzoyl peroxide, 11.3 parts by weight of 1,1,2-trichlorotrifluoroethane solvent, and 0.2 part by weight of perfluoro butanesulfonylfluoride solution in, and stirring at the temperature of 8 DEG C below zero for reacting for 30 minutes; (2) then putting 0.9 part by weight of lauroyl aminoethyl sodium sulfate, 5.7 parts by weight of polypropylene glycol solution, 62 parts by weight of polyvinyl fluoride monomer and 2.5 parts by weight of dibromo-cyclopentane in, stirring at the temperature of 25 DEG C for the reaction, and finishing the reaction when the pressure is reduced to be below 0.21MPa; (3) filtering, washing and drying to obtain the powdery polyvinylidene fluoride. The membrane prepared by the preparation method has corrosion resistance, heat resistance, cold resistance, oxidation resistance and weather resistance.
Description
Technical field
The present invention relates to the preparation method of polyvinylidene fluoride (PVDF) ultrafiltration 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 fluoride (PVDF) ultrafiltration 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 fluoride (PVDF) ultrafiltration 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 tripoly phosphate sodium STPP, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Preferably, the preparation method of polyvinylidene fluoride (PVDF) ultrafiltration membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 weight part tripoly phosphate sodium STPP, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Preferably, the preparation method of polyvinylidene fluoride (PVDF) ultrafiltration membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 2 weight part tripoly phosphate sodium STPPs, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
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 fluoride (PVDF) ultrafiltration 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 fluoride (PVDF) ultrafiltration membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 ~ 2 weight part tripoly phosphate sodium STPP, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Embodiment 2
The preparation method of polyvinylidene fluoride (PVDF) ultrafiltration membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 1 weight part tripoly phosphate sodium STPP, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Embodiment 3
The preparation method of polyvinylidene fluoride (PVDF) ultrafiltration membrane, take polyvinylidene difluoride (PVDF) as the raw material of film, described polyvinylidene difluoride (PVDF) is prepared as follows:
1) 2 weight part tripoly phosphate sodium STPPs, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
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 fluoride (PVDF) ultrafiltration 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 tripoly phosphate sodium STPP, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
2. the preparation method of polyvinylidene fluoride (PVDF) ultrafiltration 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 tripoly phosphate sodium STPP, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
3. the preparation method of polyvinylidene fluoride (PVDF) ultrafiltration 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 tripoly phosphate sodium STPPs, 2.3 weight part hydrogen peroxide, 1.4 parts by weight of inorganic alkaline solutions are dropped in reactor, mix, drop into 1.4 weight part benzoyl peroxides, 11.3 weight parts 1 again, 2,2-tri-fluoro-1,1,2-Separator, 0.2 weight part perfluoro butyl sulfonic acid fluoride solution ,-8 DEG C of stirring reactions 30 minutes;
2) drop into 0.9 weight part lauramide sodium ethyl sulfate, 5.7 weight part polypropylene glycol solution, 62 weight part vinylidene fluoride monomers, 2.5 weight part dibromo pentamethylene again, at 25 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.21MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
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Cited By (2)
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CN107304280A (en) * | 2016-04-18 | 2017-10-31 | 深圳市万福格聚合物科技有限公司 | A kind of preparation method of polyvinylidene fluoride material |
CN115028945A (en) * | 2022-07-26 | 2022-09-09 | 碧菲分离膜(大连)有限公司 | Synthetic method of polyvinylidene fluoride |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107304280A (en) * | 2016-04-18 | 2017-10-31 | 深圳市万福格聚合物科技有限公司 | A kind of preparation method of polyvinylidene fluoride material |
CN115028945A (en) * | 2022-07-26 | 2022-09-09 | 碧菲分离膜(大连)有限公司 | Synthetic method of polyvinylidene fluoride |
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