CN105413490A - Preparation method of PVDF (Polyvinylidene Fluoride) separating membrane - Google Patents
Preparation method of PVDF (Polyvinylidene Fluoride) separating membrane Download PDFInfo
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- CN105413490A CN105413490A CN201510963053.8A CN201510963053A CN105413490A CN 105413490 A CN105413490 A CN 105413490A CN 201510963053 A CN201510963053 A CN 201510963053A CN 105413490 A CN105413490 A CN 105413490A
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- kynoar
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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
-
- 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
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The invention discloses a preparation method of a PVDF (Polyvinylidene Fluoride) separating membrane, polyvinylidene fluoride is adopted as a raw material of a membrane, and the preparation steps of the polyvinylidene fluoride comprise: 1) putting 1 to 2 parts by weight of hydroxy propyl cellulose, 2.4 parts by weight of hydrogen peroxide and 3.7 parts by weight of inorganic base solution into a reaction still, uniformly mixing, then putting 1.8 parts by weight of dodecyltrimethylammonium chloride, 9.7 parts by weight of hexafluoroethane solvent and 1.8 parts by weight of chloroacetyl chloride solution into the reaction still, stirring and reacting at -5.5 DEG C for 39 minutes; 2) putting 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 parts by weight of N-methylpyrrolidone solution, 63 parts by weight of vinylidene fluoride monomer and 2.6 parts by weight of 2,2,3-trimethylpentane into the reaction still, stirring and reacting at 14 DEG C, and performing a termination reaction when the pressure is decreased to 0.23 MPa or less; 3) filtering, washing and drying to obtain powder-like polyvinylidene fluoride. The separating membrane prepared by the invention has the properties of corrosion resistance, heat resistance, cold resistance, oxidation resistance and weather resistance.
Description
Technical field
The present invention relates to the preparation method of PVDF diffusion barrier.
Background technology
Corrosion-resistant, heat-resisting, cold-resistant, resistance to oxidation, the weather resistance of existing milipore filter, diffusion barrier, 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 PVDF diffusion barrier, take Kynoar 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 PVDF diffusion barrier, and take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 ~ 2 weight portion hydroxypropyl cellulose, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;
2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Preferably, the preparation method of PVDF diffusion barrier, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 weight portion hydroxypropyl cellulose, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;
2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Preferably, the preparation method of PVDF diffusion barrier, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 2 weight portion hydroxypropyl celluloses, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;
2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Advantage of the present invention and beneficial effect are: the preparation method providing a kind of PVDF diffusion barrier, take Kynoar as the raw material of film, and the film of preparation has excellent corrosion-resistant, heat-resisting, cold-resistant, resistance to oxidation, weather resistance.
Detailed description of the invention
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 PVDF diffusion barrier, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 ~ 2 weight portion hydroxypropyl cellulose, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;
2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Embodiment 2
The preparation method of PVDF diffusion barrier, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 weight portion hydroxypropyl cellulose, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;
2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Embodiment 3
The preparation method of PVDF diffusion barrier, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 2 weight portion hydroxypropyl celluloses, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;
2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
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)
- The preparation method of 1.PVDF diffusion barrier, is characterized in that, take Kynoar as the raw material of film, described Kynoar is prepared as follows:1) 1 ~ 2 weight portion hydroxypropyl cellulose, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;3) filtration, washing, drying, obtain Powdered Kynoar.
- 2. the preparation method of PVDF diffusion barrier according to claim 1, is characterized in that, take Kynoar as the raw material of film, described Kynoar is prepared as follows:1) 1 weight portion hydroxypropyl cellulose, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;3) filtration, washing, drying, obtain Powdered Kynoar.
- 3. the preparation method of PVDF diffusion barrier according to claim 1, is characterized in that, take Kynoar as the raw material of film, described Kynoar is prepared as follows:1) 2 weight portion hydroxypropyl celluloses, 2.4 weight portion hydrogen peroxide, 3.7 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion Trimethyllaurylammonium chlorides, 9.7 weight portion perfluoroethane solvents, 1.8 weight portion chloracetyl chloride solution again ,-5.5 DEG C of stirring reactions 39 minutes;2) 3.7 parts by weight of fatty acid methyl ester sulfonate, 5.7 weight portion 1-METHYLPYRROLIDONE solution, 63 weight portion vinylidene fluoride monomers, 2.6 weight portions 2 are dropped into again, 2,3-trimethylpentane, at 14 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.23MPa;3) filtration, washing, drying, obtain Powdered Kynoar.
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| CN201510963053.8A CN105413490A (en) | 2015-12-18 | 2015-12-18 | Preparation method of PVDF (Polyvinylidene Fluoride) separating membrane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107626214A (en) * | 2017-08-25 | 2018-01-26 | 南通成山高分子材料有限公司 | A kind of preparation method of polymeric membrane for separation |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104403033A (en) * | 2014-12-06 | 2015-03-11 | 常熟丽源膜科技有限公司 | Preparation method of polyvinylidene fluoride |
| 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 |
| CN104448149A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Preparation process of polyvinylidene fluoride with thermal stability |
| CN104448075A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Preparation method of polyvinylidene fluoride with thermal stability |
| CN104448077A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Production process of polyvinylidene fluoride |
| 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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- 2015-12-18 CN CN201510963053.8A patent/CN105413490A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104403033A (en) * | 2014-12-06 | 2015-03-11 | 常熟丽源膜科技有限公司 | Preparation method of polyvinylidene fluoride |
| 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 |
| CN104448149A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Preparation process of polyvinylidene fluoride with thermal stability |
| CN104448075A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Preparation method of polyvinylidene fluoride with thermal stability |
| CN104448077A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Production process of polyvinylidene fluoride |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107626214A (en) * | 2017-08-25 | 2018-01-26 | 南通成山高分子材料有限公司 | A kind of preparation method of polymeric membrane for separation |
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