CN105413491A - Preparing method of hydrophobic PVDF ultrafiltration membrane - Google Patents
Preparing method of hydrophobic PVDF ultrafiltration membrane Download PDFInfo
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- CN105413491A CN105413491A CN201510963055.7A CN201510963055A CN105413491A CN 105413491 A CN105413491 A CN 105413491A CN 201510963055 A CN201510963055 A CN 201510963055A CN 105413491 A CN105413491 A CN 105413491A
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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
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a preparing method of a hydrophobic PVDF ultrafiltration membrane. polyvinylidene fluoride is taken as the raw material of the membrane and is prepared by following steps: (1) according to parts by weight, adding 1-2 parts of polyvinylpyrrolidone and 1.9 parts of hydrogen peroxide, 2.3 parts of inorganic alkali solution into a reaction kettle, mixing uniformly, then adding 1.8 parts of dimethyl distearyl ammonium chloride, 17.4 parts of dichlorofluoroethane solvent and 1.7 parts of isobutyryl chloride solution, and stirring for reacting at -6.5 DEG C for 38min; (2) then, according to parts by weight, adding 2.2 parts of fatty alcohol ether sodium sulfate, 4.2 parts of sodium polyacrylate solution and 73 parts of vinylidene fluoride monomer, 4.3 parts of 1,2,3-trimethylcyclopentane, stirring for reacting at 11 DEG C, and terminating the reacting when pressure drops to be below 0.18MPa; (3) filtering, washing and drying to obtain powdery polyvinylidene fluoride. The hydrophobic PVDF ultrafiltration membrane has anticorrosive, heat resistant, cold resistant, antioxidant and weather resistant performances.
Description
Technical field
The present invention relates to the preparation method of hydrophilic PVDF ultrafiltration membrane.
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 hydrophilic PVDF ultrafiltration membrane, 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 hydrophilic PVDF ultrafiltration membrane, and take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 ~ 2 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Preferably, the preparation method of hydrophilic PVDF ultrafiltration membrane, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Preferably, the preparation method of hydrophilic PVDF ultrafiltration membrane, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 2 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Advantage of the present invention and beneficial effect are: the preparation method providing a kind of hydrophilic PVDF ultrafiltration membrane, 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 hydrophilic PVDF ultrafiltration membrane, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 ~ 2 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Embodiment 2
The preparation method of hydrophilic PVDF ultrafiltration membrane, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Embodiment 3
The preparation method of hydrophilic PVDF ultrafiltration membrane, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 2 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
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)
1. the preparation method of hydrophilic PVDF ultrafiltration membrane, is characterized in that, take Kynoar as the raw material of film, described Kynoar is prepared as follows:
1) 1 ~ 2 weight account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
2. the preparation method of hydrophilic PVDF ultrafiltration membrane 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 account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
3. the preparation method of hydrophilic PVDF ultrafiltration membrane 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 account polyethylene pyrrolidones, 1.9 weight portion hydrogen peroxide, 2.3 parts by weight of inorganic aqueous slkalis are dropped in reactor, mix, drop into 1.8 weight portion chloro distearyl dimethyl ammoniums, 17.4 weight portion chloro fluoroethane solvents, 1.7 weight portion isobutyryl chloride solution again ,-6.5 DEG C of stirring reactions 38 minutes;
2) 2.2 parts by weight of fatty ether sulfate, 4.2 parts by weight of polypropylene acid sodium solutions, 73 weight portion vinylidene fluoride monomers, 4.3 weight portions 1 are dropped into again, 2,3-trimethyl cyclopentane, at 11 DEG C of stirring reactions, pressure drop is to cessation reaction during below 0.18MPa;
3) filtration, washing, drying, obtain Powdered Kynoar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510963055.7A CN105413491A (en) | 2015-12-18 | 2015-12-18 | Preparing method of hydrophobic PVDF ultrafiltration membrane |
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| CN201510963055.7A CN105413491A (en) | 2015-12-18 | 2015-12-18 | Preparing method of hydrophobic PVDF ultrafiltration membrane |
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| CN105413491A true CN105413491A (en) | 2016-03-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644077A (en) * | 2020-06-15 | 2020-09-11 | 齐松松 | Hydrophilic polyvinylidene fluoride nanofiltration membrane and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104448094A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Production 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 |
| CN104497180A (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 CN201510963055.7A patent/CN105413491A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104448094A (en) * | 2014-12-06 | 2015-03-25 | 常熟丽源膜科技有限公司 | Production 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 |
| CN104497180A (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 |
|---|---|---|---|---|
| CN111644077A (en) * | 2020-06-15 | 2020-09-11 | 齐松松 | Hydrophilic polyvinylidene fluoride nanofiltration membrane and preparation method thereof |
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