CN104448076A - Production method of polyvinylidene fluoride - Google Patents
Production method of polyvinylidene fluoride Download PDFInfo
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- CN104448076A CN104448076A CN201410731753.XA CN201410731753A CN104448076A CN 104448076 A CN104448076 A CN 104448076A CN 201410731753 A CN201410731753 A CN 201410731753A CN 104448076 A CN104448076 A CN 104448076A
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Abstract
The invention discloses a production method of polyvinylidene fluoride. The production method comprises the following steps of (1) adding 0.9 part by weight of hydrogen peroxide and 1.2 parts by weight of an inorganic alkali solution into a reaction kettle, uniformly mixing, then, adding 14.5 parts by weight of a trifluorotrichloroethane solvent and 1.8 parts by weight of a phenylmethylsulfonyl fluoride solution, and reacting at the temperature of 5 DEG C below zero for 25 minutes by stirring; (2) introducing 3.2 parts by weight of a 2-hexyl-1-decanol solution, 69 parts by weight of vinylidene fluoride monomers and 1.8 parts by weight of n-butyl cyclopentane, reacting at the temperature of 28 DEG C by stirring, and stopping reacting when the pressure is reduced to be smaller than 0.23MPa; and (3) filtering, washing and drying to obtain powdery polyvinylidene fluoride. Polyvinylidene fluoride prepared by using the production method is favorable in thermal stability and processibility and capable of meeting the requirements of production processes such as injection molding, extruding and film drawing.
Description
Technical field
The present invention relates to the production method of polyvinylidene difluoride (PVDF).
Background technology
Existing vinylidene material, its thermostability and workability have much room for improvement, and are not particularly well positioned to meet injection moulding, extrude and the production technique such as membrane.
Summary of the invention
The object of the present invention is to provide a kind of production method of polyvinylidene difluoride (PVDF), its vinylidene prepared has good thermostability and workability, can meet injection moulding, extrude and the production technique such as membrane.
For achieving the above object, technical scheme of the present invention designs a kind of production method of polyvinylidene difluoride (PVDF), comprises the steps:
1) drop into 0.9 weight part hydrogen peroxide, 1.2 parts by weight of inorganic alkaline solutions in reactor, mix, then drop into 14.5 weight part Freon 113 solvents, 1.8 weight part phenylmethylsulfonyl fluoride solution ,-5 DEG C of stirring reactions 25 minutes;
2) pass into 3.2 weight part hexyl decyl alcohol solution, 69 weight part vinylidene fluoride monomers, 1.8 weight part normal-butyl pentamethylene again, at 28 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 production method providing a kind of polyvinylidene difluoride (PVDF), and its vinylidene prepared has good thermostability and workability, can meet injection moulding, extrude and the production technique such as membrane.
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:
A production method for polyvinylidene difluoride (PVDF), comprises the steps:
1) drop into 0.9 weight part hydrogen peroxide, 1.2 parts by weight of inorganic alkaline solutions in reactor, mix, then drop into 14.5 weight part Freon 113 solvents, 1.8 weight part phenylmethylsulfonyl fluoride solution ,-5 DEG C of stirring reactions 25 minutes;
2) pass into 3.2 weight part hexyl decyl alcohol solution, 69 weight part vinylidene fluoride monomers, 1.8 weight part normal-butyl pentamethylene again, at 28 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 (1)
1. the production method of polyvinylidene difluoride (PVDF), is characterized in that, comprises the steps:
1) drop into 0.9 weight part hydrogen peroxide, 1.2 parts by weight of inorganic alkaline solutions in reactor, mix, then drop into 14.5 weight part Freon 113 solvents, 1.8 weight part phenylmethylsulfonyl fluoride solution ,-5 DEG C of stirring reactions 25 minutes;
2) pass into 3.2 weight part hexyl decyl alcohol solution, 69 weight part vinylidene fluoride monomers, 1.8 weight part normal-butyl pentamethylene again, at 28 DEG C of stirring reactions, pressure drop is to termination reaction during below 0.23MPa;
3) filtration, washing, drying, obtain Powdered polyvinylidene difluoride (PVDF).
Priority Applications (1)
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CN201410731753.XA CN104448076A (en) | 2014-12-06 | 2014-12-06 | Production method of polyvinylidene fluoride |
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CN201410731753.XA CN104448076A (en) | 2014-12-06 | 2014-12-06 | Production method of polyvinylidene fluoride |
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CN201410731753.XA Pending CN104448076A (en) | 2014-12-06 | 2014-12-06 | Production method of polyvinylidene fluoride |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105435650A (en) * | 2015-12-18 | 2016-03-30 | 常熟三爱富振氟新材料有限公司 | Preparation method of polyvinylidene fluoride separation membrane |
CN105461837A (en) * | 2015-12-18 | 2016-04-06 | 常熟三爱富振氟新材料有限公司 | Preparation method of polyvinylidene fluoride ultrafiltration membrane |
CN105536570A (en) * | 2015-12-18 | 2016-05-04 | 常熟三爱富振氟新材料有限公司 | Preparation method of hollow fiber ultrafiltration membrane |
CN105597563A (en) * | 2015-12-18 | 2016-05-25 | 常熟三爱富振氟新材料有限公司 | Preparation method of vinyl polyvinylidene fluoride hollow fiber membrane |
CN105617886A (en) * | 2015-12-18 | 2016-06-01 | 常熟三爱富振氟新材料有限公司 | Preparation method of hydrophilic hollow fiber ultra-filtration membrane |
Citations (7)
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GB1385229A (en) * | 1971-03-18 | 1975-02-26 | Diamond Shamrock Corp | Polyvinylidenefluorides |
US4076929A (en) * | 1975-10-30 | 1978-02-28 | Pennwalt Corporation | Vinylidene fluoride polymer having improved melt flow properties |
US6329471B1 (en) * | 1998-03-19 | 2001-12-11 | Nippon Mektron Limited | Process for producing carboxyl group-containing vinylidene fluoride copolymer |
EP1607417A1 (en) * | 2003-03-26 | 2005-12-21 | Daikin Industries, Ltd. | Method of forming thin film |
CN1718602A (en) * | 2005-07-20 | 2006-01-11 | 上海三爱富新材料股份有限公司 | Synthesis method of poly vinylidene difluoride and polyvinylidene difluoride obtained thereby |
CN103601827A (en) * | 2013-12-02 | 2014-02-26 | 内蒙古三爱富万豪氟化工有限公司 | Vinylidene fluoride polymer and preparation method thereof |
CN104151457A (en) * | 2014-08-11 | 2014-11-19 | 东莞市长安东阳光铝业研发有限公司 | Polyvinylidene fluoride preparation method |
-
2014
- 2014-12-06 CN CN201410731753.XA patent/CN104448076A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1385229A (en) * | 1971-03-18 | 1975-02-26 | Diamond Shamrock Corp | Polyvinylidenefluorides |
US4076929A (en) * | 1975-10-30 | 1978-02-28 | Pennwalt Corporation | Vinylidene fluoride polymer having improved melt flow properties |
US6329471B1 (en) * | 1998-03-19 | 2001-12-11 | Nippon Mektron Limited | Process for producing carboxyl group-containing vinylidene fluoride copolymer |
EP1607417A1 (en) * | 2003-03-26 | 2005-12-21 | Daikin Industries, Ltd. | Method of forming thin film |
CN1718602A (en) * | 2005-07-20 | 2006-01-11 | 上海三爱富新材料股份有限公司 | Synthesis method of poly vinylidene difluoride and polyvinylidene difluoride obtained thereby |
CN103601827A (en) * | 2013-12-02 | 2014-02-26 | 内蒙古三爱富万豪氟化工有限公司 | Vinylidene fluoride polymer and preparation method thereof |
CN104151457A (en) * | 2014-08-11 | 2014-11-19 | 东莞市长安东阳光铝业研发有限公司 | Polyvinylidene fluoride preparation method |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105435650A (en) * | 2015-12-18 | 2016-03-30 | 常熟三爱富振氟新材料有限公司 | Preparation method of polyvinylidene fluoride separation membrane |
CN105461837A (en) * | 2015-12-18 | 2016-04-06 | 常熟三爱富振氟新材料有限公司 | Preparation method of polyvinylidene fluoride ultrafiltration membrane |
CN105536570A (en) * | 2015-12-18 | 2016-05-04 | 常熟三爱富振氟新材料有限公司 | Preparation method of hollow fiber ultrafiltration membrane |
CN105597563A (en) * | 2015-12-18 | 2016-05-25 | 常熟三爱富振氟新材料有限公司 | Preparation method of vinyl polyvinylidene fluoride hollow fiber membrane |
CN105617886A (en) * | 2015-12-18 | 2016-06-01 | 常熟三爱富振氟新材料有限公司 | Preparation method of hydrophilic hollow fiber ultra-filtration membrane |
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