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Polyvinylidene fluoride resin with fluorine ether end group structure and preparation method thereof

A technology of polyvinylidene fluoride and vinylidene fluoride, which is applied in the field of manufacturing polyvinylidene fluoride resin, and can solve problems such as wide product molecular weight distribution, general end group stability, and insufficient stability

Active Publication Date: 2011-10-26
INNER MONGOLIA WANHAO FLUOROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecular weight distribution of the product obtained by this patent method is relatively wide, and the use of inorganic initiators and chain transfer agents based on hydrocarbons also faces the general problem of end group stability.
[0005] U.S. Patent No. 4,360,652 discloses the use of isopropanol as a chain transfer agent to improve the thermal stability of vinylidene fluoride copolymerization products and homopolymerization products, but compared with fluorine-containing end groups, the bond energy of the C-F bond is greater than that of the C-H bond , so its stability is still insufficient

Method used

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  • Polyvinylidene fluoride resin with fluorine ether end group structure and preparation method thereof
  • Polyvinylidene fluoride resin with fluorine ether end group structure and preparation method thereof
  • Polyvinylidene fluoride resin with fluorine ether end group structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Firstly, vinylidene fluoride and perfluoro-n-propyl vinyl ether are formulated into a mixed monomer according to the ratio of perfluoro-n-propyl vinyl ether content to 5 mol%, and placed in a monomer tank for later use, and the temperature of the mixed monomer is controlled at 45°C.

[0080] In the 1.2L reactor, first pass cold brine at -15°C in the jacket to control the temperature of the reactor at -5°C, then add 720g of 2,3-dihydrodecafluoropentane (HFC4310mee), and close the kettle Then start stirring, the stirring speed is 700rpm, replace the air with nitrogen, after the oxygen content is less than 50ppm, put hot water in the jacket, and control the reaction temperature at 35°C, then add the prepared mixed monomer to a pressure of 0.5 MPa, add 73.1g comonomer (60g vinylidene fluoride and 13.1g perfluoro n-propyl vinyl ether monomer) altogether, add 1.5g (CF 3 CF(OCF 2 CF 2 CF 3 )COO) 2 Initiator, after the pressure drop occurs, start to add monomer to maintain ...

Embodiment 2

[0083] Firstly, vinylidene fluoride and perfluoro-n-propyl vinyl ether are formulated into a mixed monomer according to the ratio of perfluoro-n-propyl vinyl ether content to 8 mol%, and placed in a monomer tank for later use. The temperature of the mixed monomer is controlled at 45°C.

[0084] In the 25L reactor, first pass cold brine at -15°C in the jacket to control the temperature of the reactor at -5°C, and then add 12.5kg of 1,1,1,3,3-pentafluorobutane (HFC365mfc ), start stirring after closing the kettle, the stirring speed is 800rpm, and replace the air with nitrogen. body to a pressure of 0.75MPa, a total of 1.702kg comonomers (1.25kg vinylidene fluoride and 0.452kg perfluoro-n-propyl vinyl ether monomer) were added, and 22.7g (CF 3 CF(OCF 2 CF 2 CF 3 )COO) 2 Initiator, after the pressure drop occurs, start to add monomers to maintain the reaction pressure at 0.75MPa. After the amount of added monomers reaches 375g, stop feeding, lower the system temperature to 10°C...

Embodiment 3

[0087] With embodiment 1, just add trifluorotrichloroethane (CFC113) as solvent, with [CF 3 CF(OCF 3 )COO] 2 As an initiator, perfluoromethyl vinyl ether is used as a comonomer.

[0088] First, vinylidene fluoride and perfluoromethyl vinyl ether are formulated into a mixed monomer according to the ratio of perfluoromethyl vinyl ether content of 12.4 mol%, and placed in a monomer tank for standby, and the temperature of the mixed monomer is controlled at 45°C.

[0089] In the 1.2L reactor, first pass cold brine at -15°C in the jacket to control the temperature of the reactor at -5°C, then add 636g of trifluorotrichloroethane, start stirring after closing the kettle, and the stirring speed is 650rpm, replace the air with nitrogen, after the oxygen content is less than 50ppm, pass hot water into the jacket, and control the reaction temperature at 30°C, then add the prepared mixed monomer to a pressure of 0.5MPa, and add a total of 154.5g copolymerization monomer (including 113...

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Abstract

A polyvinylidene fluoride resin with a fluorine ether end group structure is disclosed, which comprises: (a) 0.5-10 mol% of at least one polymer unit derived from the comonomer in the following formula (I) (wherein n=0-2); (b) the balance of polymer units derived from vinylidene fluoride monomer. The polyvinylidene fluoride copolymer has a molecular weight of 42,000-250,000, and is prepared by using the polymerization initiator in the following formula (II) (wherein n=0-2, z=0-3): CF2=CF-O-(CF2)nCF3 (I); and (CF3(CF2)nCF(O(CF2)zCF3)COO)2 (II).

Description

technical field [0001] The invention relates to a polyvinylidene fluoride resin. The polyvinylidene fluoride resin has a fluorine-containing ether end group structure and has the characteristics of high flexibility, high impact strength and high thermal stability. The present invention also relates to a method for producing the polyvinylidene fluoride resin. Background technique [0002] Among all fluororesins, the homopolymer of vinylidene fluoride (VDF) is a kind of fluororesin with high hardness, but its bending performance is not good. In order to improve this performance, it is generally possible to reduce its crystallinity by adding comonomers, thereby improving the bending performance. Common comonomers include, for example, hexafluoropropylene (HFP), chlorotrifluoroethylene (CTFE), trifluoroethylene (TRFe) or a mixture of two or more thereof. Generally, the longer the branch chain is, the more favorable it is to reduce the crystallinity, that is, to improve the ben...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F216/14C08F4/36C08F2/06
Inventor 吴君毅张冰冰俞子豪盛虹钱辉陆秋生徐刚
Owner INNER MONGOLIA WANHAO FLUOROCHEM