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Preparation method of polytrifluorostyrene

A technology of polytrifluorostyrene and trifluorostyrene, applied in the field of preparation of polytrifluorostyrene, can solve the problem of inability to use trifluorostyrene emulsion polymerization, low surface tension, and inability to obtain yield polytrifluorostyrene And other issues

Active Publication Date: 2021-10-26
CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is reported in the literature (Chem.Abs., 1965, 63 16475) that common fluorine-containing surfactants that can be used for emulsion polymerization of fluorine-containing monomers (such as tetrafluoroethylene, vinylidene fluoride, chlorotrifluoroethylene, etc.), such as PFOA (perfluorooctanoic acid) and other perfluorinated emulsifiers cannot obtain polytrifluorostyrene with higher yield and higher molecular weight
[0006] Although the existing emulsion polymerization technology can prepare polytrifluorostyrene with a certain yield, due to the special monomer structure of trifluorostyrene, secondary Polymerization reaction, when using hydrocarbon surfactants for emulsion polymerization, due to its high surface tension (30-40mN / M), the amount of hydrocarbon emulsifier added is very large, which is the amount of trifluorostyrene monomer 10% to 20% of the total, the post-treatment is not easy to wash, and a large number of emulsifiers have serious foaming; and the common perfluorosurfactant used for emulsion polymerization of fluorine-containing monomers has low surface tension (18-20mN / M), although the amount used is extremely small, generally less than 1% of the monomer amount, it cannot be used for the emulsion polymerization of trifluorostyrene

Method used

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  • Preparation method of polytrifluorostyrene

Examples

Experimental program
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preparation example Construction

[0026] 1. The preparation method of the microemulsion polymerization of polytrifluorostyrene with high glass transition temperature and high molecular weight of the present invention comprises the step of providing the pre-emulsion of trifluorostyrene monomer and non-perfluorinated fluorinated anionic surfactant .

[0027] The anionic surfactant suitable for the method of the present invention contains hydrocarbon structures such as methylene and benzene rings in the main chain, straight chain or branched fluorine-containing structures such as fluorocarbon chains and fluorocarbon ether chains, carboxylate, sulfonic acid Anionic surfactants such as salts, which have the general formula:

[0028] CF 3 (CFX)n-(CH 2 )m-(C 6 h 4 )o-M

[0029] Wherein, n is an integer of 1-7, preferably an integer of 1-6, more preferably an integer of 1-5, preferably an integer of 1-4, preferably an integer of 1-3;

[0030] m is an integer of 1-4, preferably an integer of 1-3, more preferably ...

Embodiment

[0065] testing method

[0066] (1) Determination of solid content of polytrifluorostyrene microemulsion

[0067] Weigh about 5 g of polytrifluorostyrene microemulsion after polymerization, heat at 140° C. for 2 hours, weigh to calculate the solid content, and take the average value of three experiments.

[0068] (2) Determination of the molecular weight of polytrifluorostyrene

[0069] About 5mg of the polymer was weighed and dissolved in 2mL of HPLC-grade DMF, and its molecular weight was characterized by gel permeation chromatography. The specific test conditions are as follows: DMF containing 0.02mol / L LiBr, flow rate: 1mL / min, column temperature: 70°C, sample concentration: 2.5mg / mL.

[0070] (3) Determination of the glass transition temperature of polytrifluorostyrene

[0071] About 10 mg of polymer was weighed and placed in a solid dry pot, and its glass transition temperature was characterized by differential scanning calorimetry. The specific test conditions are ...

Embodiment 1

[0089] In this example, with CF 3 (CF 2 ) 5 CH 2 CH 2 SO 3 Na is an emulsifier for trifluorostyrene microemulsion polymerization.

[0090] Weigh 1.2g CF 3 (CF 2 ) 5 CH 2 CH 2 SO 3 Add Na into a 500mL reaction vessel, add 182g of deionized water, and stir to dissolve. After it is completely dissolved, add 140g of trifluorostyrene monomer and continue to stir for 45min to form a pre-emulsion. The temperature of the pre-emulsion was raised to 55° C., 0.54 g of potassium persulfate and 0.28 g of sodium bisulfite were added, and the stirring was continued at a constant temperature for 18 hours. After the polymerization is completed, the temperature is lowered, and after coagulation and demulsification, the white powdery polytrifluorostyrene resin is obtained after washing and drying.

[0091] Test the performance parameters of the polytrifluorostyrene microemulsion with the above method, the results are shown in the table below.

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Abstract

The invention discloses a preparation method of polytrifluorostyrene. The preparation method comprises the following steps: (i) providing a pre-emulsion of a trifluorostyrene monomer and a non-perfluorinated fluorine-containing anionic surfactant, wherein based on the weight of the trifluorostyrene monomer, the amount of the non-perfluorinated fluorine-containing anionic surfactant in the emulsion is 0.1-5 wt%, and the general formula of the non-perfluorinated fluorine-containing anionic surfactant is CF3(CFX)n-(CH2)m-(C6H4)o-M, wherein in the general formula, n is an integer from 1 to 7, m is an integer from 1 to 4, o is an integer from 0 to 2, X is selected from the group consisting of-F, -CF3, -OCF3, -FCF2C(CF3)2, and M is selected from a carboxyl group, a sulfo group or respective salts of the carboxyl group and the sulfo group; (ii) adding an initiator to initiate a microemulsion polymerization reaction of the trifluorostyrene monomer; and (iii) adding a coagulant for demulsification.

Description

technical field [0001] The invention relates to a preparation method of polytrifluorostyrene. The polytrifluorostyrene prepared by the method has high molecular weight or high glass transition temperature. Background technique [0002] Polytrifluorostyrene is an amorphous polymer with a high melting point. It combines the excellent properties of polytetrafluoroethylene and polystyrene. It not only has good heat resistance, low dielectric loss, and radiation resistance of polytetrafluoroethylene. And other properties, but also has a good solubility of polystyrene. In addition, polytrifluorostyrene has high transparency and has excellent optical properties and light transmission properties. Based on the above unique properties, polytrifluorostyrene has great application prospects in the fields of proton exchange membranes, ion exchange membranes, photoelectric communications, filter materials and microelectronics. [0003] Compared with conventional fluorine-containing monom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F114/18C08F2/26
CPCC08F114/185C08F2/26Y02E60/50
Inventor 杜丽君吴君毅袁利兵
Owner CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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