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Method for preparing fluorine-containing polymer without containing perfluorocaprylic acid

A technology of perfluorooctanoic acid and polymers, applied in chemical instruments and methods, chemical/physical processes, transportation and packaging, etc., can solve problems such as untimely treatment, loss of anion resin particles, unavoidable gelation of anion exchange beds, etc., to avoid hazards Effect

Active Publication Date: 2010-06-23
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the final product of perfluoroalkyl compounds prepared by telomerization is a mixture of different carbon chains, and its carbon chain is relatively wide. How to control the reaction conditions to ensure the termination of the reaction within the required carbon chain range is difficult.
[0012] Some people have also used low-carbon chain fluorosurfactants (C1-C2), which have very significant shortcomings in the synthesis of fluoropolymers: that is, non-telomerization performance, which makes the transfer of low-carbon chains in the growth of polymer chains, resulting in Unwanted low-molecular-weight polymers are removed, affecting product quality
However, the above-mentioned recycling technology also has disadvantages: firstly, it is a problem of treatment efficiency. The fixed-bed anion exchange process can effectively feed the fluorosurfactant, and the concentration of C8 after treatment can be lower than 5PPM
However, it does not concentrate well for bulky polymer dispersions or latexes, so there is no time to deal with them
Each fluorinated body must be equipped with a dedicated anion exchange bed, which is difficult to ensure that recovery and bed washing can effectively avoid contamination
And the exchange column is often opened, and the gelation of the anion exchange bed cannot be avoided
Furthermore, for some polymer dispersions and flocs with large particles, the anion resin particles are easily broken and lost during the exchange.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Taking a 10L polymerization kettle as an example, add 7.2kg of ion-free water and 72g of emulsifier K to the cleaned polymerization kettle 2 o 3 SCF 2 (CF 2 OCF (CF 3 )) 3 COOK and 22g of initiator cumene hydrogen peroxide solution and other additives; evacuate and remove oxygen until the oxygen content ≤ 30ppm is qualified; After the kettle pressure reached the technological requirement, the polymerization reaction was started at a temperature of 150° C., and then 350 ml of carbon tetrachloride, a molecular weight regulator with a mass concentration of 3.0%, was poured in at a constant speed with a metering pump. During the polymerization reaction, keep the temperature and pressure of the kettle constant, and stop the reaction when a certain amount of reaction is reached. Condensation, washing, drying, crushing, and finally PVDF products.

Embodiment 2

[0030] Example 2: Changing the emulsifier to CF 3 CF 2 (CF 2 OCF (CF 3 )) 3 COOK, other operations are performed in the same manner as in Example 1.

Embodiment 3

[0035] Add 2500g deionized water, 25g (NH 4 ) 2 o 3 SCF 2 (CF 2 OCF (CF 3 )) 2 COONH 4 , Evacuate the reactor to ensure that the oxygen content is not greater than 30ppm. With the mass ratio of 20:80 tetrafluoroethylene and hexafluoropropylene mixed monomer, the polymerization kettle is boosted. When the pressure is 2.5MPa and the temperature reaches 85°C, inject 20ml of initiator potassium persulfate with a concentration of 10%, and Continue to feed a mixture of tetrafluoroethylene and hexafluoropropylene with a mass ratio of 80:20 to maintain the pressure in the reactor at 2.5 MPa. Thereafter, maintain the sub-pressure and temperature reaction, and stop the reaction when the reaction reaches a certain amount. The emulsion is coagulated, sintered and granulated to obtain FEP finished products.

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PUM

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Abstract

The invention belongs to the field of fluorine-containing polymer preparation, and provides a fluorine-containing emulsifying agent for replacing perfluorocaprylic acid and salt thereof. A2O3SCF2 (CF2OCF (CF3))n-1COOA, CF3CF2 (CF2OCF (CF3))n-1COOA, H3COOCF2 (CF2OCF (CF3))n-1COOA, in the formula, n is 1 to 4, and A is hydrogen atom, alkali metal or NH4. The invention also provides a method for preparing fluorine-containing polymer without containing perfluorocaprylic acid by using the fluorine-containing emulsifying agent. The fluorine-containing emulsifying agent of the invention has better emulsifying and dispersing effects, and the quality of an obtained product is in accordance with that of a reaction product in presence of PFOA.

Description

technical field [0001] The invention belongs to the field of fluorine-containing polymer preparation, and in particular relates to a preparation method of a fluorine-containing resin not containing perfluorooctanoic acid (PFOA). Background technique [0002] Fluorine containing surfactant is mainly a surfactant in which the hydrogen in the hydrophobic group of the hydrocarbon chain is partially or completely replaced by fluorine atoms, also known as fluorocarbon surfactant (fluorocarbonsurfactant), fluorinated Surfactant (fluorinated surfactant). The hydrophilic part of the fluorine-containing surfactant is the same as that of the ordinary hydrocarbon surfactant, and its classification is the same as that of the hydrocarbon surfactant. When it dissolves in water, it is called non-ionized. Ionic fluorocarbon surfactants are called ionic fluorocarbon surfactants that can be ionized, and the latter can be divided into anionic, cationic and amphoteric fluorocarbon surfactants a...

Claims

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Application Information

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IPC IPC(8): B01F17/00C08F14/18C08F2/24C09K23/00
Inventor 王汉利房瑾李文薇李秀芬郝宏伟
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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