Preparation method of ethylene-tetrafluoroethylene copolymer with high thermal stability

A technology with high thermal stability and tetrafluoroethylene, which is applied in the field of preparation of fluoropolymers, can solve the problems of limiting polymer performance and application fields, not improving the thermal stability of ETFE, and limiting the application of ETFE, reaching the product application range Wide range, good product performance, and large operating flexibility

Active Publication Date: 2018-08-24
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composition of the polymer determines the performance of the polymer, which in turn determines the use of the polymer. This solution limits the composition of the polymer, which will have adverse effects that limit the performance and application of the polymer.
At the same time, the scheme actually points out in which composition range ETFE has better thermal stability during processing, which is the property of the polymer itself, and does not improve the thermal stability of ETFE under this composition
[0006] Another example is that US3893971, US4110308, and US4267098 respectively propose adding alumina, copper compounds, phosphoric acid or phosphate to the prepared ETFE to improve the thermal stability of the polymer, but this method will introduce impurities in the ETFE resin, Thus limiting the application in fields requiring pure ETFE
[0007] So far, there is no report on improving the thermal stability of the prepared ETFE by starting from the polymerization system

Method used

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  • Preparation method of ethylene-tetrafluoroethylene copolymer with high thermal stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 60 kg of solvent C to a 100L stainless steel high-pressure vertical reactor 2 Cl 3 f 3 , and add 600 grams of liquid phase monomer perfluorohexylethylene, chain transfer agent methanol 50 grams, then add ethyl trifluoromethanesulfonate, its addition is C 2 Cl 3 f 3 0.3% by weight, start stirring and keep the temperature of the kettle at 80°C, and add the mixed gas of tetrafluoroethylene and ethylene (the molar ratio of tetrafluoroethylene to ethylene = 90:10) into the reaction kettle through a membrane press until the pressure is 20bar. Add 20 grams of diisopropyl peroxydicarbonate to initiate polymerization, and continue to add the mixed gas of tetrafluoroethylene and ethylene (tetrafluoroethylene and ethylene molar ratio=70:30) by membrane press simultaneously so that the reactor pressure is maintained at 20bar, and maintain the temperature of the kettle at 80°C. When the mixed gas of tetrafluoroethylene and ethylene reaches 4.8 kg, the polymerization reaction...

Embodiment 2

[0028] Add 78 kg of solvent C to the 100L stainless steel high-pressure vertical reactor 7 f 14 , and add 800 grams of liquid phase monomer perfluoropropyl vinyl ether, 150 grams of chain transfer agent cyclohexane, then add ethyl trifluoromethanesulfonate, and its addition is C 7 f 14 0.01% by weight, start stirring and keep the temperature of the kettle at 40°C, add the mixed gas of tetrafluoroethylene and ethylene (the molar ratio of tetrafluoroethylene to ethylene = 60:40) into the reaction kettle through a membrane press until the pressure is 10bar, Add 100 grams of tert-butyl peroxypivalate to initiate polymerization, and continue to add the mixed gas of tetrafluoroethylene and ethylene (tetrafluoroethylene and ethylene molar ratio=40:60) by membrane press simultaneously so that the reactor pressure is maintained at 10bar, and maintain the temperature of the kettle at 40°C. When the mixed gas of tetrafluoroethylene and ethylene reaches 3.3 kg, the polymerization reacti...

Embodiment 3

[0031] Add 51 kg of solvent CCl to a 100L stainless steel high-pressure vertical reactor 2 f 2 , and add 400 grams of liquid phase monomer perfluorobutyl ethylene, 150 grams of chain transfer agent acetone, then add ethyl trifluoromethanesulfonate, and its addition is CCl 2 f 2 0.1% by weight, start stirring and keep the temperature of the kettle at 60°C, add the mixed gas of tetrafluoroethylene and ethylene (the molar ratio of tetrafluoroethylene to ethylene = 75:25) into the reaction kettle through a membrane press until the pressure is 15bar, add 80 grams of tert-butyl peroxyisobutyrate start to initiate polymerization, while the mixed gas of tetrafluoroethylene and ethylene (tetrafluoroethylene and ethylene molar ratio=50:50) is continuously added by a membrane press so that the reactor pressure is maintained at 15bar , and maintain the temperature of the kettle at 60°C. When the mixed gas of tetrafluoroethylene and ethylene reaches 7.8 kg, the polymerization reaction is...

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Abstract

The invention discloses a preparation method of an ethylene-tetrafluoroethylene (ETFE) copolymer with high thermal stability. The preparation method comprises the following steps: based on weight parts, adding 500 to 1000 parts of solvent, 4 to 8 parts of liquid-phase monomer, 0.5 to 1.5 parts of chain transferring agent and 0.05 to 5 parts of ethyl trifluoromethanesulfonate into a reaction kettle; introducing a first mixed monomer of tetrafluoroethylene and ethylene to raise the pressure of the reaction kettle to 10 to 20bar; then adding 0.1 to 1 part of initiator and carrying out polymerization reaction at 40 to 80 DEG C; after the polymerization reaction is started, additionally adding a second mixed monomer of the tetrafluoroethylene and the ethylene and keeping the pressure of the reaction kettle at 10 to 20bar; when additionally adding the second mixed monomer to 20 to 100 parts, finishing the polymerization reaction; drying obtained slurry containing the ETFE to obtain an ethylene-tetrafluoroethylene product with the high thermal stability. The preparation method disclosed by the invention has the advantages of simple technology, great operation elasticity, good product performance and wide application field.

Description

technical field [0001] The invention relates to a preparation method of a fluorine-containing polymer, in particular to a preparation method of a highly thermally stable ethylene-tetrafluoroethylene copolymer. Background technique [0002] Ethylene-tetrafluoroethylene copolymer (ETFE or F40) is a fusible fluoropolymer, which retains the excellent chemical resistance, aging resistance and electrical properties of general fluoropolymers. The introduction makes ETFE have a lower specific gravity and excellent radiation resistance. [0003] However, when ETFE is processed and applied at high temperature, it is prone to degradation, which is manifested in the decrease of molecular weight (increase in melt index), decrease in tensile strength, discoloration and other phenomena, resulting in a decrease in product quality. Especially when the content of tetrafluoroethylene units in ETFE is high, the melting point of ETFE will rise, resulting in the narrowing of the temperature rang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F210/02C08F214/18C08F2/38C08F2/00
CPCC08F2/00C08F2/38C08F210/02C08F214/182C08F214/26C08F214/265C08F216/1408
Inventor 徐煜韬陈振华刘进朝赵洁余晓斌王树华
Owner JUHUA GROUP TECH CENT
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