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Preparation method of ethylene-tetrafluoroethylene copolymer resin

A tetrafluoroethylene copolymer resin and tetrafluoroethylene technology are applied in the field of fluorine-containing plastics and their preparation, which can solve the problems of high initiation temperature of inorganic peroxides, harsh storage and use conditions, and high initiator costs, and avoid high costs. And the problem of harsh use conditions, high shear mechanical strength, and the effect of solving high initiating temperature

Active Publication Date: 2012-10-10
泰兴梅兰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Domestic related reports on ETFE only involve processing and application fields, and there are no relevant patent reports on polymerization preparation; foreign ETFE preparation processes use organic peroxide initiators, which have the advantage of not requiring molecular tails Base treatment, the disadvantages are high cost of initiator, harsh storage and use conditions
In contrast, inorganic peroxides (such as ammonium persulfate, etc.) are low in cost and do not require special solvents, but the initiation temperature of inorganic peroxides in ETFE polymerization needs to be higher than 60 ° C, and low temperature in the copolymerization reaction is conducive to alternation The formation of structural ETFE, the initiation temperature of inorganic peroxides is too high, which has an adverse effect on the alternating structure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A preparation method of ethylene-tetrafluoroethylene copolymer resin, characterized in that the steps are:

[0018] ⑴ Evacuate and replace the gas mixing tank with a volume of 20L and its related pipelines, add tetrafluoroethylene gas to a gauge pressure of 0.7MPa (that is, an absolute pressure of 0.8MPa), and then add ethylene gas to a gauge pressure of 1.5MPa (absolute pressure of 1.6MPa) , the absolute pressure and partial pressure of tetrafluoroethylene and ethylene are both equal to 0.8MPa, that is, the number of moles is equal), and the gas in the tank is passed through an external circulating return line / pressurized buffer line by a compression pump to generate a circulating flow;

[0019] (2) Add 5 L of 1‰ ammonium persulfate solution to a 10L reaction kettle, use a circulating constant temperature tank to lower the temperature in the kettle to 10°C, add tetrafluoroethylene gas to a gauge pressure of 1.37MPa (absolute pressure 1.47MPa), and then Add ethylene gas...

Embodiment 2

[0023] Change the gas mixing tank volume into 10L among the embodiment 1, change the reactor volume into 2L, change the ammonium persulfate solution volume into 1 liter, change the ferrous sulfate solution volume into 150ml, change the metering pump flow into 75ml / h, other same Example 1 operation. The test results of this example are: fluorine content 58.99%; melting point 277.94°C, melting peak width 21°C; X-ray diffraction angle 18.620° single peak.

Embodiment 3

[0025] Change the gas mixing tank volume into 1000L among the embodiment 1, change the reactor volume into 500L, change the ammonium persulfate solution volume into 250 liters, change the ferrous sulfate solution volume into 3.75L, and change the metering pump flow into 1.875L / h, Others operate with embodiment 1. The test results of this example are: the fluorine content is 59.34%, the melting point is 275.66°C, the melting peak width is 30.3°C, and the X-ray diffraction angle is 18.780° single peak.

[0026] Elemental analysis characterizes the content of fluorine in the polymer. Through calculation, the corresponding fluorine content should be 59.375% when the molecular numbers of the two monomer components are equal (that is, the molar ratio is equal); XRD represents the X-ray diffraction angle, -CH 2 -CF 2 - 18.6° is the eigenvalue of the alternating structure, other structures - CF 2 -CF 2 -Diffraction angle is 25°, -CH 2 -CH 2 - According to different crystal forms,...

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PUM

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Abstract

The invention relates to a method for preparing ethylene-tetrafluoroethylene copolymer resin by utilizing an inorganic oxidation-reduction system, which solves the technical problems of high initiation temperature of inorganic peroxides and adverse influence on alternating structures, and belongs to the technical field of fluoroplastics. The method is characterized in that an independent gas-mixing tank and a pressurizing system of the gas-mixing tank are arranged, and the gas-mixing tank and a reaction kettle are connected through a check valve, so that gas can only flow from the mixing groove to the reaction kettle in a unidirectional manner; during polymerization reaction, the temperature is reduced to 10 DEG C and is kept constant, the following monomer is added and supplied in the form of mixed gas, and constant pressure is kept in the kettle; and the polymerization reaction adopts an ammonium persulfate-ferrisulphas inorganic redox initiation system. The method has the beneficial effects that the initiation temperature of the inorganic peroxides is lowered, the prepared copolymer resin is in an alternating copolymer structure, radiation-resisting and mechanical performances are improved to a great degree while the good performance of PTFE (Polytetrafluoroethylene) is kept, and the tensile strength can reach 50MPa which is approximately twice as that of the PTFE.

Description

technical field [0001] The invention belongs to the technical field of fluorine-containing plastics and preparation methods thereof, and relates to a preparation method of ethylene-tetrafluoroethylene copolymer resin, in particular to a method for preparing ethylene-tetrafluoroethylene copolymer resin initiated by an inorganic redox system. Background technique [0002] Ethylene-tetrafluoroethylene (ETFE) copolymer resin is a crystalline high polymer with a melting point of 256-280°C. It is self-extinguishing when burned. It is the strongest fluoroplastic with high shear mechanical strength and low-temperature impact resistance. , is the best among the existing fluoroplastics, while maintaining the good heat resistance, chemical resistance and electrical insulation properties of polytetrafluoroethylene (PTFE), radiation resistance and mechanical properties have been greatly improved. The tensile strength can reach 50MPa, nearly twice that of PTFE. The operating temperature ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/02C08F214/26C08F4/40
Inventor 司耀俊钱厚琴殷铭
Owner 泰兴梅兰新材料有限公司
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