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Preparation method of low-temperature-resistant binary fluorine rubber

A binary fluororubber, low-temperature-resistant technology, applied in the field of preparation of low-temperature-resistant binary fluororubber, can solve the problems of low yield, slow polymerization speed, expensive production cost, etc., achieve less dosage, simple preparation process, reduce The effect of production costs

Active Publication Date: 2013-07-10
ZHEJIANG FLUORINE CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This directly leads to very expensive production costs. On the other hand, the higher the PMVE content, the lower the reactivity of the comonomers, the slower the polymerization rate, and the lower the yield, which is very unfavorable for mass commercial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] at 1m 3 In the polymerization reactor, the air in the reactor is removed by filling with water, and then purged with nitrogen, the lower the oxygen content, the better. Then 450Kg of distilled water, 0.65Kg of potassium persulfate, and 0.15Kg of ammonium perfluorooctanoate are introduced into the reactor, and a monomer mixture composed of VDF, HFP, and PMVE in a molar ratio of 73:24:3 is introduced into the middle tank, and the storage tank is The pressure is 5MPa, normal temperature. A certain amount of monomer mixture is delivered to the reactor through the outlet at the bottom of the storage tank, so that the pressure in the reactor reaches 0.35 MPa. The reaction mixture was heated to 73 °C. The pressure was adjusted to 2.0 MPa by introducing more of the above monomer mixture. After the reaction started, the pressure dropped, and the above-mentioned monomer mixture was periodically introduced to maintain a stable pressure, while maintaining a stirring rate of 550 ...

Embodiment 2

[0027] at 1m 3 In the polymerization reactor, the air in the reactor is removed by filling with water, and then purged with nitrogen, the lower the oxygen content, the better. Then 450Kg of distilled water, 0.15Kg of potassium persulfate, and 0.10Kg of ammonium perfluorooctanoate are introduced into the reactor, and a monomer mixture composed of VDF, HFP, and PMVE in a molar ratio of 70:24:6 is introduced into the intermediate tank, and the storage tank is The pressure is 5MPa, normal temperature. A certain amount of monomer mixture is delivered to the reactor through the outlet at the bottom of the storage tank, so that the pressure in the reactor reaches 0.40 MPa. The reaction mixture was heated to 85 °C. The pressure was adjusted to 2.5 MPa by introducing more of the above monomer mixture. After the reaction started, the pressure dropped, and the above-mentioned monomer mixture was introduced periodically to maintain a stable pressure, while maintaining a stirring rate o...

Embodiment 3

[0029] at 1m 3In the polymerization reactor, the air in the reactor is removed by filling with water, and then purged with nitrogen, the lower the oxygen content, the better. Then 450Kg distilled water, 0.35Kg ammonium persulfate, 3.3Kg perfluorooctanoic acid are introduced in the reactor, VDF, HFP, PMVE are introduced in the intermediate tank with the monomer mixture formed by the molar ratio of 64:28:8, and the storage tank is made The pressure is 5MPa, normal temperature. A certain amount of monomer mixture is delivered to the reactor through the outlet at the bottom of the storage tank, so that the pressure in the reactor reaches 0.38MPa. The reaction mixture was heated to 78 °C. The pressure was adjusted to 1.5 MPa by introducing more of the above monomer mixture. After the reaction started, the pressure dropped, and the above-mentioned monomer mixture was periodically introduced to maintain a stable pressure, while maintaining a stirring rate of 580r / min to maintain t...

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Abstract

The invention relates to a preparation method of low-temperature-resistant binary fluorine rubber, belonging to the technical field of fluorine chemical industry. The preparation method is characterized by comprising the following steps of: 1) mixing 1,1-difluoroethylene, hexafluoropropylene and perfluoro methyl vinyl ether in a molar ratio of (60-80):(15-30):(2-8) to obtain a monomer mixture forlater use; and 2) reacting the monomer mixture in an aqueous dispersion form under the action of an initiator, an emulsifier and a chain transfer agent in a reaction kettle, adjusting the temperatureto 60-95 DEG C, pressure to 1.0-3.0MPa and stirring rate to 400-700 r / min, and carrying out copolymerization reaction for 3-7 hours to obtain a finished product. The preparation method of the low-temperature-resistant binary fluorine rubber has the advantages that the preparation process is simple, the use amount of expensive perfluoro methyl vinyl ether in the reaction is low, and the productioncost is greatly lowered; and the glass transition temperature of the prepared fluorine rubber can be effectively reduced by 2-7 DEG C and the brittleness temperature is reduced by 10-18 DEG C, thereby being suitable for low-temperature sealing requirements.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical industry, in particular to a preparation method of low temperature resistant binary fluorine rubber. Background technique [0002] Binary fluororubbers based on 1,1-difluoroethylene (VDF) and hexafluoropropylene (HFP) have outstanding properties such as high temperature resistance, oil resistance, chemical corrosion resistance and aging resistance, but at the same time have poor low temperature resistance. Weaknesses, usually the glass transition temperature (Tg) of binary fluororubber is -17°C, and the brittle temperature (Th) is -20°C. [0003] However, relative to many engineering applications, the key application threshold is that Tg does not exceed -19°C and Th does not exceed -30°C. Therefore, rubber engineers have made great efforts to improve the low temperature flexibility of fluororubber. Generally, the low-temperature performance of fluororubber mainly depends on the molecula...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F214/22C08F214/28C08F216/14C08F2/38C08F2/24B29B7/00
Inventor 苗国祥王振兴李晓育陈炜
Owner ZHEJIANG FLUORINE CHEM NEW MATERIAL
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