Method for preparing fluorine-containing nitrile rubber through low-temperature emulsion polymerization

A technology of emulsion polymerization and fluorine-containing nitrile, which is applied in the field of preparation of fluorine-containing nitrile rubber by low-temperature emulsion polymerization, can solve the problems of not specifying the preparation method of ternary copolymer rubber, and achieve good elasticity, good stain resistance, The effect of improving performance

Active Publication Date: 2018-10-02
PETROCHINA CO LTD
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Problems solved by technology

[0008] JP Hei 1-242643A provides a rubber composition with improved cold resistance, a ternary copolymer rubber of acrylonitrile, butadiene and trifluoroethyl acrylate prepared by conventional emulsion polymerization and then hydrogenated to form a highly saturated hydrogenated Rubber, in order to achieve the effect of improving the cold resistance of rubber, and does not specify the preparation method of its ternary copolymerization rubber

Method used

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  • Method for preparing fluorine-containing nitrile rubber through low-temperature emulsion polymerization
  • Method for preparing fluorine-containing nitrile rubber through low-temperature emulsion polymerization
  • Method for preparing fluorine-containing nitrile rubber through low-temperature emulsion polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0047] In the reaction kettle, first add 25 parts of acrylonitrile, 2.1 parts of hexafluorobutyl acrylate, 2.9 parts of hexafluorobutyl methacrylate mixed monomer and 0.1 part of tm-200s, 75 parts of butadiene, 150 parts of water, 2.7 Part sodium dodecylbenzenesulfonate, 2.4 parts emulsifier A, 0.55 parts tert-dodecyl mercaptan, 0.2 parts sodium carbonate, 0.01 parts ferrous sulfate, 0.1 parts sodium formaldehyde sulfoxylate, 0.05 parts EDTA disodium salt , pre-emulsified for 40 minutes, then added 0.2 parts of cumene hydroperoxide, and controlled the temperature to carry out copolymerization at a polymerization temperature of 5°C. When reaching 80%, 0.4 part of diethylhydroxylamine was added to terminate the polymerization. The properties of the obtained fluorine-containing nitrile rubber are shown in Table 1.

Embodiment 2

[0060] In the reaction kettle, first add 20 parts of acrylonitrile and 10 parts of dodecafluoroheptyl methacrylate mixed monomer and 0.45 parts of tm-200s, 80 parts of butadiene, 250 parts of water, 1.8 parts of dodecylbenzenesulfonate Sodium phosphate, 5.5 parts of synthetic potassium fatty acid, 2.5 parts of emulsifier B, 1 part of emulsifier C, 1.2 parts of n-dodecyl mercaptan, 0.5 parts of sodium carbonate, 0.09 parts of EDTA iron sodium salt, 0.36 parts of glucose, 0.2 parts of amino tris Sodium acetate, pre-emulsified for 50min, then add 0.4 part of dicumyl hydroperoxide, and carry out copolymerization reaction at 8°C polymerization temperature under temperature control, and then add 0.08 part of n-dodecyl mercaptan when the conversion rate reaches 42%. When the conversion rate reached 75%, 0.3 parts of hydroquinone and 0.3 parts of diethylhydroxylamine were added to terminate the polymerization. The properties of the obtained fluorine-containing nitrile rubber are shown...

Embodiment 3

[0064] In the reaction kettle, first add 45 parts of acrylonitrile and 1 part of hexafluorobutyl acrylate mixed monomer and 0.0011 parts of tm-200s, 55 parts of butadiene, 300 parts of water, 1 part of synthetic fatty acid potassium, 4 parts of disproportionated abietic acid Potassium, 0.5 part of emulsifier C, 0.2 part of tertiary dodecyl mercaptan, 0.1 part of dithiodiisopropyl xanthate, 0.1 part of sodium acetate, 0.001 part of cuprous sulfate, 0.006 part of sodium formaldehyde sulfoxylate, 0.01 part of EDTA disodium salt, pre-emulsified for 30 minutes, then added 0.007 part of hydrogen peroxide p-menthane, controlled the temperature at 14°C for copolymerization reaction, and added 0.035 part of n-dodecane when the conversion rate reached 45% Mercaptan and 0.015 parts of dithiodiisopropyl xanthate, when the conversion rate reaches 84%, add 0.04 parts of diethylhydroxylamine and 0.07 parts of hydroquinone to terminate the polymerization. The properties of the obtained fluori...

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Abstract

The invention provides a method for preparing fluorine-containing nitrile rubber by adopting a low-temperature emulsion polymerization method and a product obtained by using the method. The fluorine-containing nitrile rubber is prepared by adopting a fluorine-containing monomer emulsion polymerization method. In the polymerization process, a chelating titanate coupling agent is adopted, so that the ternary copolymerization efficiency of a fluorine-containing monomer and acrylonitrile and butadiene can be remarkably improved. A molecular weight regulator needs to be added for multiple times, and preferably, at the first time, 0.2-1 part of the molecular weight regulator is added; and when the conversion rate reaches 40%-65%, 0.05-0.2 part of the molecular weight regulator is supplemented. The comprehensive performance of the fluorine-containing nitrile rubber prepared according to the method is improved, the prepared fluorine-containing nitrile rubber is high in oil resistance and highin tensile strength, compared with fluorine-containing nitrile rubber prepared according to a common method, the oil resistance of the fluorine-containing nitrile rubber prepared according to the method provided by the invention is improved by 20% or above, and the tensile strength is 30 MPa or above, and meanwhile, the fluorine-containing nitrile rubber is outstanding in high and low temperatureresistance and excellent in ageing resistance, and has the characteristics of being good in elasticity, high in stretching strength, low in compression set, good in abrasion resistance, good in weather resistance, good in stain resistance and narrow in molecular weight distribution.

Description

technical field [0001] The invention relates to the field of preparation of nitrile rubber, in particular to a method for preparing fluorine-containing nitrile rubber by using a low-temperature emulsion polymerization method using a fluorine-containing monomer. Background technique [0002] Nitrile rubber (NBR) has the advantages of excellent oil resistance, good tensile properties, heat resistance, air tightness, compression deformation, etc., but it is mostly used in ordinary oil-resistant products, and it is rarely used in fields with harsh environmental requirements , mainly due to the limited application temperature range and weather resistance. [0003] Fluorine-containing polymers have excellent weather resistance, high temperature resistance, stain resistance, electrical insulation, durability, and chemical resistance due to fluorine-containing bonds. Fluorine is the most electronegative element, the covalent radius of the fluorine atom is very small, the bond energ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/12C08F220/44C08F220/22C08F2/26C08F2/30C08L15/02
CPCC08F2/26C08F2/30C08F236/12C08L15/02C08F220/44C08F220/22
Inventor 桂强刘鹏李晶梁滔付含琦杨绮波宋同江张元寿田力钟启林郑红兵张志强龚光碧郑聚成曹凤霞胡育林李怀宁高志兴王真琴邵卫
Owner PETROCHINA CO LTD
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