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A kind of method that emulsion polymerization prepares carboxylated nitrile butadiene rubber

A technology of carboxyl nitrile rubber and emulsion polymerization, which is applied in the field of preparing carboxyl nitrile rubber by emulsion polymerization, can solve problems such as affecting product quality and service life, non-uniformity of molecular structure, affecting vulcanization strength, etc., and achieves the binding acid index. Controllable, improved application range, good dimensional stability

Active Publication Date: 2018-06-01
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Due to the presence of unsaturated bonds of acrylic acid, carboxylated nitrile rubber is particularly easy to form gel during the polymerization process. Since the gel has formed a three-dimensional network macromolecule of rubber before rubber processing, it will not dissolve in the rubber during rubber processing. In the rubber solution, it is easy to cause the heterogeneity of the molecular structure of the rubber product, which will affect the vulcanization strength. During the stress deformation process, the molecular chain will be broken, and the surface of the product will be cracked, which will seriously affect the quality and service life of the product.

Method used

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  • A kind of method that emulsion polymerization prepares carboxylated nitrile butadiene rubber
  • A kind of method that emulsion polymerization prepares carboxylated nitrile butadiene rubber
  • A kind of method that emulsion polymerization prepares carboxylated nitrile butadiene rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add water to a 10-liter reaction kettle, add 500.59 grams of emulsifier C and 29.7 grams of reducing agent B, disperse and dissolve under stirring, add 990 grams of acrylonitrile, 4.4 grams of tertiary dodecyl mercaptan, and 0.1692 grams of sodium dithionite, Nitrogen inflation-after vacuum replacement, add 2010 grams of butadiene, add 2.012 grams of cumene peroxide, and control the temperature to 11-13 ° C for reaction. When the conversion rate reaches 68%, add emulsifier synthetic fatty acid potassium soap 100 grams, acrylic acid After the mixture of 30 grams and 1.25 grams of tertiary dodecyl mercaptan, the temperature is controlled to 4.5 ~ 5.5 ° C to continue the reaction. When the reaction conversion rate reaches 85%, add 55 grams of sodium nitrite aqueous solution terminator, and flash degassing after 30 minutes , and then carry out coagulation, washing, dehydration, drying, after glue sample detection, the results are shown in Table 1:

[0031] Table 1

[0032]...

Embodiment 2

[0034] Add 1600 kg of water to the 3M3 reaction kettle, then add 60.5 kg of potassium stearate solution and 56.86 kg of potassium oleate solution, 21 kg of potassium chloride solution, and 14.98 kg of diffusing agent N solution, and disperse and dissolve under stirring. 61.6 kilograms of butyl solution, add 215.6 kilograms of acrylonitrile, 800 kilograms of ammonium persulfate solution, 625.8 kilograms of butadiene, heat up to 25~29 ℃ of reaction, add emulsifier synthetic fatty acid potassium soap 19.0 kilograms, oil 24.5 kilograms of potassium acid potassium solution, 35.5 kilograms of acrylic acid, 0.85 kilograms of tertiary dodecyl mercaptan emulsified liquid mixture, temperature control to 10~14 ℃ of reactions continue to react, when the reaction conversion rate reaches more than 85%, add terminator, 30 Minutes later, flash degassing, then coagulation, washing, dehydration, drying, after glue sample detection, the results are shown in Table 2:

[0035] Table 2

[0036] ...

Embodiment 3

[0038] Add 4549 milliliters of water into a 10-liter reactor, then add 425.50 grams of emulsifier C and 19.02 grams of reducing agent B, disperse and dissolve under stirring, add 456.60 grams of acrylonitrile, 3.9 grams of tertiary dodecyl mercaptan, and Sodium sulfite 0.17 grams, after nitrogen inflation-vacuum replacement, add 0.956 grams of cumene peroxide, 732 grams of butadiene, temperature control to 4.5~5.5 ℃ of reaction, when conversion rate reaches 64%, add emulsifier C 35 grams after, synthetic 35 grams of fatty acid potassium soaps, 0.35 grams of positive dodecyl mercaptans, 28 grams of methacrylic acid prefabricated emulsion mixtures to continue the reaction, add 25 grams of emulsifying agent emulsifier C, 15 grams of synthetic fatty acid potassium soaps when the conversion rate reaches 72% , after 26 grams of methacrylic acid prefabricated emulsion mixture, continue to react, when the reaction conversion rate reaches more than 89%, add the terminator, degas after 3...

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Abstract

The invention relates to a method for preparing carboxylated nitrile rubber by emulsion polymerization. Acrylonitrile, emulsifier, regulator and initiator are added to a polymerization kettle, and after adding butadiene, emulsion polymerization is carried out under stirring. In the later stage of the reaction, the The unsaturated carboxylic acid and / or its anhydride are added to the polymerization tank at the end of the reaction. The carboxyl nitrile butadiene rubber prepared by the method of the present invention has low gel content, controllable binding acid index, has a double-layer molecular structure, and is easy to form a three-dimensional network shape structure in the processing process, and has good physical and mechanical properties of the rubber product, and is easy to process. After the Mooney viscosity increases, the degree of crosslinking of the finished product is good, especially the elongation at break is significantly improved.

Description

technical field [0001] The invention relates to a method for preparing carboxylated nitrile rubber by emulsion polymerization. Background technique [0002] At present, there are many methods for preparing carboxylated nitrile rubber by emulsion method, such as continuous polymerization and batch polymerization. [0003] CN 1181390A describes a carboxylated nitrile rubber powder and its preparation process, wherein the carboxylated nitrile rubber components are butadiene, acrylonitrile, and carboxyl-containing unsaturated hydrocarbons, and their weight percentages are respectively 55-93%, 4-43% %, 1-6%, characterized in that in the emulsion polymerization reaction, a compound emulsifier containing an amphoteric emulsifier, a peroxide initiator, and dodecyl mercaptan are sequentially added, at 45-75°C: under reaction conditions, acrylonitrile Nitrile latex is obtained by binary copolymerization with butadiene. The pH value of the emulsion is controlled at 6.5-7, and the reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F279/02C08F220/06C08F220/08C08F222/02C08F222/06C08F220/44C08F236/06C08F2/24C08F4/40C08F2/38
Inventor 张元寿钟启林张茵刘俊保梁滔龚光碧赵玉中桂强翟云芳朱晶郑红兵张志强史工昌燕鹏华赵洪国史小文王真琴詹常青邵卫
Owner PETROCHINA CO LTD
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