Method of preparing carboxyl styrene butadiene rubber through emulsion polymerization

A technology of carboxylated styrene-butadiene rubber and emulsion polymerization, which is applied in the field of surface-grafted carboxylated styrene-butadiene rubber raw materials by emulsion polymerization, which can solve problems such as unstable physical and mechanical properties, unstable characterization data, and uneven product mixing. Achieve the effect of improving the application range, controlling the combined acid index, and improving the modulus stress

Active Publication Date: 2016-07-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The current styrene-butadiene rubber is formed by binary copolymerization of butadiene and styrene. The terpolymerized carboxylated styrene-butadiene rubber has a high gel content due to the structure of more ether bonds and unsaturated bonds in the main chain. The physical and mechanical properties of the product after processing are poor, and the characterization data is unstable. The existing method to change the properties of styrene-butadiene rubber is to add polymers containing carboxyl components to the mixing formula to achieve the purpose of improving the physical and mechanical properties of styrene-butadiene rubber products. Complexity, many equipment requirements, pollution, high energy consumption, uneven mixing of final products, unstable physical and mechanical properties, and limited applications

Method used

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  • Method of preparing carboxyl styrene butadiene rubber through emulsion polymerization
  • Method of preparing carboxyl styrene butadiene rubber through emulsion polymerization
  • Method of preparing carboxyl styrene butadiene rubber through emulsion polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 5100 milliliters of water into a 10-liter reactor, add 38.09 grams of emulsifier A4 and 8.5 grams of reducing agent B, disperse and dissolve under stirring, add 467 grams of styrene, 4.65 grams of tert-dodecyl mercaptan, and Sodium disulfite 0.1692 grams, after nitrogen inflation-vacuum replacement, add 0.4726 grams of cumene peroxide, then add 1243 grams of butadiene, control the temperature to 11.5-12.5 ℃ for reaction, when the conversion rate reaches 55%, add emulsifier to synthesize fatty acid Continue the reaction after 105 grams of potassium soap, 25.65 grams of acrylic acid, and 0.45 grams of tertiary dodecyl mercaptan. When the reaction conversion rate reaches more than 68%, add 32 grams of terminators, degas after 30 minutes, and obtain latex, then coagulate and wash , dehydration, drying, and the results of glue sample testing are shown in Table 1:

[0035] Table 1

[0036]

Embodiment 2

[0038] at 3M 3 Add 1600 kilograms of water to the reaction kettle, then add 67.25 kilograms of potassium stearate solution and 61.39 kilograms of potassium oleate solution, 20 kilograms of potassium chloride solution, and 14.28 kilograms of diffusing agent N solution, disperse and dissolve under stirring, positive dodecyl 2.6 kilograms of mercaptans, add 254 kilograms of styrene, 46 kilograms of ammonium persulfate solution, and 576 kilograms of butadiene, and control the temperature to 7.5-8.5° C. for reaction. When the conversion rate reaches 52%, add emulsifier to synthesize 25.5 kilograms of potassium fatty acid solution Continue to react with 17.22 kilograms of methacrylic acid, and add 38 kilograms of terminator sodium nitrite solution after the reaction conversion rate reaches more than 70%, flash degassing after 30 minutes, obtain latex, then coagulate, wash, dehydrate, dry, The results of the glue sample test are shown in Table 2:

[0039] Table 2

[0040]

Embodiment 3

[0042] Add 4449 milliliters of water into a 10-liter reactor, add 473.56 grams of emulsifier A and 15.37 grams of reducing agent B, disperse and dissolve under stirring, add 454.59 grams of styrene, 4.75 grams of tertiary dodecyl mercaptan, and Sodium disulfite 0.179 grams, after nitrogen inflation-vacuum replacement, add 0.856 grams of dicumyl peroxide, then add 1440 grams of butadiene, control the temperature to 4.5-5.5 ℃ for reaction, when the conversion rate reaches 60%, add an emulsifier to synthesize Continue to react after 75 grams of potassium fatty acid solution, 25.9 grams of fumaric acid, 0.35 grams of tert-dodecyl mercaptan, add 35 grams of terminators after the reaction conversion ratio reaches more than 72%, degas after 30 minutes, obtain latex, and then After coagulation, washing, dehydration, and drying, the results of glue sample testing are shown in Table 3:

[0043] table 3

[0044]

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Abstract

The invention relates to a method of preparing carboxyl styrene butadiene rubber through emulsion polymerization. According to the method, styrene, an emulsifier, a conditioning agent, and an initiator are added into a polymerization kettle, then butadiene is added to carry out emulsion polymerization under stirring, and in the later period of reactions, unsaturated carboxylic acid and / or unsaturated carboxylic anhydride are added into the polymerization kettle. The prepared carboxyl styrene butadiene rubber has a low gel content, a controllable combined acid index, and a dual layer molecular structure; during the processing process, a three dimensional net-like structure can be formed easily; the mechanical and physical properties of rubber product are good, after processing, Mooney viscosity is increased, the crosslinking degree of finished product is good, and especially, the elongation at break is obviously improved.

Description

technical field [0001] The invention relates to a method for preparing carboxylated styrene-butadiene rubber by emulsion polymerization, in more detail, a method for producing surface-grafted carboxylated styrene-butadiene rubber raw materials by emulsion polymerization. Background technique [0002] At present, there are many methods for preparing styrene-butadiene rubber by emulsion method, such as continuous polymerization method and batch polymerization method. [0003] CN200710042967.6 discloses a styrene-butadiene emulsion and its preparation method and application. The preparation method comprises the following steps: carboxylic acid monomer, butadiene monomer, (methyl) styrene monomer, molecular weight regulator, emulsifier The aqueous solution of the mixture of the initiator and the initiator is subjected to free radical emulsion copolymerization, and the reaction time is 3 to 10 hours. The pH of the reaction product is adjusted to 7 to 10 with an alkaline substance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F279/02C08F220/06C08F222/02C08F222/08C08F220/04C08F2/26C08F2/42
Inventor 张元寿赵玉中赵继忠龚光碧梁滔钟启林桂强刘俊保翟云芳朱晶张志强詹常青燕鹏华史晓杰邵卫
Owner PETROCHINA CO LTD
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