Preparation method of carboxyl nitrile rubber through emulsion polymerization

A technology of carboxylated nitrile rubber and emulsion polymerization, which is applied in the field of emulsion polymerization to prepare carboxylated nitrile rubber, which can solve problems affecting product quality and service life, molecular structure non-uniformity, product surface cracking, etc., and achieve the goal of combining acid The index is controllable, the application range is improved, and the cross-linking degree is good.

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

[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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  • Preparation method of carboxyl nitrile rubber through emulsion polymerization
  • Preparation method of carboxyl nitrile rubber through emulsion polymerization
  • Preparation method of carboxyl nitrile rubber through emulsion polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add water to a 10-liter reactor, add 0.59 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 gram, after nitrogen inflation-vacuum replacement, add 2010 grams of butadiene, add cumene peroxide 2.012 grams, temperature control is to 11~13 ℃ of reaction, when conversion ratio reaches 68%, add emulsifier synthetic fatty acid potassium soap 100 grams , a mixture of 30 grams of acrylic acid and 1.25 grams of tertiary dodecyl mercaptan, and 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, flash after 30 minutes Degassing, then 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 25.50 grams of emulsifier C4 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, 0.17 grams of sodium dithionite, after nitrogen inflation-vacuum replacement, add 0.956 grams of cumene peroxide, 732 grams of butadiene, and control the temperature to 4.5-5.5 ° C for reaction. When the conversion rate reaches 64%, add 35 grams of emulsifier C, 35 grams of synthetic fatty acid potassium soaps, 0.35 grams of positive dodecyl mercaptans, 28 grams of methacrylic acid prefabricated emulsion mixtures and continue to react, 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, de...

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Abstract

The invention relates to a preparation method of carboxyl nitrile rubber through emulsion polymerization. According to the preparation method, acrylonitrile, an emulsifier, an adjusting agent, and an initiator are added into a polymerization kettle, then butadiene is added, emulsion polymerization is carried out under stirring, and in the late phase of emulsion polymerization, unsaturated carboxylic acid and / or anhydride thereof is added into the polymerization kettle. The obtained carboxyl nitrile rubber has a low content of gel and a two-layer molecular structure, the index of conjugated acid is controllable; during the processing process, a three-dimensional network structure can be easily formed, thus the mechanical and physical properties of rubber products made of the carboxyl nitrile rubber are good; after processing, the Mooney viscosity is increased, the crosslinking degree of finished products is good, and especially, the elongation at break is prominently 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] CN1181390A 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 the weight percentages are 55-93% and 4-43% respectively , 1~6%, characterized in that in the emulsion polymerization reaction, sequentially add a composite emulsifier containing an amphoteric emulsifier, a peroxide initiator, and dodecyl mercaptan, at 45~75°C: under reaction conditions, acrylonitrile and Nitrile latex is obtained by binary copolymerization of butadiene, the pH value of the emulsion is controlled at 6.5-7, and the reaction...

Claims

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Application Information

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Patent Type & Authority Applications(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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