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Process for preparing carboxylic acrylonitrile butadiene rubber through emulsion polymerization method

A carboxyl nitrile rubber and emulsion polymerization technology, which is applied in the field of producing carboxyl nitrile rubber raw materials with high content of microgel structure, can solve problems such as affecting product quality and service life, non-uniformity of molecular structure, affecting vulcanization strength, etc. , to achieve the effect of controllable binding acid index, good dimensional stability and good physical and mechanical properties

Active Publication Date: 2013-12-18
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Since the gel has formed a three-dimensional network macromolecule of rubber before rubber processing, it will not dissolve in the rubber solution during rubber processing, which will easily cause the inhomogeneity of the molecular structure of rubber products, which will affect the vulcanization strength. The process will cause the breakage of the molecular chain and cracks on the surface of the product, which will seriously affect the quality and service life of the product

Method used

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  • Process for preparing carboxylic acrylonitrile butadiene rubber through emulsion polymerization method
  • Process for preparing carboxylic acrylonitrile butadiene rubber through emulsion polymerization method
  • Process for preparing carboxylic acrylonitrile butadiene rubber through emulsion polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Add 5100 ml of water into a 10-liter reactor, then add 3.59 grams of CP-2034 and 8.7 grams of CP-50, disperse and dissolve under stirring, add 477 grams of acrylonitrile, 7 grams of acrylic acid, and 4.4 grams of tertiary dodecyl mercaptan, Sodium dithionite 0.1692 grams, after nitrogen inflation-vacuum replacement, add 678 grams of butadiene, add 0.4726 grams of cumene peroxide, control the temperature to 12±1°C for reaction, and add emulsifier when the conversion rate reaches 33±2% The mixture of 105 grams of CP-20 and 34 grams of ethylene glycol dimethacrylate continued to react, and when the conversion rate reached 70±2%, 105 grams of emulsifier CP-20 and 16 grams of ethylene glycol dimethacrylate were added , 0.45 g of tertiary dodecyl mercaptan, and then control the temperature to 5 ° C to continue the reaction. When the reaction conversion rate reaches more than 90%, add 2.58 g of tetraalkoxy titanate and 25 g of CP-20 mixed emulsion , after 10 minutes, add the t...

Embodiment 2

[0070] at 3M 3 Add 1600 kilograms of water to the reaction kettle, then add 55.96 kilograms of potassium stearate solution and 54.56 kilograms of potassium oleate solution, 20 kilograms of potassium chloride solution, 14.98 kilograms of diffusing agent N solution, disperse and dissolve under stirring, and adjust agent D solution 61.6 kg, add 210.6 kg of acrylonitrile, 41.5 kg of acrylic acid, 800 kg of potassium persulfate solution, 622.2 kg of butadiene, heat up to 45±2°C for reaction, and add emulsifier potassium stearate when the conversion rate reaches 33±2%. After the mixture of 9.6 grams of solution, 4.7 kilograms of potassium oleate solution and 16.16 kilograms of ethylene glycol dimethacrylate, the reaction was continued, and the conversion rate reached 73% ± 2 hours, and 9.0 kilograms of emulsifier potassium stearate solution, potassium oleate After the emulsion mixture of 4.5 kg of solution, 4.04 kg of ethylene glycol dimethacrylate, and 0.85 kg of tert-dodecyl merca...

Embodiment 3

[0074] Add 4449 ml of water into a 10-liter reactor, then add 405.50 grams of CP-20 and 16..02 grams of CP-50, disperse and dissolve under stirring, add 456.60 grams of acrylonitrile, 81 grams of methacrylic acid, t-12 3.9 grams of carbon mercaptan, 0.17 grams of sodium dithionite, nitrogen inflation-after vacuum replacement, add 0.856 grams of cumene peroxide, control the temperature to 5±0.5°C for reaction, and add emulsifier CP when the conversion rate reaches 30±2%. -20 95 grams, 26.51 grams of ethylene glycol dimethacrylate, 0.65 grams of n-dodecyl mercaptan prefabricated mixture emulsion and continue the reaction. When the conversion rate reaches 70 ± 2%, add emulsifier CP-20 75 grams, After the prefabricated emulsion mixture of 0.35 g of n-dodecyl mercaptan and 25 g of ethylene glycol dimethacrylate, the reaction is continued, and when the reaction conversion rate reaches more than 90%, 68.68 g of tetraalkoxy titanate and CP-20 105 grams of mixed emulsion, add terminato...

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Abstract

The invention relates to a process for preparing carboxylic acrylonitrile butadiene rubber through an emulsion polymerization method. An emulsifier and an adjusting agent are added in batch, and a crosslinking agent and a pre-crosslinking agent titanate are added at different times, so the carboxylic acrylonitrile butadiene rubber has the characteristics of high content of a microgel, low content of a gel, controllable combined acid index, easy formation of a stereo netted structure in the processing process, uniform distribution of carboxylic groups on a molecular chain, uniform structure formed in the vulcanizing and product processing processes, slight stress relax phenomenon, and good dimension stability. The rubber obtained through adopting the method has good physical and mechanical properties and an improved Mooney viscosity, and has corresponding better compression set, Shore A hardness, tearing strength, tensile strength, elongation at break and 100% stress at definite elongation than common carboxylic rubber.

Description

technical field [0001] The invention relates to a method for preparing carboxylated nitrile butadiene rubber by emulsion polymerization, in more detail, a method for producing carboxylated nitrile butadiene rubber raw materials with higher microgel structure content 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] During the polymerization process of rubber production, insoluble substances in good rubber solvents will be generated due to increased branching of rubber molecules and chemical crosslinking between molecules, that is, insoluble substances when rubber is in a viscous fluid state. It is the increase of the branching of a single linear molecule (branch molecular chain growth) or the three-dimensional network-shaped macromolecule formed by the interaction between linear molecules, which is calle...

Claims

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Application Information

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IPC IPC(8): C08F236/12C08F220/06C08F222/02C08F2/24C08F2/38
Inventor 张元寿张茵姜平李晶龚光碧钟启林翟云芳吴宇郑聚成徐典宏王锋季江东胡育林陈跟平康安福
Owner PETROCHINA CO LTD
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