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Method for preparing hydrogenated copolymer from conjugated diene hydrogenated latex

A technology of conjugated dienes and hydrogenated copolymers, which is applied in the field of hydrogenated copolymers prepared from conjugated dienes hydrogenated latex, can solve the problems of poor conversion rate, easy gel formation, environmental pollution, etc., and achieve the goal of reducing the total amount of additives. The effect of adding amount, improving catalytic efficiency and reducing industrial cost

Active Publication Date: 2020-06-19
山东京博中聚新材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, both methods have the problems of hydrogenation reaction rate, poor conversion rate and easy gel formation, and the hydrogenation reaction usually needs to be carried out in the presence of organic solvents. Due to the use of organic solvents, environmental pollution and cost increase

Method used

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  • Method for preparing hydrogenated copolymer from conjugated diene hydrogenated latex
  • Method for preparing hydrogenated copolymer from conjugated diene hydrogenated latex
  • Method for preparing hydrogenated copolymer from conjugated diene hydrogenated latex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0094] S1. Add 50 mL of latex and 0.000118 g of Hevida-Grubbs II into the reactor.

[0095] S2. Add 50 mL of latex, 2 g of potassium oleate, and 1 g of sodium tetradecenyl sulfonate, and stir at 200 rpm for 30 min.

[0096] S3. Nitrogen gas is introduced into the system, the degassing temperature is 25° C., the pressure is 2 MPa, the time is 60 minutes, and the stirring speed is 200 rpm during degassing; after the degassing is completed, continue stirring for 4 hours.

[0097] S4. Raise the temperature to 90° C., raise the nitrogen pressure to 800 psi (5.52 MPa), and react for 50 minutes. The hydrogenated NBR latex is coagulated with ethanol to obtain a HNBR copolymer.

[0098] Infrared tests were carried out on the samples before and after hydrogenation, and the results were as follows: figure 1 as shown, figure 1 It is the infrared spectrogram of the sample before and after hydrogenation in Example 1 of the present invention. Wherein the upper line is the raw material, t...

Embodiment 2

[0102] S1. Add 50 mL of latex and 0.000122 g of Hevida-Grubbs II into the reactor.

[0103] S2. Add 50 mL of latex, 2 g of potassium oleate, and 0.5 g of sodium tetradecenyl sulfonate, and stir at 200 rpm for 30 min.

[0104] S3. Nitrogen gas is introduced into the system, the degassing temperature is 25° C., the pressure is 2 MPa, the time is 60 minutes, and the stirring speed is 200 rpm during degassing; after the degassing is completed, continue stirring for 4 hours.

[0105] S4. Raise the temperature to 90° C., raise the nitrogen pressure to 800 psi (5.52 MPa), and react for 85 minutes. The hydrogenated NBR latex is coagulated with ethanol to obtain a HNBR copolymer.

[0106] The results showed that no gel was produced in the reaction, and the obtained polymer was soluble in methyl ethyl ketone.

Embodiment 3

[0108] S1. Add 50 mL of latex and 0.000117 g of Hevida-Grubbs II into the reactor.

[0109] S2. Add 50 mL of latex, 2 g of potassium oleate, and 0.3 g of sodium tetradecenyl sulfonate, and stir at 200 rpm for 30 min.

[0110] S3. Nitrogen gas is introduced into the system, the degassing temperature is 25° C., the pressure is 2 MPa, the time is 60 minutes, and the stirring speed is 200 rpm during degassing; after the degassing is completed, continue stirring for 4 hours.

[0111] S4. The temperature is raised to 90° C., the hydrogen pressure is raised to 800 psi (5.52 MPa), and the reaction is carried out for 150 minutes. The hydrogenated NBR latex is coagulated with ethanol to obtain a HNBR copolymer.

[0112] The results showed that no gel was produced in the reaction, and the obtained polymer was soluble in methyl ethyl ketone.

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Abstract

The invention provides a method for preparing a hydrogenated copolymer from a conjugated diene hydrogenated latex. The method comprises the following steps: mixing a part of a conjugated diene latex with a Hoveyda-Grubbs II catalyst so as to obtain a mixture A; mixing the residual conjugated diene latex, the mixture A and a composite auxiliary agent so as to obtain a mixture B, wherein the composite auxiliary agent is a combination of two or more selected from the group consisting of sodium oleate, potassium oleate, sodium tetradecenylsulfonate, potassium tetradecenylsulfonate, linear alkyl sulfate and alkyl betaine; introducing nitrogen into the mixture B, carrying out stirring and degassing treatment, and continuing stirring treatment so as to obtain a mixture C; and heating the mixtureC, introducing hydrogen, and carrying out a hydrogenation reaction so as to obtain the hydrogenated copolymer. According to the invention, through a batch-adding mixing mode, introduction of a specific composite auxiliary agent and stirring after nitrogen degassing treatment, selective hydrogenation of conjugated diene is realized; the usage amount of a catalyst is reduced; a high-hydrogenation-degree product is obtained; the reaction rate is increased; and the catalytic efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrogenation, in particular to a method for preparing a hydrogenated copolymer from a conjugated diene hydrogenated latex. Background technique [0002] The research and development of hydrogenated diene-based rubber products is mainly based on the application environment of rubber parts, through formula design and subsequent processing methods to obtain rubber products with required properties. At present, whether in the laboratory or in industrial production, there are mainly three ways to hydrogenate the parent diene-based unsaturated polymer to prepare hydrogenated diene-based rubber, such as nitrile rubber prepared by polymerization of acrylonitrile and butadiene (also known as NBR), taking NBR as an example, three preparation methods are as follows: [0003] (1) Acrylonitrile-ethylene copolymerization method. In the ethylene-acrylonitrile copolymerization reaction, since there is a larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08C19/02
CPCC08C19/02
Inventor 王辉曹峰郭宗磊佟伟超赵而英周德芳王勇杜庆之王传奇郝福兰王英超任学斌黎艳艳栾波
Owner 山东京博中聚新材料有限公司
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