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A kind of method for preparing hydrogenated copolymer by hydrogenation of conjugated diene

A technology of conjugated dienes and hydrogenated copolymers, which is applied in the field of catalytic hydrogenation, can solve problems such as easy gel formation, poor conversion rate, and increased costs, and achieve the goals of improving catalytic efficiency, reducing industrial costs, and reducing catalyst consumption. Effect

Active Publication Date: 2021-10-26
SHANDONG CHAMBROAD PETROCHEMICALS CO LTD +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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  • A kind of method for preparing hydrogenated copolymer by hydrogenation of conjugated diene
  • A kind of method for preparing hydrogenated copolymer by hydrogenation of conjugated diene
  • A kind of method for preparing hydrogenated copolymer by hydrogenation of conjugated diene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0086] S1. Add 50 mL of latex and 0.00212 g of Hevida-Grubbs II to the reactor.

[0087] S2. Add 50 mL of latex and 2 g of potassium oleate, and stir at 200 rpm for 30 min.

[0088] S3. Introduce hydrogen 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.

[0089] S4. Raise the temperature to 90° C., raise the hydrogen pressure to 800 psi (5.52 MPa), and react for 1 hour. The hydrogenated NBR latex is coagulated with ethanol to obtain a HNBR copolymer.

[0090] The route of above-mentioned hydrogenation reaction is as follows:

[0091]

[0092] The samples before and after hydrogenation were tested by infrared test and hydrogen nuclear magnetic spectrum respectively, and the results were as follows: figure 1 and figure 2 as shown, figure 1 It is the infrared spectrogram of the sample before and after hyd...

Embodiment 2

[0096] S1. Add 50 mL of latex and 0.00212 g of Hevida-Grubbs II to the reactor.

[0097] S2. Add 50 mL of latex and 10 g of potassium oleate, and stir at 200 rpm for 30 min.

[0098] S3. Introduce hydrogen 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.

[0099] 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 30 minutes. The hydrogenated NBR latex is coagulated with ethanol to obtain a HNBR copolymer.

[0100] The results showed that no gel was produced in the reaction, and the obtained polymer was soluble in methyl ethyl ketone.

Embodiment 3

[0102] S1. Add 50 mL of latex and 0.00212 g of Hevida-Grubbs II to the reactor.

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

[0104] S3. Introduce hydrogen 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 hydrogen pressure to 800 psi (5.52 MPa), and react for 2 hours. 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.

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Abstract

The invention provides a method for preparing a hydrogenated copolymer by hydrogenating conjugated diene, comprising: a) mixing part of the conjugated diene latex with Hevida-Grubbs II catalyst to obtain a mixture A; b) mixing The remaining conjugated diene latex, the mixture A and the auxiliary agent are mixed to obtain the mixture B; the auxiliary agent is potassium oleate and / or sodium oleate; c) passing hydrogen into the mixture B for stirring and degassing After the treatment, continue the stirring treatment to obtain a mixture C; d) raise the temperature of the mixture C and increase the hydrogen pressure to carry out a hydrogenation reaction to obtain a hydrogenated copolymer. The present invention introduces specific additives through the mixing method of conjugated diene latex and Heveda-Grubbs II catalyst in batches, and degasses with hydrogen in advance and stirs after degassing The treatment method can efficiently realize the selective hydrogenation reaction of conjugated dienes under solvent-free conditions, and obtain products with high hydrogenation degree.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrogenation, in particular to a method for hydrogenating conjugated dienes to prepare hydrogenated copolymers. 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 large differenc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08C19/02
CPCC08C19/02
Inventor 王耀伟王辉马韵升黎艳艳栾波任学斌刘振学曹峰郝福兰周德芳郭宗磊佟伟超杜庆之王勇王英超
Owner SHANDONG CHAMBROAD PETROCHEMICALS CO LTD
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