Method for producing hydrogenated copolymer through hydrogenation of conjugated diene

A technology of conjugated diene and hydrogenated copolymer, applied in the field of catalytic hydrogenation, can solve the problems of easy formation of gel, poor conversion rate, increased cost, etc. Effect

Active Publication Date: 2019-12-31
SHANDONG JINGBO PETROCHEM +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 producing hydrogenated copolymer through hydrogenation of conjugated diene
  • Method for producing hydrogenated copolymer through hydrogenation of conjugated diene
  • Method for producing hydrogenated copolymer through 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 producing a hydrogenated copolymer through hydrogenation of conjugated diene. The method for producing the hydrogenated copolymer through hydrogenation of the conjugated diene comprises the following steps: (1) mixing part of conjugated diene latex and a Hoveyda-Grubbs II catalyst to obtain a mixture A; (2) mixing the rest of conjugated diene latex, the mixtureA and assistants to obtain a mixture B, wherein the assistants are potassium oleate and / or sodium oleate; (3) introducing hydrogen into the mixture B for stirring and degassing treatment, and then conducting stirring treatment continuously to obtain a mixture C; and (4) heating the mixture C, and improving hydrogen pressure for a hydrogenation reaction to obtain the hydrogenated copolymer. According to the method for producing the hydrogenated copolymer through hydrogenation of the conjugated diene, through a mixing mode where the conjugated diene latex and the Hoveyda-Grubbs II catalyst are added in batches, introduction of the specific assistants, and a treatment method where the hydrogen is adopted for degassing treatment in advance, and stirring is conducted after degassing treatment is conducted, the selective hydrogenation reaction of the conjugated diene can be efficiently achieved without solvents to obtain a product with a 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 Applications(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 JINGBO PETROCHEM
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