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Hydrogenation method of butyronitrile latex

A technology for nitrile rubber and hydrogenation reaction is applied in the field of hydrogenation of nitrile latex, which can solve the problems that the hydrogenation degree of the hydrogenation product needs to be improved, the reaction activity of the hydrogenation catalyst is low, and the gel content of the product is high, and the reaction is shortened. Time, short response time, simple operation effect

Active Publication Date: 2017-09-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the higher production cost in the nitrile latex hydrogenation process of existing method, be difficult for implementing (reaction temperature is high, energy consumption is high), hydrogenation catalyst reactivity is lower, the degree of hydrogenation of hydrogenation product To improve the defects of higher gel content in the product, provide a method with lower production cost, easier implementation (lower reaction temperature, simple operation, low energy consumption), high hydrogenation reaction activity of the hydrogenation catalyst, and high hydrogenation product The hydrogenation method of the nitrile latex that the degree of hydrogenation is significantly improved and the hydrogenation product has no obvious gel growth

Method used

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Examples

Experimental program
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Effect test

Embodiment

[0040] The following examples will further illustrate the present invention, but do not limit the present invention thereby.

[0041] In the following examples and comparative examples, the method for determining the degree of hydrogenation is to test according to the method in the literature (nuclear magnetic analysis method for calculating the microstructure of hydrogenated nitrile rubber and the degree of hydrogenation. Petrochemical Industry, 2014, 43, 403).

[0042] Determination method of gel content: Weigh w1 gram of dry glue, add chlorobenzene to make a solution of 1g / 100mL, after dissolving for 24 hours, pour the solution into a filter screen with constant weight (w2 grams) to filter, and then put the The filter screen with insoluble matter is dried to constant weight, and the weight is recorded as w3 grams, then the gel content is: (w3-w2) / w1*10 6 ppm.

[0043] Hydrogenation catalyst (PPh 3 ) 3 RhCl was purchased from Acros Company and was denoted as C1.

[0044]...

preparation example 1

[0047] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x m L n The preparation method of (C2), wherein, M 1 for rhodium, M 2 is ruthenium, X is chlorine, L is triphenylphosphine, a:b:m:n is 2:1:4:9.

[0048] 4.5 g PPh 3 Dissolve in hot ethanol solution at 70°C under the protection of argon, and add the dissolved solution into the reaction flask; weigh 0.5 g of RhCl 3 .H 2 O and 0.23 g RuCl 3 .H 2 O was dissolved in ethanol solution under the protection of argon, heated to reflux at 78°C, and RhCl 3 .H 2 O and RuCl 3 .H 2 The ethanol solution of O was added dropwise into the reaction flask to react for 2.5 hours, cooled to 25°C, filtered with suction, washed with ether to obtain a powdered hydrogenation catalyst with Rh:Ru=2:1, denoted as C2.

preparation example 2

[0050] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x m L n The preparation method of (C3), wherein, M 1 for rhodium, M 2 is ruthenium, X is chlorine, L is triphenylphosphine, a:b:m:n is 3:1:5:12.

[0051] 6 g PPh 3 Dissolve in hot ethanol solution at 70°C under the protection of argon, and add the dissolved solution into the reaction flask; weigh 0.75 g of RhCl 3 .H 2 O and 0.23 g RuCl 3 .H 2 O was dissolved in ethanol solution under the protection of argon, heated to reflux at 78°C, and RhCl 3 .H 2 O and RuCl 3 .H 2 The ethanol solution of O was added dropwise into the reaction flask to react for 2.5 hours, cooled to 25°C, filtered with suction, and washed with ether to obtain a powdered hydrogenation catalyst with Rh:Ru=3:1, denoted as C3.

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Abstract

The invention relates to the hydrogenation field of butyronitrile latex, and discloses a hydrogenation method of butyronitrile latex. The method includes steps of (1), mixing butyronitrile latex, hydrogenation catalyst and ligand; (2), orderly performing first hydrogenation reaction and second hydrogenation reaction on the mixture obtained in step (1) in the presence of hydrogen, wherein the reaction temperature of the first hydrogenation reaction is 0-30 DEG C, and the reaction temperature of the second first hydrogenation reaction is 50-180 DEG C; (3), removing solvent in the reaction product obtained in step (2). The method is applied to perform hydrogenation on the butyronitrile latex, improve the hydrogenation activity of the hydrogenation catalyst and hydrogenation degree of the hydrogenation product; the hydrogenation product is free from obvious gel growth by comparing with the nitrile rubber before the butyronitrile latex before hydrogenation; moreover, the hydrogenation method is simple in operation, short in reaction time, easy to practice, and low in hydrogenation cost.

Description

technical field [0001] The invention relates to the field of hydrogenation of nitrile latex, in particular to a hydrogenation method of nitrile latex. Background technique [0002] In recent years, with the continuous development of automobile manufacturing, machining, metallurgical sealing, engineering construction, petroleum industry and other industries, the demand for high-end polymers is also rising. Hydrogenated nitrile rubber not only has good wear resistance, low temperature resistance, oxidation resistance, ozone resistance and other properties, more importantly, hydrogenated nitrile rubber has excellent thermal stability, these properties make it occupy a high-end polymer. A place, and the amount is increasing year by year. [0003] However, for hydrogenated nitrile rubber, its high price seriously restricts its promotion and application in various industries in my country. The main reasons for the long-term high price of hydrogenated nitrile rubber are as follow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08C19/02
CPCC08C19/02
Inventor 毕海鹏邵明波刘天鹤李建成徐林王雪
Owner CHINA PETROLEUM & CHEM CORP
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