Unsaturated copolymer hydrogenation method

A copolymer and unsaturated technology, which is applied in the field of unsaturated copolymers, can solve the problems of high hydrogenation degree of hydrogenation products, high catalyst application cost, and low hydrogenation reaction activity, so as to shorten the reaction time and short reaction time , Improve the effect of hydrogenation reaction activity

Active Publication Date: 2016-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects of high catalyst application cost, difficult implementation (high reaction temperature, complex operation, high energy consumption), low hydrogenation reaction activity and the degree of hydrogenation of hydrogenation products to be improved in the prior art method, Provide a catalyst with lower application cost, easier implementation (lower reaction temperature, simple operation, low energy consumption), high hydrogenation reaction activity, significantly improved hydrogenation degree of hydrogenated products and no obvious gel growth of hydrogenated products Hydrogenation method of unsaturated copolymer

Method used

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  • Unsaturated copolymer hydrogenation method
  • Unsaturated copolymer hydrogenation method
  • Unsaturated copolymer hydrogenation method

Examples

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Embodiment

[0037] The following examples will further illustrate the present invention, but do not limit the present invention thereby.

[0038] In the following examples and comparative examples, the measuring method of hydrogenation degree is bromoiodide method.

[0039] 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 360-mesh filter with constant weight (w2 grams) to filter, and then Dry the 360-mesh filter filled with insoluble matter to constant weight, record the weight as w3 grams, then the gel content is: (w3-w2) / w1*10 6 ppm.

[0040] Adopt nuclear magnetic analysis method to measure the cyano group reduction rate in hydrogenated nitrile butadiene rubber, concrete method is: take by weighing w4 gram dry glue, its cyano group content is A mass % (known), dissolves with deuterated chloroform, with styrene as Internal standard, the addition of styrene is M1 mol...

preparation example 1

[0044] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x m L n (P1) preparation method, wherein, M 1 for rhodium, M 2 is ruthenium, X is chlorine, L is triphenylphosphine, a:b is 2:1.

[0045] 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, and washed with ether to obtain a powdered Rh:Ru=2:1 catalyst for hydrogenation.

preparation example 2

[0047] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x m L n (P2) preparation method, wherein, M 1 for rhodium, M 2 is ruthenium, X is chlorine, L is triphenylphosphine, a:b is 3:1.

[0048] 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, washed with ether to obtain a powdered Rh:Ru=3:1 catalyst for hydrogenation.

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Abstract

The present invention discloses an unsaturated copolymer hydrogenation method, which comprises: (1) dissolving a unsaturated copolymer in an organic solvent, and carrying out inflation discharge deaeration; (2) adding a hydrogenation catalyst and a ligand, wherein the hydrogenation catalyst has the following general formula: M1aM2bXmLn; (3) introducing hydrogen, stirring, and carrying out a reaction, wherein the reaction conditions comprise that the reaction temperature is 0-30 DEG C, the hydrogen pressure is 0.05-15 Mpa, and the reaction time is 1-120 min; (4) heating to a temperature of 50-180 DEG C, maintaining the hydrogen pressure at 0.1-15 Mpa, and carrying out a reaction for 1-20 h; and (5) removing the organic solvent in the reaction product obtained in the step (4). With the method of the present invention, the catalyst application cost can be reduced, the reaction is easy to perform, the hydrogenation reaction activity is high, the hydrogenation degree of the hydrogenated product can be significantly improved, and the product does not have the significantly-increased gel content.

Description

technical field [0001] The invention relates to the field of unsaturated copolymers, in particular to a method for hydrogenating unsaturated copolymers, in particular to a method for preparing low-gel, highly saturated nitrile rubber. Background technique [0002] Hydrogenated nitrile rubber (HNBR) has good oil resistance, heat resistance, high temperature resistance, high pressure resistance, oxidation resistance and other properties, and also has excellent mechanical properties, and is widely used in automobile manufacturing, mechanical processing, metallurgical sealing, petroleum industry and other fields. [0003] For many years, the preparation of hydrogenated nitrile rubber has always been concerned by chemists, and its focus is mainly on: how to use a new, cheap catalyst system to prepare hydrogenated nitrile rubber products with high saturation and low gel content; How to realize the selective hydrogenation of carbon-carbon double bond (C=C) more efficiently through...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08C19/02C08F236/12B01J31/24
Inventor 梁爱民毕海鹏冯普凌李传清徐林李建成刘天鹤
Owner CHINA PETROLEUM & CHEM CORP
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