Preparation method of copolymer

A copolymer and unsaturated technology, which is applied in the field of copolymers, can solve problems such as the degree of hydrogenation of hydrogenation products needs to be improved, the cost of catalyst application is high, and the activity of hydrogenation reaction is low, so as to reduce the preparation cost, shorten the reaction time, improve The effect of hydrogenation reactivity

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
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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 The preparation method of the copolymer

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preparation example Construction

[0015] The invention provides a kind of preparation method of copolymer, and this method comprises the following steps:

[0016] (1) dissolving the unsaturated copolymer in an organic solvent to obtain a glue solution, which is filled and degassed;

[0017] (2) Add catalyst and ligand for hydrogenation, the catalyst for hydrogenation has the following general formula: (R m A) z wxya n , wherein, each R is independently selected from C1-C8 alkyl, C4-C8 cycloalkyl, C6-C15 aryl or C7-C15 aralkyl; A is selected from phosphorus, arsenic, sulfur or sub Sulfone group S=O; X is selected from hydrogen or anion; z is 2, 3 or 4; m is 2 or 3; n is 1, 2 or 3;

[0018] (3) Filling with hydrogen, stirring, and reacting, the conditions of the reaction include: the reaction temperature is 0-30°C, the hydrogen pressure is 0.05-15Mpa, and the reaction time is 1-120 minutes;

[0019] (4) heating up to 50-180°C, keeping the hydrogen pressure at 0.1-15Mpa, and reacting for 1-20 hours;

[0020]...

Embodiment 1-14

[0040] Embodiment 1-14 of the present invention is used to illustrate the preparation method of copolymer of the present invention:

[0041] (1) dissolving the unsaturated copolymer in an organic solvent to obtain a glue solution, which is added to the reaction kettle, and degassed;

[0042] (2) Add hydrogenation catalyst and ligand;

[0043] (3) Filling with hydrogen, stirring, and reacting, the conditions of the reaction include: the reaction temperature is b°C, the hydrogen pressure is aMPa, and the reaction time is c minutes;

[0044] (4) be warming up to e ℃, keep the hydrogen pressure as dMPa, and react for f hours;

[0045] (5) The hydrogenated product was condensed and precipitated by ethanol, and dried in vacuum at 60° C. for 8 hours.

[0046] In embodiment 1-14, unsaturated copolymer is all butadiene-acrylonitrile rubber, and the gel content of butadiene-acrylonitrile rubber is 304ppm, and the quality of glue solution is 540g, and glue solution concentration (i.e. ...

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Abstract

The invention discloses a preparation method of a copolymer. The method comprises the following steps: (1) dissolving an unsaturated copolymer in an organic solvent, and filling and draining and degassing; (2) adding a hydrogenation catalyst and a ligand, wherein the hydrogenation catalyst has the following general formula: (RmA)zRhXn; (3) filling hydrogen, stirring, and reacting at the reaction temperature of 0-30 DEG C and at hydrogen pressure of 0.05-15 Mpa for 1-120 min; (4) heating to 50-180 DEG C, keeping hydrogen pressure to 0.1-15 Mpa, and reacting for 1-20 h; and (5) removing an organic solvent in the reaction product obtained in the Step (4). By the method, application cost of the catalyst can be reduced, the reaction is easier to implement, hydrogenation reaction activity is high, hydrogenation degree of a hydrogenation product can be obviously raised, and the product has no obvious increase of gel content.

Description

technical field [0001] The invention relates to the field of copolymers, in particular to a method for preparing a copolymer, in particular to a method for preparing a 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 the continuous improveme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08C19/02
Inventor 毕海鹏李建成刘天鹤李传清徐林
Owner CHINA PETROLEUM & CHEM CORP
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