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A kind of preparation method of hydrogenated nitrile rubber

A technology for hydrogenating nitrile-butadiene rubber and nitrile-butadiene rubber, which is applied to the preparation of hydrogenated nitrile-butadiene rubber, and the field of preparing hydrogenated nitrile-butadiene rubber from the catalytic hydrogenation of nitrile-butadiene rubber, can solve the difficulty of catalyst separation, harsh reaction conditions, low catalytic activity, etc. problem, to achieve the effect of high recycling efficiency, low cost and high catalytic activity

Active Publication Date: 2016-01-27
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, although the NBR homogeneous catalytic system is mature in technology, it has the disadvantages of difficult catalyst separation and high cost; although the heterogeneous catalytic system is simple to separate and recover the catalyst, its low catalytic activity leads to harsh reaction conditions. How to improve The catalytic activity of heterogeneous catalysts, organic combination of the advantages of homogeneous and heterogeneous catalytic systems, the development of new NBR hydrogenation process has important practical significance

Method used

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  • A kind of preparation method of hydrogenated nitrile rubber
  • A kind of preparation method of hydrogenated nitrile rubber
  • A kind of preparation method of hydrogenated nitrile rubber

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Embodiment 1

[0037] Present embodiment provides a kind of preparation method of hydrogenated nitrile butadiene rubber, it may further comprise the steps:

[0038] with PdCl 2 The HCl solution was used as the impregnation solution, and Pd was impregnated on the TM-SHMs by the equal volume impregnation method to prepare a heterogeneous catalyst Pd / TM-SHMs with an active metal Pd loading of 2wt.%. The transmission electron microscope (TEM) of the catalyst photos such as Figure 2a As shown, the Pd grain size distribution is as Figure 2b shown;

[0039] Dissolve 4g NBR in 100mL chlorobenzene solvent, add 0.4g heterogeneous catalyst Pd / TM-SHMs, 0.02g homogeneous catalyst triphenylphosphine rhodium chloride, 0.05g triphenylphosphine, in a high-pressure hydrogenation reactor Carry out catalytic hydrogenation reaction to obtain glue, the reaction conditions are: temperature 80°C, hydrogen pressure 6MPa, reaction time 5h;

[0040] After the reaction, the heterogeneous catalyst Pd / TM-SHMs was r...

Embodiment 2

[0042] Present embodiment provides a kind of preparation method of hydrogenated nitrile butadiene rubber, it may further comprise the steps:

[0043] With Pd(NH 3 ) 4 Cl 2 The ammonia solution was used as the impregnation solution, and Pd was loaded on TM-SHMs by ion exchange method to prepare a heterogeneous catalyst Pd / TM-SHMs with an active metal loading of 4wt.%.

[0044] Dissolve 5g NBR in 100mL acetone solvent, add 0.5g heterogeneous catalyst Pd / TM-SHMs, 0.02g homogeneous catalyst triphenylphosphine rhodium chloride, 0.05g triphenylphosphine rhodium chloride, and carry out in a high-pressure hydrogenation reactor Catalytic hydrogenation reaction to obtain glue, the reaction conditions are: temperature 60°C, hydrogen pressure 8MPa, reaction time 8h;

[0045] After the reaction, the heterogeneous catalyst Pd / TM-SHMs was recovered by centrifugation, and then the organic solvent was evaporated from the glue to obtain the product HNBR, and the degree of hydrogenation was l...

Embodiment 3

[0047] Present embodiment provides a kind of preparation method of hydrogenated nitrile butadiene rubber, it may further comprise the steps:

[0048] with RhCl 3 The HCl solution was used as the impregnating solution, and the Rh was impregnated on the TM-SHMs by the equal volume impregnation method to prepare the heterogeneous catalyst Rh / TM-SHMs with an active metal loading of 5wt.%.

[0049] Dissolve 5g NBR in 100mL tetrahydrofuran solvent, add 0.6g heterogeneous catalyst Pd / TM-SHMs, 0.02g homogeneous catalyst triphenylphosphine rhodium chloride, 0.05g triphenylphosphine, and carry out in a high-pressure hydrogenation reactor Catalytic hydrogenation reaction to obtain glue, the reaction conditions are: temperature 70°C, hydrogen pressure 5MPa, reaction time 6h;

[0050] After the reaction, the heterogeneous catalyst Rh / TM-SHMs was recovered by centrifugation, and then the organic solvent was evaporated from the glue to obtain the product HNBR, and the degree of hydrogenatio...

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Abstract

The invention relates to a hydrogenated butadiene-acrylonitrile rubber preparation method. The hydrogenated butadiene-acrylonitrile rubber preparation method is realized by catalytic hydrogenation of butadiene-acrylonitrile rubber, and comprises the following steps: silica hollow microspheres with through macroporea on the surface are taken as a carrier, the carrier is loaded with an active component to obtain a non homogeneous hydrogenation catalyst; 2 of 10g butadiene-acrylonitrile rubber is dissolved in 100mL organic solvent, the non homogeneous hydrogenation catalyst, triphenylphosphine chloro rhodium and triphenylphosphine are added for reaction to obtain a glue liquid; the glue liquid is centrifugally separated, the non homogeneous hydrogenation catalyst is recovered, the centrifugally separated glue liquid is evaporated to obtain the hydrogenated butadiene-acrylonitrile rubber. The method adopts the non homogeneous hydrogenation catalyst with high catalytic activity and high reuse efficiency, the homogeneous catalyst use amount is greatly reduced, and the method has the advantages of mild hydrogenation conditions, simple process and low cost.

Description

technical field [0001] The invention relates to a method for preparing hydrogenated nitrile rubber, in particular to a method for preparing hydrogenated nitrile rubber by catalytic hydrogenation of nitrile rubber, which belongs to the technical field of petrochemical industry. Background technique [0002] Hydrogenated nitrile rubber (HNBR) is a special rubber with excellent performance obtained by selectively hydrogenating the unsaturated olefin segment on the hydrocarbon chain of nitrile rubber (NBR), which has oil resistance, corrosion resistance, ozone resistance and weather resistance. , radiation resistance and other advantages, are widely used in automobiles, petroleum, machinery, aviation and other industries. [0003] At present, there are two main preparation methods of HNBR, namely homogeneous hydrogenation method and heterogeneous hydrogenation method. Homogeneous solution hydrogenation means that the active components of the catalyst are dispersed in the polyme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08C19/02C08F236/12B01J27/13B01J27/24
Inventor 鲍晓军袁珮潘登石冈龚光碧郑聚成艾纯金
Owner PETROCHINA CO LTD
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