Preparation of silane coupling agent-modified SiO2 loaded rhodium catalyst and selective hydrogenation application of catalyst to butadiene-acrylonitrile rubber

A silane coupling agent, rhodium catalyst technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, sustainable manufacturing/processing, etc. It is easy to adsorb polymer molecules and reduce the efficiency of the catalyst, so as to achieve the effect of improving the catalytic efficiency, simplifying the preparation process and saving production costs.

Active Publication Date: 2014-01-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrogenation activity of general supported heterogeneous catalysts is not as good as that of homogeneous catalysts, and the surface of the carrier is also easy to adsorb polymer molecules, and the catalyst efficiency is greatly reduced.
In addition, heterogeneous catalysts require higher hydrogen pressure and reaction temperature, and longer reaction time, which will have some impact on the structure and properties of the final product HNBR

Method used

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  • Preparation of silane coupling agent-modified SiO2 loaded rhodium catalyst and selective hydrogenation application of catalyst to butadiene-acrylonitrile rubber
  • Preparation of silane coupling agent-modified SiO2 loaded rhodium catalyst and selective hydrogenation application of catalyst to butadiene-acrylonitrile rubber
  • Preparation of silane coupling agent-modified SiO2 loaded rhodium catalyst and selective hydrogenation application of catalyst to butadiene-acrylonitrile rubber

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Experimental program
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preparation example Construction

[0024] APTS modified SiO 2 The process of the preparation method is as follows:

[0025] Add 300ml deionized water to a three-neck flask, weigh 5g of SiO 2 Import into the bottle, add 4ml of APTS, stir and react for 2 hours at 40°C, add dropwise 8ml of ammonia water (w25%), react for 4 hours, filter and dry to obtain APTS modified SiO 2 .

[0026] Supported Catalyst APTS-SiO 2 -RhCl 3 The preparation method steps are as follows:

[0027]Immersion method, take by weighing 1.0g rhodium chloride, be mixed with the rhodium chloride solution that concentration is 1g / L, drop 20ml rhodium chloride solution in 2.0g APTS modified SiO 2 Add it dropwise evenly, let it stand for 10h, wash it, and dry it in an oven to get APTS-SiO 2 -RhCl 3 catalyst.

[0028] APTS-SiO 2 -RhCl 3 The general steps of carrying out solution method catalytic hydrogenation to nitrile rubber with supported catalyst are as follows:

[0029] Prepare nitrile rubber into a solution with a certain concentra...

example 1

[0031] According to the above-mentioned general steps of hydrogenation, measure 120ml of the prepared nitrile rubber chlorobenzene glue with a graduated cylinder, the concentration of the glue is 3%, and add it to a 0.5L high-pressure reactor, APTS modified SiO 2 Post-prepared supported catalyst APTS-SiO 2 -RhCl 3 The mass is 0.6g, triphenylphosphine (PPh 3 ) dosage is 0.6g. Under the conditions of reaction temperature of 120°C and hydrogen pressure of 3.0 MPa, react for 8 hours, cool to obtain the product, condense with ethanol, dry in a vacuum oven, and measure the degree of hydrogenation. The experimental results are shown in Table 1

example 2

[0037] Modified SiO by APTS above 2 In the modification process, the deionized water is replaced with ethanol, water-ethanol (volume ratio is 1:1) mixed solution. Preparation of Supported Catalyst APTS-SiO 2 -RhCl 3 The process of hydrogenation is the same, and the hydrogenation step is also the same. To study the influence of different modified solvents on the degree of hydrogenation of NBR. The experimental results are shown in Table 2

[0038] Table 2 The influence of different modified solvents on the degree of hydrogenation of NBR

[0039]

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Abstract

The invention discloses preparation of a silane coupling agent-modified SiO2 loaded rhodium catalyst and a selective hydrogenation application of the catalyst to butadiene-acrylonitrile rubber. The method comprises the following steps: (1) carrier modification, namely, modifying SiO2 by utilizing a silane coupling agent with an amino group in an organic solution or water so as to obtain modified SiO2; and (2) loading catalyst preparation, namely, adding the modified SiO2 into a rhodium solution, standing, washing and drying so as to obtain the loaded catalyst APTS (aminopropyltriethoxysilane)-SiO2-Rh. The prepared catalyst is used for nitrile butadiene rubber (NBR) hydrogenation research, and the hydrogenated butadiene-acrylonitrile rubber with the hydrogenation strength being more than 98% can be obtained. The preparation process is simple, and the adopted reaction raw materials are wide in source scope and small in toxicity and are economic and practicable. The NBR hydrogenation research shows that the hydrogenation efficiency is greatly improved, the hydrogenation strength is improved to above 98% from the original 52% under the same condition, and moreover, the recycling performance of the catalyst is also greatly improved after the reaction is ended. The APTS-SiO2-Rh is a high activity recycled NBR hydrogenation heterogeneous catalyst and is beneficial to HNBR (hydrogenated butadiene-acrylonitrile rubber) large-scale production.

Description

[0001] The invention relates to a silane coupling agent modified SiO 2 Supported rhodium catalyst and its application to NBR hydrogenation. The preparation process of the supported catalyst is simple. It can perform catalytic hydrogenation on polymers containing carbon-carbon double bonds such as NBR, showing high hydrogenation activity, good selectivity and good of recycling. Background technique [0002] Catalytic hydrogenation technology is an important method for chemical modification of organic matter in petrochemical industry. The catalysts used are divided into homogeneous catalysts and heterogeneous catalysts. In the process of catalytic hydrogenation, the recovery and regeneration of catalyst is an urgent problem in production. Therefore, in order to better separate the catalyst and the product after the reaction, a heterogeneous catalyst, that is, a supported catalyst, is generally used. Some active centers (mainly some noble metal elements, such as nickel, rhodium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/13B01J31/24C08C19/02
CPCY02P20/50Y02P20/584
Inventor 岳冬梅曹朋邓磊张立群刘堃
Owner BEIJING UNIV OF CHEM TECH
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