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Silica-supported platinum-containing hydrosilylation catalyst and its preparation method and application

A silicon dioxide and hydrogen addition technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, catalytic reaction, etc., can solve the problem of low activity and selectivity, difficulty in separation and recovery, stable Poor properties and other problems, to achieve the effect of large specific surface area, easy separation, high stability

Active Publication Date: 2018-03-20
国科广化(南雄)新材料研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the most homogeneous catalysts used in industry are Speier catalyst (isopropanol solution of chloroplatinic acid) and Karstedt catalyst ([(ViMe 2 Si) 2 O]PtCl 2 ), these homogeneous catalysts have high activity, but there are also disadvantages such as difficult separation and recovery, high cost, and poor stability.
The heterogeneous catalysts commonly used in hydrosilylation are formed by adsorbing transition metals on inorganic particles such as carbon black and alumina. The advantages of this type of heterogeneous catalysts are relatively high stability, easy recovery, and reusability. and less selective

Method used

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  • Silica-supported platinum-containing hydrosilylation catalyst and its preparation method and application
  • Silica-supported platinum-containing hydrosilylation catalyst and its preparation method and application
  • Silica-supported platinum-containing hydrosilylation catalyst and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0042] (2) Add 10.0 g of surface hydroxylated silica to 80.0 g of analytically pure toluene, disperse evenly with 800 W ultrasonic for 30 min, and then add 20.0 g of functional organic ligands (shown in formula I) dropwise to silica and In the mixed solution of toluene, magnetically stir the reaction at 50°C for 20h. After the reaction is completed, filter it with a Buchner funnel covered with filter paper, wash the obtained precipitate with analytically pure toluene five times, each time with 20mL of analytically pure toluene, and then Vacuum drying to obtain the organic ligands supported by silica;

[0043] (3) Dissolve 0.4g of analytically pure chloroplatinic acid in 8.0g of analytically pure ethanol, then add 10.0g of the silica-immobilized organic ligand and 1.0g of analytically pure sodium bicarbonate prepared in step (1), 600W Ultrasound for 50 minutes to disperse evenly, under the condition of atmospheric nitrogen, stir and react at 50°C for 6 hours, stop heating and s...

Embodiment 2

[0045] (2) Add 10.0 g of surface hydroxylated silicon dioxide to 100.0 g of analytically pure carbon tetrachloride, disperse evenly with 800 W ultrasound for 30 min, and then add 30.0 g of functional organic ligands (shown in formula I) dropwise to the two In the mixed solution of silicon oxide and carbon tetrachloride, stir and react with magnetic force at 70°C for 20 hours, centrifuge after the reaction is completed, wash the obtained precipitate with analytically pure carbon tetrachloride five times, each time with 20 mL of analytically pure carbon tetrachloride , and then vacuum-dried at room temperature to obtain a silica-immobilized organic ligand;

[0046](3) 0.8g analytical pure chloroplatinic acid is dissolved in 20.0g analytical pure isopropanol, then add the organic ligand that the silicon dioxide of 10.0g step (1) makes and 2.0g analytical pure sodium bicarbonate , 600W ultrasonic wave for 40 minutes to disperse evenly, under the condition of normal pressure nitrog...

Embodiment 3

[0048] (2) Add 10.0 g of surface-hydroxylated silica to 120.0 g of analytically pure toluene, disperse evenly with 800 W ultrasonic for 30 minutes, and then add 30.0 g of functional organic ligand (shown in formula I) dropwise to silica and In the mixed solution of toluene, magnetically stir the reaction at 70°C for 18h. After the reaction is completed, filter it with a Buchner funnel with filter paper, wash the obtained precipitate with analytically pure toluene five times, each time with 20mL of analytically pure toluene, and then Vacuum drying to obtain the organic ligands supported by silica;

[0049] (3) 1.2g analytical pure sodium chloroplatinate is dissolved in 40.0g analytical pure ethanol, then add the 10.0g silicon dioxide immobilized organic ligand and 3.0g analytical pure sodium bicarbonate that step (1) makes, 800W ultrasonic wave for 30 minutes to disperse evenly, under the condition of normal pressure nitrogen, stir and react at 70°C for 5 hours, stop heating an...

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Abstract

The invention belongs to the technical field of platinum-containing hydrosilylation catalyst synthesis and particularly relates to a silicon dioxide immobilized platinum-containing hydrosilylation catalyst and a preparation method and application.A functional organic ligand of the structure shown in the formula (I) is supported to surface hydroxylated silicon dioxide, and a novel ligand supported by silicon dioxide is obtained; then, complex platinum is removed by means of the novel ligand supported by silicon dioxide, and the silicon dioxide immobilized platinum-containing hydrosilylation catalyst is obtained.The catalyst is a metal organic complex catalyst supported by silicon dioxide with the hydroxylated surface and belongs to heterogeneous catalysts.The catalyst is mainly applied to hydrosilylation reaction, has high catalytic activity, and is easy to separate, capable of being repeatedly used and low in cost.The formula (I) is as shown in the description.

Description

technical field [0001] The invention belongs to the technical field of synthesis of platinum-containing hydrosilylation catalysts, and in particular relates to a silicon dioxide immobilized platinum-containing hydrosilylation catalyst, its preparation method and application. Background technique [0002] Hydrosilylation reaction refers to the addition reaction between organosilicon compounds containing silicon-hydrogen bonds and unsaturated compounds under certain conditions. It occupies an important position in the field of organosilicon chemistry and is widely used in polymer modification and catalytic hydrogenation. , asymmetric synthesis and other fields. For the hydrosilylation reaction, the selection and preparation of the catalyst is a crucial link, which directly affects the reaction efficiency. [0003] The catalysts currently used to catalyze the hydrosilylation reaction are mainly complexes of noble metals, such as platinum, rhodium, ruthenium, palladium, osmium ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07F7/08
CPCB01J31/1633B01J31/2291B01J2231/323B01J2531/0241B01J2531/828C07F7/0838C07F7/0879Y02P20/50
Inventor 胡继文魏彦龙涂园园张培杨公华胡美龙林树东陈又军姚文英郝晓鹏
Owner 国科广化(南雄)新材料研究院有限公司
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