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Novel supported Pt catalyst as well as preparation method and application thereof in hydrosilylation

A supported catalyst technology, which is applied in the field of hydrogen silicon addition catalyst modification, can solve the problems of complex synthesis route, raw material irritation and corrosion, inconvenient operation, etc., and achieve high product selectivity, good process safety, good The effect of applying the foreground

Active Publication Date: 2020-04-24
苏州东杏表面技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, perfluoroalkyl siloxane compounds are mainly synthesized by hydrogen silicon reaction of perfluoroalkyl ethylene and silane series compounds, such as Chinese patent CN102070662A, with full Fluoroalkylethylene iodide is used as a raw material, in the presence of a precious metal catalyst, trichlorosilane is continuously added dropwise for reaction to obtain an intermediate product; then a high boiling point solvent is added, methanol or ethanol is continuously added dropwise for reaction, and the target product is obtained by rectification under reduced pressure , its main disadvantage is that the chemical activity of perfluoroalkylethylene in the reactant is poor, and the raw material is irritating and corrosive
In addition, in order to achieve better anti-fouling and wear-resistant effects, it is necessary to prepare perfluoroalkyl siloxane compounds with longer carbon chains, but the synthesis of long-chain perfluorocarbons and their derivatives is more difficult
[0004] In comparison, long-chain perfluoropolyether is easy to obtain, but when it reacts with silane compounds, it is usually synthesized by hydrogen silicon reaction , such as the Chinese patent CN102666759A, the synthetic route adopted is more complex, first synthesize the perfluoropolyether compound, then connect the propylene group to the carbon chain, and finally connect the propylene group and the silane compound to the end of the silane under the action of a noble metal catalyst compound, and then through alcohol exchange reaction to obtain fluorine-containing polyether siloxane compound
The whole synthetic route is more complicated, and also uses irritating and corrosive reactants, which is not conducive to industrial production
[0005]In the above multiple processes, hydrogen silicon addition is a very important step. The current practice is to use Pt-containing complex catalysts for homogeneous reactions to carry out batch Operation, involving the feeding of trichlorosilane, etc., due to the irritation and corrosion of trichlorosilane, the operation is very inconvenient
At the same time, due to the use of Pt complex catalysts, the residue of the noble metal component Pt after the reaction will also cause product quality problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Configure H 2 PtCl 6 Solution 30ml, which contains 0.1g of metal platinum, weigh 10g of SiO 2 The carrier was added to the above solution, stirred at room temperature for 30 minutes, then evaporated to dryness in a water bath at 80°C, then dried in an oven at 100°C for 12 hours, and then baked in a muffle furnace at 400°C for 2 hours. Then dechlorinate, put the sample into a quartz tube and heat it at 500°C, and dechlorinate with 80°C water vapor for 6 hours by blowing air at 30mL / min. h 2 Reduction conditions, flow rate 40mL / min, reduction at 400°C for 2h. The Pt content in the catalyst is 1wt.%. Add 0.05g of perfluorodecyltrimethoxysilane to 30ml of perfluorobutyl ethyl ether to form a solution, impregnate the catalyst above for 0.5h at 20°C, use a rotary evaporator to remove the solvent, take out the catalyst in Dry at 80°C to obtain the modified catalyst, which is designated as the new supported Pt catalyst A. After the catalyst was pressed, the water contact ...

Embodiment 2

[0028] Configure H 2 PtCl 6 Solution 30ml, which contains 0.1g of metal platinum, weigh 10g of Al 2 o 3 The carrier was added to the above solution, stirred at room temperature for 30 minutes, then evaporated to dryness in a water bath at 80°C, then dried in an oven at 100°C for 12 hours, and then baked in a muffle furnace at 400°C for 2 hours. Then dechlorinate, put the sample into a quartz tube and heat it at 500°C, and dechlorinate with 80°C water vapor for 6 hours by blowing air at 30mL / min. h 2 Reduction conditions, flow rate 40mL / min, reduction at 400°C for 2h. The Pt content in the catalyst is 1wt.%. Add 0.05g of perfluorodecyltrimethoxysilane to 30ml of perfluorobutyl ethyl ether to form a solution, impregnate the catalyst above for 0.5h at 20°C, use a rotary evaporator to remove the solvent, take out the catalyst in Dry at 80°C to obtain the modified catalyst, which is designated as the new supported Pt catalyst B. After the catalyst was pressed, the water cont...

Embodiment 3

[0030] Configure H 2 PtCl 6 Solution 30ml, which contains 0.1g of metallic platinum, weighed 10g of ZSM-5 molecular sieve carrier and added to the above solution, stirred at room temperature for 30min, then evaporated to dryness in a water bath at 80°C, and then dried in an oven at 100°C for 12h. Afterwards, it was fired in a muffle furnace at 400°C for 2 hours. Then dechlorinate, put the sample into a quartz tube and heat it at 500°C, and dechlorinate with 80°C water vapor for 6 hours by blowing air at 30mL / min. h 2 Reduction conditions, flow rate 40mL / min, reduction at 400°C for 2h. The Pt content in the catalyst is 1wt.%. Add 0.05g of perfluorodecyltrimethoxysilane to 30ml of perfluorobutyl ethyl ether to form a solution, impregnate the catalyst above for 0.5h at 20°C, use a rotary evaporator to remove the solvent, take out the catalyst in Dry at 80°C to obtain the modified catalyst, which is designated as the new supported Pt catalyst C. After the catalyst was presse...

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PUM

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Abstract

The invention discloses a novel supported Pt catalyst as well as a preparation method and an application thereof in hydrosilylation, which belong to the technical field of hydrosilylation catalyst modification. The perfluoroalkyl trialkoxy silane is modified to the surface of a catalyst by an impregnation method to prepare the novel supported Pt catalyst. The preparation method is simple and easyto implement, has the advantages of accessible raw materials and low cost, and can implement large-scale industrial production. The novel supported Pt catalyst is applied to hydrogen-silicon hydrogenation, the reaction is successfully optimized from a kettle type reaction adopting a homogeneous catalyst to a continuous reaction adopting a heterogeneous catalyst, and the process safety is better; the reaction conversion rate reaches 99mol%, the product selectivity is high, and the catalyst has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of hydrogen silicon addition catalyst modification, and in particular relates to a novel supported Pt catalyst, a preparation method thereof and an application in hydrogen silicon addition. Background technique [0002] The fluorine-containing siloxane compound can react with the hydroxyl groups on the surface of the substrate to form a film with amphiphobic properties (neither lipophilic nor hydrophilic), which can prevent dirt such as moisture or oil from adhering, And it increases the surface sliding property, thereby improving the surface wear resistance. It is a surface layer with anti-fouling and wear-resistant properties. It has been widely used in lenses, mobile phones and tablet computer displays. [0003] At present, perfluoroalkylsiloxane-based compounds are mainly synthesized by hydrogen-silicon reaction of perfluoroalkylethylene and silane series compounds, such as Chinese patent CN102070662A, u...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J37/02C08G77/08
CPCB01J31/0274B01J37/0203C08G77/08B01J2231/323
Inventor 许波连何丽蓉王兴钱红梅
Owner 苏州东杏表面技术有限公司
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