Catalyst for catalyzing efficient conversion of silane to silanol, preparation and application thereof

A technology for catalyzing silane and catalysts, which is applied in the field of preparation of new heterogeneous catalysts SBA-PIL-Au, which can solve problems such as difficulty and lack of interaction force, and achieve high loading capacity, exquisite preparation route design, and the effect of inhibiting agglomeration

Inactive Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the lack of effective interaction between organosilicon and gol

Method used

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  • Catalyst for catalyzing efficient conversion of silane to silanol, preparation and application thereof
  • Catalyst for catalyzing efficient conversion of silane to silanol, preparation and application thereof
  • Catalyst for catalyzing efficient conversion of silane to silanol, preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The first step: the synthesis of [VBMI][Cl]: 4-(chloromethyl)styrene (1.53g, 10mmol) and 1-methylimidazole (0.82g, 10mmol) were blended and reacted at 45°C under nitrogen protection 24h. After the reaction was finished, cool to room temperature, filter and wash the precipitate, and dry it in vacuum.

[0035] The second step: SBA-15 surface modification initiator CTS

[0036] SBA-15 was mixed with 17% HCl solution and refluxed for 4 hours to expose as many silicon hydroxyl groups as possible on the surface of SBA-15. The treated SBA-15 (2.0g) was mixed with CTS (1.0g), toluene (40mL) and pyridine (1.0g) and then stirred and refluxed for 16h under nitrogen protection. The product was washed successively with acetone and water, and then dried under vacuum at 100°C overnight. The surface of SBA-15 was successfully grafted with chlorine-containing ATRP initiator CTS.

[0037] Step 3: Grafting PIL on the surface of SBA-CTS

[0038] Ionic liquid polymer brushes were in si...

Embodiment 2-4

[0044] SBA-PIL-Au catalyzes the conversion reaction of triethylsilane to triethylsilanol, and the catalytic performance does not decline at all after being recycled for 3 times. According to Table 1, other preparation, reaction, and test conditions are the same as in Example 1. .

[0045] Table 1

[0046]

Embodiment 5-11

[0048] SBA-PIL-Au shows high conversion rate and high selectivity to a series of different kinds of silane to silanol conversion reactions, as described in Table 2, and other preparation, reaction and test conditions are the same as in Example 1.

[0049] Table 2

[0050]

[0051] The present invention successfully prepares SBA-15 supported Au nano particle heterogeneous catalyst SBA-PIL-Au for the first time, and uses it to catalyze the efficient conversion of silane to silanol. In order to enhance the interaction force between the substrate and the gold nanoparticles, we innovatively propose an ionic liquid polymer brush (PIL): poly(1-(4-enylphenyl)-3-methylimidazolium chloride ) in situ grafted onto the pore wall of SBA-15. SBA-PIL-Au showed high conversion and high selectivity for a series of conversion reactions of different kinds of silanes to silanols. After the catalyst is recycled for 3 times, the catalytic performance does not decrease at all, and only water is ...

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Abstract

The invention discloses a method for preparation of a heterogenous catalyst SBA-PIL-Au by loading Au nanoparticles in SBA-15 mesopore channels and application of the catalyst to reaction for efficient catalysis of silane conversion to silanol. In order to enhance the action force between a substrate and nanogold particles, the invention, for the first time, proposes in-situ graft growth of an ionic liquid polymer brush: poly(1-(4-allyl phenyl)-3-methyl imidazolium chloride) to the hole walls of a mesoporous material SBA-15. SBA-PIL-AU shows a high conversion rate (greater than 98%) and high selectivity (in the product, with the ratio of silanol to silicone being greater than 99:1) on a series of various silane-to-silanol conversion reactions. The catalytic performance of the catalyst does not decline after reuse 3 times, only water is used as the solvent and oxidant in the reaction process, and no organic solvent is used, thus being green and environment-friendly.

Description

technical field [0001] The invention relates to the preparation of a novel heterogeneous catalyst SBA-PIL-Au: the mesoporous material SBA-15 supports Au nanoparticles to catalyze the efficient conversion of silane to silanol. Background technique [0002] The selective oxidation of silane to prepare silanol is an important organic reaction, and the product silanol can be further used as raw material to synthesize organosilicon polymer. However, strong oxidants such as permanganate, ozone, and silver salts need to be used to catalyze this type of reaction. The selectivity of the reaction is not good, and a large amount of siloxane and other toxic by-products will be generated, which not only reduces economic benefits, but also causes environmental pollution. How to find a new catalyst and improve the selectivity of this reaction has become the direction of people's efforts to explore. [0003] Gold nanoparticles are a catalyst with excellent performance, but because of thei...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07F7/08
CPCY02P20/584
Inventor 高艳安冷文光王畅冯璐马丽娜
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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