Catalyst for efficient conversion of silane to silanol and its preparation and application

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 no reduction in catalytic performance Effect

Inactive Publication Date: 2017-04-05
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 gold nanoparticles, it is not easy to obtain SBA-15 loaded with gold nanoparticles

Method used

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  • Catalyst for efficient conversion of silane to silanol and its preparation and application
  • Catalyst for efficient conversion of silane to silanol and its preparation and application
  • Catalyst for efficient conversion of silane to silanol and its preparation and application

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 preparing a heterogeneous catalyst SBA-PIL-Au by loading Au nanoparticles in SBA-15 mesoporous channels, which is used to efficiently catalyze the conversion reaction of silane to silanol. In order to enhance the interaction force between the substrate and gold nanoparticles, we proposed for the first time to graft and grow an ionic liquid polymer brush: poly(1-(4-enylphenyl)-3-methylimidazolium chloride) in situ onto the pore walls of the mesoporous material SBA‑15. SBA‑PIL‑Au exhibited high conversion (>98%) and high selectivity (silanol:siloxane>99:1 in product) for a series of different kinds of silane to silanol conversion reactions. After the catalyst is recycled for 3 times, the catalytic performance does not decrease at all. In the reaction process, only water is used as solvent and oxidant, and no organic solvent is used, which is green and environmentally 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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Patent Type & Authority Patents(China)
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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