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A method for synthesizing all-silicon micro-mesoporous composites

A mesoporous and silicon-micro technology, applied in the field of all-silicon micro-mesoporous composite materials and their synthesis, to achieve the effects of increasing production, increasing solid content, and saving raw material costs

Active Publication Date: 2017-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses Tianqing powder and activated carbon powder as templates (referred to as hard templates in the present invention) to produce mesopores, and does not involve further improving the activity of the synthesized all-silicon molecular sieve.

Method used

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  • A method for synthesizing all-silicon micro-mesoporous composites
  • A method for synthesizing all-silicon micro-mesoporous composites
  • A method for synthesizing all-silicon micro-mesoporous composites

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Experimental program
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Embodiment approach

[0027] In one embodiment, the all-silicon micro-mesoporous composite molecular sieve has an MFI structure, and the organic quaternary ammonium compound includes or is tetrapropylammonium hydroxide, tetrapropylammonium chloride, tetrapropylammonium bromide one or more of . Wherein the molar ratio of one or more of tetrapropylammonium hydroxide, tetrapropylammonium chloride, and tetrapropylammonium bromide to the silicon source is preferably not less than 0.01:1, such as 0.02 to 0.2:1 , or 0.04~0.15:1.

[0028] In one embodiment, the all-silicon micro-mesoporous composite molecular sieve has a MEL structure, and the organic quaternary ammonium compound includes or is one of tetrabutylammonium hydroxide, tetrabutylammonium bromide, and tetrabutylammonium chloride. one or more species. Wherein the molar ratio of one or more of tetrabutylammonium hydroxide, tetrabutylammonium bromide, and tetrabutylammonium chloride to the silicon source is preferably not less than 0.01:1, such a...

Embodiment 1

[0056] (1) Mix 12.1g of tetrapropylammonium hydroxide aqueous solution with a concentration of 25.05% by weight, 0.8g of tetrapropylammonium bromide solid, 20.8g of tetraethyl silicate, 2g of ethylenediamine, 13.14g of cetyltri Methyl ammonium bromide, 0.26g concentration of 20% by weight of ammonia and 120g deionized water were added to a 500ml beaker successively, put into a magnetic stirrer with heating and stirring functions, and stirred at 80°C for 4 hours. Supplement the evaporated water to obtain the organic alkali hydrolyzate of silicon; wherein the content of monohydric alcohol does not exceed 10ppm;

[0057] (2) cooling the obtained silicon organic alkali hydrolyzate to room temperature under stirring, and then standing at room temperature for 12 hours for aging to obtain an aged product;

[0058] (3) Under stirring, add 12g of white carbon black powder to the aging product, stir for 1 hour, transfer it to a closed stainless steel reaction kettle, and crystallize at ...

Embodiment 2～4

[0062] The molecular sieve was prepared according to the method of Example 1, except that the ratio and preparation conditions were adjusted, wherein the conditions of step (4) were unchanged, the preparation conditions were shown in Table 1, and the characterization results of the obtained molecular sieve were shown in Table 2. The resulting molecular sieve has an MFI structure.

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Abstract

The invention relates to a method for synthesizing an all-silicon micro-mesoporous composite material. The method for synthesizing the all-silicon micro-mesoporous composite material comprises the following steps: mixing a template agent, an organic silicon source, an inorganic ammonium source and water, ageing, uniformly mixing with a solid silicon source, crystallizing, and recycling an all-silicon micro-mesoporous composite molecular sieve, wherein the template agent is an organic quaternary ammonium compound, a long-chain alkylammonium compound and optional organic amine. The synthesized all-silicon micro-mesoporous composite material has a high defect site and has high activity when used for converting of cyclohexanone-oxime.

Description

technical field [0001] The invention relates to an all-silicon micro-mesoporous composite material and a synthesis method thereof, in particular to a method for synthesizing a micro-mesoporous composite molecular sieve by using a soft template agent. Background technique [0002] All-silicon molecular sieves such as S-1, S-2, and β molecular sieves have no exchangeable cations on their skeletons, and their adsorption capacity for water molecules is far lower than that for organic molecules. They have high hydrophobicity and can be used as membranes. Separation materials and catalytic materials can also be used as parent materials for preparing other catalytic materials. For example, the all-silicon MFI structure molecular sieve S-1 has been used as a catalyst for the rearrangement of cyclohexanone oxime to prepare caprolactam; the research on the synthesis of molecular sieves with all-silicon S-1 molecular sieve and all-silicon beta molecular sieve as the matrix is ​​also in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/02B01J20/10B01J20/30B01J29/03C07D223/10C07D201/04
CPCB01J20/103B01J20/3085B01J29/03B01J2220/4806C01B37/02C01P2002/72C01P2002/86C01P2006/14C01P2006/16C07D201/04C07D223/10
Inventor 舒兴田夏长久林民朱斌彭欣欣
Owner CHINA PETROLEUM & CHEM CORP
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