Mesoporous silicon material, its synthesis method and application, and a method for oxidizing cyclic ketones

A technology for oxidizing cyclic ketones and mesoporous silicon, applied in chemical instruments and methods, inorganic chemistry, organic chemistry, etc., to achieve the effects of reducing dosage, improving synthesis efficiency, and relatively high crystallinity

Active Publication Date: 2018-02-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis efficiency and product yield of the silicon molecular sieve SBA-15 synthesized by the existing method still need to be further improved.

Method used

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  • Mesoporous silicon material, its synthesis method and application, and a method for oxidizing cyclic ketones
  • Mesoporous silicon material, its synthesis method and application, and a method for oxidizing cyclic ketones
  • Mesoporous silicon material, its synthesis method and application, and a method for oxidizing cyclic ketones

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Embodiment approach

[0047] According to a preferred embodiment of the present invention, the preferred molar ratio of cyclic ketone, oxygen-containing gas and optional solvent is 1:0.2-5:1-100, the reaction temperature is preferably 20-160°C, and the reaction pressure is preferably 0.3-2.5MPa.

[0048] In the method for oxidizing cyclic ketones provided by the present invention, said solvent is preferably selected from alcohols such as water or methanol, ethanol, n-propanol, isopropanol, tert-butanol, isobutanol or ketones such as acetone and butanone or nitriles such as acetonitrile, or carboxylic acids such as formic acid and acetic acid, or a mixture thereof, preferably acetone, water, or a mixture thereof.

[0049] In the method for oxidizing cyclic ketones provided by the present invention, the cyclic ketones are one or more of cyclohexanone, cyclopentanone and methylcyclohexanone.

[0050] The present invention will be further described below by embodiment, but content of the present inven...

Embodiment 1

[0062] First mix 50 grams of tetraethyl orthosilicate and EO 20 PO 70 EO 20 (Pluronic P123) was added to the aqueous solution of hydrochloric acid and stirred and mixed, wherein the molar ratio of tetraethyl orthosilicate, hydrochloric acid, P123 and water was 1:0.45:0.15:85, and the organosilicate was SiO 2 meter, acid source as H + After the silicon ester is hydrolyzed (the hydrolysis rate of the organic silicon source is 100%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 110°C for 12 hours. After cooling, the reactor is opened to add silica gel A to the crystallization system and mix well. , in which the molar ratio of the added silica gel to the organosilicon source is 1:0.2 in terms of silicon dioxide, and then the mixture is continuously crystallized in a sealed reaction vessel at a temperature of 150°C and autogenous pressure for 18 hours, and the obtained crystallized product Filter, wash, and dry at 110° C. for 120 minutes, an...

Embodiment 2

[0065] First, 50 grams of tetramethyl orthosilicate and surfactant P123 are added to the aqueous solution of hydrochloric acid and stirred and mixed, wherein the molar ratio of tetramethyl orthosilicate, hydrochloric acid, P123 and water is 1:0.15:0.05:25, wherein Organosilicate with SiO 2 meter, acid source as H +After the silicon ester is hydrolyzed (the hydrolysis rate of the organic silicon source is 50%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 120°C for 5 hours, and after cooling, the reactor is opened to add silica gel B to the crystallization system and mix well , wherein the silica gel added and the organosilicon source molar ratio is 1:0.1 in terms of silicon dioxide, and then the mixture is continued to crystallize in a sealed reactor at a temperature of 140°C and autogenous pressure for 17h, and the obtained crystallized product Filter, wash, and dry at 110°C for 120 minutes, and then bake at 550°C for 3 hours to obtain m...

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Abstract

The present invention relates to the field of synthesis of catalytic materials, and specifically provides a mesoporous silicon material and a synthesis method thereof, the method comprising: (1) hydrolyzing an organic silicon source, an acid source and a surfactant to obtain a mixture A, and preparing the obtained mixture A performing the first crystallization; (2) mixing the first crystallized material with an inorganic silicon source to obtain a mixture B, and performing the second crystallization on the obtained mixture B. The invention provides the mesoporous silicon material synthesized according to the method of the invention. The invention provides the application of the mesoporous silicon material of the invention in oxidation reaction. The invention provides a method for oxidizing cyclic ketones. The method for synthesizing mesoporous silicon materials provided by the present invention can use relatively cheap inorganic silicon sources such as silica gel or silica sol as part or even the main silicon source, reducing the amount of organic silicon esters and greatly improving the synthesis efficiency.

Description

technical field [0001] The invention relates to a method for synthesizing a mesoporous silicon material, the mesoporous silicon material synthesized by the method and its application in oxidation reaction, and a method for oxidizing cyclic ketones. Background technique [0002] Zhao Dongyuan and others reported the SBA-15 series of mesoporous molecular sieves and their synthesis methods for the first time (Science, 1998, 279, 548). This series of materials has uniform particle size and regular mesoporous structure, which has attracted great attention from the relevant academic circles. It brings hope for the catalysis and separation of macromolecules. Its mesoporous structure is characterized by its X-ray diffraction spectrum with diffraction peaks around 0.8°, 1.5°, and 1.7° in 2θ. However, the synthesis efficiency and product yield of the silicon molecular sieve SBA-15 synthesized by the existing method still need to be further improved. Contents of the invention [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00B01J29/03C07C409/22C07C409/20
Inventor 史春风林民龙军朱斌
Owner CHINA PETROLEUM & CHEM CORP
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