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Water resistant catalyst for aldol condensation as well as preparation method and application thereof

A technology of aldol condensation and water resistance, which is applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of unavoidable water and insufficient effects, and achieve enhanced physical and mechanical properties. The method is simple and the effect of prolonging the service life

Active Publication Date: 2014-02-05
HAO HUA CHENGDU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the applicant has found that the presence of water is unavoidable due to the aldol condensation reaction, although existing studies have proposed adding a small amount of ZrO to the carrier 2 It can improve the water resistance of the catalyst, but its effect is still not obvious enough. The single service life of the aldol condensation catalyst of formaldehyde and methyl propionate is about 100h or less

Method used

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  • Water resistant catalyst for aldol condensation as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0039] Example 1 Preparation of Water-resistant Catalyst MAC-02

[0040] Weigh 29.1g of cesium acetate and dissolve it in deionized water to make solution a with a concentration of 82% by mass; weigh 3.2g of AgNO 3 , add deionized water to dissolve, and make a solution b with a concentration of 62% by mass; weigh hydrophobic nano-SiO 2 85.2g, kaolin 14.1g, ZrO 2 2.0g, after mixing evenly, add the solution prepared in steps a and b, knead for 6 hours, extrude or roll ball, dry at 100°C for 3 hours, and roast at 500°C for 4 hours to obtain the catalyst, which is designated as MAC-02.

Embodiment 2

[0041] Example 2 Preparation of water-resistant catalyst MAC-03

[0042] Weigh 29.0g of cesium acetate and dissolve it in deionized water to make a solution a with a mass percentage concentration of 73%; weigh 3.2g AgNO3 and add deionized water to dissolve it to make a solution b with a mass percentage concentration of 56%; Propyltriethoxysilane was dispersed in 400g 2% trimethylethylammonium hydroxide aqueous solution by high-speed stirring, and the stirring time was 6h to form a mixed solution c; weigh nano-SiO 2 82.1g, kaolin 14.0g, ZrO 2 2.0g, after mixing evenly, add the solution prepared in steps a and b and knead for 6 hours; add the above mixed solution c, mix thoroughly at 60°C for 12 hours, evaporate water at the same time, extrude or roll, and dry at 100°C After 3 hours, it was calcined at 500°C for 4 hours to obtain a catalyst, which was designated as MAC-03.

Embodiment 3

[0043] Example 3 Preparation of Water-resistant Catalyst MAC-04

[0044] Weigh 29.0g of cesium acetate and dissolve it in ethanol to make a solution a with a concentration of 12% by mass; disperse 11g of chloropropyltriethoxysilane in 367g of 2% trimethylethylammonium hydroxide aqueous solution by high-speed stirring , stirring for 6 hours to form a mixed solution b; take 310ml of ethyl orthosilicate, slowly add it dropwise to absolute ethanol, add glacial acetic acid while stirring, and form a colloidal solution after stirring vigorously for a period of time, then slowly add 14.1g under stirring Kaolin, 2.0gZrO 2 and 3.2gAgNO 3 , add deionized water until a gel is formed. Then the gel was dried at constant temperature at 80°C for 10 hours, the dried crystals were calcined at 400°C for 10 hours, and ground to 30 mesh to 50 mesh to obtain the carrier precursor; Fully mixed at 120°C for 12 hours while evaporating water, extruded or ball-rolled; dried at 120°C for 2 hours, a...

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Abstract

The invention discloses a water resistant catalyst for aldol condensation. The water resistant catalyst comprises a main active ingredient, an active agent and a carrier, wherein the main active ingredient is one or more selected from oxides or salts of Cs; the active agent is one or more selected from oxides or salts of Sb, Nb, Ag, Al and Zr; the carrier comprises SiO2 and a carrier aid; the carrier aid is one or more selected from Al2O3, ZrO2, diatomite and kaolin; the SiO2 is hydrophobic nano SiO2; or (2) the catalyst is subjected to water-resistant treatment. The water resistant catalyst is used for aldol condensation, has the characteristics of high activity, high selectivity and long service life, is especially used for synthesizing methyl methacrylate through formaldehyde and methyl propionate. With calculation of methyl propionate, the selectivity of methyl methacrylate is 94 percent, and the single service life of the catalyst is over 400 hours. The catalyst is simple in preparation method and is suitable for industrial application.

Description

technical field [0001] The invention relates to a catalyst, especially a water-resistant catalyst for aldol condensation, especially the aldol condensation of formaldehyde and methyl propionate, as well as its preparation method and application. Background technique [0002] The aldol condensation reaction is an important reaction in organic chemistry, which is used to form C-C bonds to increase molecular chains, and its products can be undehydrated product hydroxy aldehydes, or dehydrated products Unsaturated aldehydes, if in the gas phase Reaction, because the reaction temperature is higher, what usually obtain is the dehydration product unsaturated aldehyde. [0003] The catalysts usually used for aldol condensation reaction can be alkali metal or alkaline earth metal hydroxides, oxides, soluble salts, etc. loaded on an inert carrier, such as inert particles such as alumina in Chinese patent CN01809710.3 , Silica is used as a carrier to support basic metal compounds for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/66B01J23/18B01J23/20B01J23/68C07C67/343C07C69/54
Inventor 赖崇伟李洁熊国焱李军应理
Owner HAO HUA CHENGDU TECH
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