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Solid acid catalyst for preparing acetal/ketal, and preparation method and application thereof

A solid acid catalyst and solid acid technology, applied in the direction of physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, chemical instruments and methods, etc., can solve problems such as industrial wastes and complex processes, and achieve high Selective, low dosage effect

Active Publication Date: 2019-09-13
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a green method for preparing acetal / ketone, which solves the problems in the prior art methods such as the need to add a large amount of water-absorbing agent, the process is complicated, and a large amount of industrial wastes are produced.

Method used

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  • Solid acid catalyst for preparing acetal/ketal, and preparation method and application thereof
  • Solid acid catalyst for preparing acetal/ketal, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 2.5 g of a modified cyclodextrin-supported mesylate-based solid acid catalyst into the reaction kettle (in the catalyst, the mass ratio of the modified cyclodextrin to the solid acid is 1:1), and pre-cool to -50°C. Mix 0.5 moles of acetone and 2.0 moles of methanol in a mixing tank, then cool down to -50°C, add them into the reaction kettle, and stir and react at -50°C for 4 hours. After the reaction was completed, the reaction solution was obtained by filtration and separation. The reaction liquid is subjected to rectification, and methanol and acetone are firstly separated to obtain methanol and acetone, which are returned to the raw material mixing tank and used mechanically; and then the product 2,2-dimethoxypropane is obtained by rectification and dehydration. The one-way acetone conversion rate is 85%, the product selectivity is 98.5%, and the GC content is 97%.

Embodiment 2

[0047] Add 3.0 g of a modified cyclodextrin-supported mesylate-based solid acid catalyst into the reaction kettle (in the catalyst, the mass ratio of the modified cyclodextrin to the solid acid is 1:1.5), and pre-cool to -50°C. Mix 0.5 moles of acetone and 2.0 moles of ethanol in a mixing tank, then cool down to -50°C, add them into the reaction kettle, and stir and react at -50°C for 4 hours. After the reaction was completed, the reaction solution was obtained by filtration and separation. The reaction liquid is subjected to rectification, and ethanol and acetone are firstly separated to obtain ethanol and acetone, which are returned to the raw material mixing tank and used mechanically; and then the product 2,2-diethoxypropane is obtained by rectification and dehydration. The one-way acetone conversion rate is 87%, the product selectivity is 99.0%, and the GC content is 97%.

Embodiment 3

[0049] Add 2.5 g of a modified cyclodextrin-supported mesylate-based solid acid catalyst into the reaction kettle (in the catalyst, the mass ratio of the modified cyclodextrin to the solid acid is 1:0.5), and pre-cool to -30°C. Mix 0.5 moles of acetone and 1.0 moles of methanol in a mixing tank, then cool down to -30°C, add them into the reaction kettle, and stir and react at -30°C for 2 hours. After the reaction was completed, the reaction solution was obtained by filtration and separation. The reaction liquid is subjected to rectification, and methanol and acetone are firstly separated to obtain methanol and acetone, which are returned to the raw material mixing tank and used mechanically; and then the product 2,2-dimethoxypropane is obtained by rectification and dehydration. The one-way acetone conversion rate is 63%, the product selectivity is 97.6%, and the GC content is 97%.

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Abstract

The invention relates to a modified cyclodextrin-supported solid acid catalyst and application of the catalyst in the preparation of acetal / ketal. Modified cyclodextrin is polyethyleneimine modified carboxymethyl-beta-cyclodextrin; solid acid is selected from the group consisting of SO4<2-> / ZrO2, CH3COO<-> / ZrO2 and CH3SO3<-> / ZrO2; and in the catalyst, a mass ratio of the modified cyclodextrin to the solid acid is 1: (0.1-10). A preparation method for acetal / ketal comprises a step of subjecting starting raw materials consisting of aldehyde / ketone and alcohol to a condensation reaction under theaction of a catalyst. The preparation method has the characteristics of high selectivity and indiscriminate reusability of unreacted raw materials and the unreacted catalyst. According to the invention, no other water absorbing agent is added, no other solvent is used, almost no by-product is produced, and high selectivity is realized; so the method is an environmentally-friendly novel method forsynthesizing acetal and ketal.

Description

technical field [0001] The invention relates to a solid acid catalyst for preparing acetal / ketone and its preparation method and application, specifically a modified cyclodextrin-supported solid acid catalyst for preparing acetal / ketone and its preparation method Applications in acetal / ketone. Background technique [0002] Acetal and ketal are a common means of protecting carbonyl groups in organic synthesis; at the same time, they are also intermediates in the synthesis of many important compounds, such as 2,2-dimethoxypropane, which is widely used in the synthesis of perfumes and pharmaceutical intermediates 2 -Methoxypropene, linalool, isophytol, vitamin A and β-carotene and other compounds. The reaction of alcohol and aldehyde or ketone to prepare acetal or ketal under acidic catalyst is a forward exothermic reversible reaction, and at room temperature or higher temperature, the equilibrium of the reaction strongly shifts to the reverse direction. [0003] In the exist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38C07C41/56C07C43/303
CPCB01J31/38C07C41/56C07C43/303
Inventor 杨宗龙张涛吕英东林龙刘英瑞郭劲资张旭程晓波王延斌朱龙龙李莉宋军伟翟文超黎源
Owner WANHUA CHEM GRP CO LTD
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