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Method for preparing ketal by catalysis of ionic liquid and dehydration of acid-resistant molecular sieve membrane

A molecular sieve membrane, ionic liquid technology, applied in chemical instruments and methods, preparation of organic compounds, formation/introduction of ether groups/acetal groups/ketal groups, etc. and other problems, to achieve the effect of high degree of greening, lower production cost and low cost

Inactive Publication Date: 2012-07-18
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest problem with this method is that it uses a large amount of calcium sulfate as a water-absorbing agent, which is difficult to reuse and will produce a large amount of solid waste and pollute the environment.

Method used

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  • Method for preparing ketal by catalysis of ionic liquid and dehydration of acid-resistant molecular sieve membrane
  • Method for preparing ketal by catalysis of ionic liquid and dehydration of acid-resistant molecular sieve membrane
  • Method for preparing ketal by catalysis of ionic liquid and dehydration of acid-resistant molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 0.5 mol acetone, 1 mol methanol, 0.2 g [Pr 3 NH]][HSO 4] The acidic ionic liquid is mixed and added to the reaction tank 1, and the stirring reaction is started at 0°C; the metering pump 2 is started, and the reaction mixture is pumped into the preheater 3, and after the feed liquid is heated to 70°C, it enters the acid-resistant molecular sieve membrane module 5 for further Permeation separation, the permeated steam enters the cold trap 7 driven by negative pressure, and is quickly condensed and collected by liquid nitrogen, and the retained liquid is cooled by the condenser 6, and then returns to the reaction tank 1 to continue to participate in the reaction; after 2 hours of continuous operation of the membrane pervaporation device , the reaction ends, and the reaction mixture in the reaction tank 1 is statically separated. Since the product ketal is insoluble in [Pr 3 NH][HSO 4 ] in acidic ionic liquids, while acetone and methanol are soluble in [Pr 3 NH][HSO 4...

Embodiment 2

[0030] 0.5 mol acetone, 1 mol ethanol, 0.3 g [Et 3 NH]][HSO 4 ] The acidic ionic liquid is mixed and added to the reaction tank 1, and the stirring reaction is started at 0°C; the metering pump 2 is started, and the reaction mixture is pumped into the preheater 3, and after the feed liquid is heated to 70°C, it enters the acid-resistant molecular sieve membrane module 5 for further Permeation separation, the permeated steam enters the cold trap 7 driven by negative pressure, and is quickly condensed and collected by liquid nitrogen, and the retentate is cooled by the condenser 6, and then returned to the reaction tank 1 to continue to participate in the reaction; after the membrane pervaporation device has been continuously operated for 1.5 hours , the reaction ends, and the reaction mixture in the reaction tank 1 is statically separated. Since the product ketal is insoluble in [Et 3 NH][HSO 4 ] in acidic ionic liquids, while acetone and ethanol can be dissolved in [Et 3 N...

Embodiment 3

[0032] 0.5 mol acetone, 1 mol propanol, 0.5 g [Bu 3 NH][HSO 4 ] The acidic ionic liquid is mixed and added to the reaction tank 1, and the stirring reaction is started at 0°C; the metering pump 2 is started, and the reaction mixture is pumped into the preheater 3, and after the feed liquid is heated to 70°C, it enters the acid-resistant molecular sieve membrane module 5 for further Permeation separation, the permeated steam enters the cold trap 7 driven by negative pressure, and is quickly condensed and collected by liquid nitrogen, and the retentate is cooled by the condenser 6, and then returned to the reaction tank 1 to continue to participate in the reaction; after the membrane pervaporation device has been continuously operated for 1.5 hours , the reaction ends, and the reaction mixture in the reaction tank 1 is statically separated. Since the product ketal is insoluble in [Bu 3 NH][HSO 4 ] in acidic ionic liquids, while acetone and propanol can be dissolved in [Bu 3 ...

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Abstract

The invention provides a method for preparing ketal by catalysis of an ionic liquid and dehydration of an acid-resistant molecular sieve membrane. According to the method, alcohol and ketone are used as initial raw materials, the acidic ionic liquid is used as a catalyst, water generated by reaction is removed in situ by adopting an acid-resistant molecular sieve membrane pervaporation device, and ketal with high selectivity and high yield is finally obtained. The method integrates the catalysis of the ionic liquid and the dehydration of the acid-resistant molecular sieve membrane, realizes separation while reacting, has the advantages of mild reaction conditions, high reaction selectivity, high product yield and the like; and in the method, waste acid or waste water is not discharged. Thus, the method is an environment-friendly high-efficiency new method for synthesizing ketal.

Description

technical field [0001] The present invention relates to a kind of preparation method of ketal. In particular, it involves taking alcohol and ketone as starting materials, using acidic ionic liquid as a catalyst to carry out condensation reaction, and using acid-resistant molecular sieve membrane to remove the water generated by the reaction in situ, and finally prepare ketal, which belongs to the field of chemical materials and its preparation technology . Background technique [0002] Ketals are an important class of fine chemical intermediates developed in the past ten years, and are widely used in the perfume and pharmaceutical industries. For example, 2,2-dimethoxypropane, 2,2-diethoxypropane is a key intermediate in the synthesis of fragrances and pharmaceutical intermediates 2-methoxypropene, ionone, linalool, vitamin A, etc.; Hexanone diisopropanol is an important intermediate in the synthesis of broad-spectrum antibiotic clarithromycin. In addition, ketals are als...

Claims

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Application Information

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IPC IPC(8): C07B41/04C07C41/56C07D325/00
Inventor 陈祥树陶端健张小亮卢章辉杨振李章敏
Owner JIANGXI NORMAL UNIV
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