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Preparation method of 2, 2-dimethoxypropane

A technology of dimethoxypropane and methanol, which is applied in 2 fields, can solve the problems of high energy consumption cost, failure to meet the demand of intermediates, and high cost of raw materials, and achieve the effects of high safety, improved product quality, and low energy consumption

Inactive Publication Date: 2014-05-07
ZHEJIANG HUTU PHARMCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2,2-dimethoxypropane is an important intermediate, the traditional synthetic method is to use acetone and methanol as raw materials, dehydration by molecular sieve under the action of catalyst to obtain 2,2-dimethoxypropane, in this step a large amount of Molecular sieve needs to be regenerated, and the energy cost is high. In addition, the molecular sieve contains products and raw materials, resulting in high cost of raw materials, and the total reaction yield is about 85%.
Therefore, there are many problems in the process of production, which cannot meet the demand for intermediates of rapidly developing pharmaceutical products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 500 g of methanol and 275 g of acetone in a 1000 ml four-neck flask with mechanical stirring, thermometer, and condenser, stir, cool to -15°C, add 5 g of molecular sieve A4 as a catalyst, and the reaction is exothermic during the process, and salt water is required. Keep the temperature at -15°C to react, take a sample for about 3 hours to complete the reaction, the crude product content is 23%, filter, neutralize the mother liquor to extract and distill, and then rectify to obtain 172.5g of the finished product, the product purity is 99.3%, and the yield is 91%; the above The chemical reaction formula is:

[0013]

Embodiment 2

[0015] In a 2000L reactor, put methanol 900kg, acetone 500kg, stir, cool down to -25°C, add 5Kg of molecular sieve A4 as a catalyst, the reaction is exothermic during the process, need to pass brine, keep the temperature at -25°C for reaction, and take about 5 Hours of reaction is completed, filtered, the crude product content is 28%, the mother liquor is neutralized to extract and distill, and then the finished product is 364.6kg through rectification, the product purity is 99.4%, and the yield is 93%. Chemical reaction formula is the same as embodiment one.

Embodiment 3

[0017] Add 500 g of methanol and 275 g of acetone in a 1000 ml four-neck flask with mechanical stirring, a thermometer and a condenser, stir, cool to 15° C., add 5 g of sulfuric acid as a catalyst, and the reaction is exothermic during the process, and salt water is required to keep the temperature at React at 15°C, take a sample for about 2 hours to complete the reaction, the crude product content is 22.5%, filter, neutralize the mother liquor to extract and distill, and then rectify to obtain 170g of the finished product, the product purity is 99%, and the yield is 90%. Chemical reaction formula is the same as embodiment one.

[0018] Four, embodiment four

[0019] In a 2000L reactor, put 900kg of methanol and 500kg of acetone, stir, cool down to -10°C, add 5Kg of solid acid as a catalyst, the reaction is exothermic during the process, need to pass brine, keep the temperature at 25°C for reaction, and take a sample for about 1 hour to react Finished, filtered, the crude pro...

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PUM

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Abstract

The invention relates to a preparation method of 2, 2-dimethoxypropane. The method comprises the steps of adding a catalyst after mixing methanol and acetone, and reacting under a certain condition to obtain a crude product of 2, 2-dimethoxypropane; then, carrying out extractive distillation and redistillation to obtain a finished product of 2, 2-dimethoxypropane. The preparation method is simple in process, low in energy consumption and high in safety; experimental data proves that the yield can be up to over 90%, the purity of 2, 2-dimethoxypropane can be up to over 99%, and the quality of 2, 2-dimethoxypropane can be effectively improved.

Description

technical field [0001] The present invention relates to a kind of preparation method of 2,2-dimethoxypropane. Background technique [0002] 2,2-dimethoxypropane is an important intermediate, the traditional synthetic method is to use acetone and methanol as raw materials, dehydration by molecular sieve under the action of catalyst to obtain 2,2-dimethoxypropane, in this step a large amount of The molecular sieve needs to be regenerated, and the energy cost is high. In addition, the molecular sieve contains products and raw materials, resulting in high raw material costs, and the total reaction yield is about 85%. Therefore, there are many problems in the process of production, which cannot meet the demand for intermediates of the rapidly developing pharmaceutical products. Contents of the invention [0003] The purpose of this invention is to provide a kind of preparation method of 2,2-dimethoxypropane with low energy consumption, high yield and high product quali...

Claims

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Application Information

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IPC IPC(8): C07C43/303C07C41/56
CPCC07C41/56C07C43/303
Inventor 顾金林胡文江
Owner ZHEJIANG HUTU PHARMCHEM
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