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Reactive distillation method and device for 4emd production

A technology of reactive distillation and reactive distillation column, which is applied in the field of reactive distillation methods and devices produced by 4EMD, can solve the problems such as difficulty in breaking through the reaction equilibrium for single-pass conversion rate, unsuitable for large-scale industrial applications, and complicated operation streams. , to achieve the effect of saving equipment investment, reducing energy consumption, and simple process flow

Active Publication Date: 2020-11-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation method of dioxolane is often obtained by condensation reaction cyclization of diols and corresponding aldehydes or ketones. However, the above reactions are reversible reactions, and the single-pass conversion rate is difficult to break through the limitation of reaction equilibrium.
[0003] At present, dioxolane compounds are obtained by reactive distillation, extraction and dehydration, and then refined. For example, in the patent CN96112618, alkyl-substituted benzenes such as toluene, ethylbenzene, and n-propylbenzene are used as organic extractants. , but this method will sacrifice part of the 1,3-dioxolane, the operation stream is also complicated, and the energy consumption is relatively high
In small and medium-sized applications, there is also a dehydration method to obtain 1,3-dioxolane by adsorption and dehydration of desiccants such as salt, but this method is not suitable for large-scale industrial applications

Method used

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  • Reactive distillation method and device for 4emd production
  • Reactive distillation method and device for 4emd production

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Embodiment 1

[0030] The method of the present invention is used for 1,2-butanediol acetal reaction and prepares the production process of 4EMD, as figure 1 As shown, the feed 1,2-butanediol and acetaldehyde are raw materials of considerable purity, the processing capacity of 1,2-butanediol is 45kg / hr, the amount of acetaldehyde used in the reactive distillation column and the quality of butanediol The ratio is 0.59. The total number of theoretical plates in the reactive distillation column is 22, and the 7th to 22nd stages are the reactive distillation section. The macroporous acidic cationic resin (NKC-9) is used as the catalyst. The operating pressure is 0.5atm by absolute pressure, the reflux ratio is 0.15, and the top control Extract the content of butanediol. The total number of theoretical plates of the acetaldehyde recovery tower is 20, the operating pressure is 2 atm in terms of absolute pressure, the reflux ratio is 1.7, and the purity of acetaldehyde is controlled at the top of ...

Embodiment 2

[0033] The method of the present invention is used for 1,2-butanediol acetal reaction and prepares the production process of 4EMD, as figure 1 As shown, the processing capacity of feed 1,2-butanediol is 1000kg / hr, the water content of acetaldehyde is 10w%, and the ratio of the molar amount of acetaldehyde entering the reactive distillation column to the molar amount of butanediol is maintained at 1.2. Other operating conditions are also shown in Example 1.

[0034] After the above-mentioned process, the mass purity of the product 4EMD is as high as 99.9%, and the recovery rate can reach 97.6%.

Embodiment 3

[0036] The method of the present invention is used for 1,2-butanediol acetal reaction and prepares the production process of 4EMD, as figure 2 As shown, the feed 1,2-butanediol and acetaldehyde are raw materials of considerable purity, the processing capacity of 1,2-butanediol is 200kg / hr, the amount of acetaldehyde used in the reactive distillation column and the quality of butanediol The ratio is 0.60. The total number of theoretical plates of the reactive distillation column is 30, and the 16th to 30th grades are the reactive distillation section. Strong acidic molecular sieves (macroporous acidic cationic resin NKC-9) are used as catalysts. The operating pressure is absolute pressure as normal pressure, and the reflux ratio is 16. The 15th theoretical plate of the butanediol stream is fed, and the reaction product is withdrawn from the side line at the 11th theoretical plate, and the purity of acetaldehyde is controlled at the top of the tower for recycling. The mixture ...

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Abstract

The invention relates to a reactive distillation method and device for 4EMD (4-ethyl-2-methyl-1,3-dioxolame) production. A reactive distillation tower comprises a distillation section and a reactive distillation section, wherein a 1,2-butanediol feed port is formed in the top of the reactive distillation section, acetaldehyde is fed into tower bottom, a reaction product is produced from tower top and enters an acetaldehyde recovery tower for acetaldehyde separation, a 4EMD and water mixture after acetaldehyde separation enters a distillation tower through a tower top phase splitter or one tower plate of the 4EMD distillation tower, by means of the tower top phase splitter, an organic phase flows back, an aqueous phase is produced, and a 4EMD product is obtained from the tower bottom. The method and the device have the advantages that the reaction and the separation coupling are performed in the same equipment simultaneously, so that the equipment investment can be saved, energy consumption can be reduced, the forward reaction is promoted, and a high reaction conversion rate is acquired. By means of the phase splitter arranged at the tower top, water can be removed very well, the 4EMD product with high purity is obtained, and meanwhile, the high recovery rate of the 4EMD product can be guaranteed.

Description

technical field [0001] The invention belongs to the field of chemical distillation and separation, and relates to a reactive distillation method and device for 4EMD production. Background technique [0002] Dioxolane compounds such as 1,3-dioxolane and 2-methyl-1,3-dioxolane have important applications in chemical industry, and can be used as solvents for oils and fats, extractants, and pharmaceutical intermediates Body, electrolyte solvent, solvent stabilizer, raw material of acetal resin, etc., the dioxolane compound used as a raw material of acetal resin needs to strictly control the water content therein, and trace amounts of water usually very hinder the polymerization reaction. The preparation method of dioxolane is often obtained by condensation reaction cyclization of dihydric alcohols and corresponding aldehydes or ketones. However, the above reactions are reversible reactions, and the single-pass conversion rate is difficult to break through the limitation of react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/12
CPCC07D317/12Y02P20/10
Inventor 李鑫钢高鑫黄伟进李洪丛山
Owner TIANJIN UNIV
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