Membrane dryer, intermittent esterification reaction system and dimethyl adipate preparation method

A technology of esterification reaction and dryer, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., can solve problems affecting the conversion rate of adipic acid, etc., and achieve the effect of broad market prospects

Pending Publication Date: 2022-03-11
岳阳职业技术学院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the embodiments of the present invention is to provide a membrane dryer to solve the problem that the moisture generated in the esterification process

Method used

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  • Membrane dryer, intermittent esterification reaction system and dimethyl adipate preparation method
  • Membrane dryer, intermittent esterification reaction system and dimethyl adipate preparation method
  • Membrane dryer, intermittent esterification reaction system and dimethyl adipate preparation method

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preparation example Construction

[0053] Such as figure 2 As shown, further, an embodiment of the present invention also provides a kind of dimethyl adipate preparation method, adopts above-mentioned intermittent esterification reaction system, described dimethyl adipate preparation method ( figure 2 Arrow in the schematically represents the flow chart of described dimethyl adipate preparation side) specifically comprises the following steps: add methanol and catalyst in reaction kettle 1, add oxalic acid after heating and carry out esterification reaction, simultaneously pass through preliminary The heater 3 heats the mixture of methanol vapor and water vapor produced during the esterification reaction, and then transports it to the membrane dryer 4 to remove the water in the mixture of methanol vapor and water vapor produced during the esterification reaction. Steam to obtain dry methanol vapor, and then condense the methanol vapor through the condenser 5, so as to transport the methanol vapor to the react...

Embodiment 1

[0058] Using the above-mentioned intermittent esterification reaction system, a 2000L enamel kettle was used as the reaction kettle 1. After cleaning and drying with methanol, 250kg of methanol and 25kg of catalyst were added. Turn on stirring and heat the kettle with steam. When the temperature in the kettle is 60°C, add 250kg of adipic acid from the manhole. Turn on the vacuum pump 11 and turn on the reflux pump 10, and control the temperature of the reflux methanol between 30-35°C. After the adipic acid is completely dissolved, increase the steam pressure to keep the temperature in the kettle at about 80°C. By adjusting the kettle temperature and the temperature of the preheater 3, the reflux methanol flow through the membrane dryer 4 is controlled. Monitor 1h, 2h, 4h, 6h, 9h, 14h, 18h, 22h in the reflux methanol water content and the acid value of the solution in the kettle. The water content in the methanol is detected by gas chromatography, and the acid value of the s...

Embodiment 2

[0063]Using the above-mentioned intermittent esterification reaction system, a 2000L enamel kettle was used as the reaction kettle 1. After cleaning and drying with methanol, 250kg of methanol and 25kg of catalyst were added. Turn on stirring and heat the kettle with steam. When the temperature in the kettle is 60°C, add 250kg of adipic acid from the manhole. Turn on the vacuum pump 11 and turn on the reflux pump 10, and control the temperature of the reflux methanol between 30-35°C. After the adipic acid is completely dissolved, increase the steam pressure to keep the temperature in the kettle at about 100°C. By adjusting the kettle temperature and the temperature of the preheater 3, the reflux methanol flow through the membrane dryer 4 is controlled. Monitor 1h, 2h, 4h, 6h, 9h, 14h, 18h, 22h in the reflux methanol water content and the acid value of the solution in the kettle. The water content in the methanol is detected by gas chromatography, and the acid value of the s...

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Abstract

The invention relates to the field of chemical engineering, and particularly discloses a membrane dryer, an intermittent esterification reaction system and a dimethyl adipate preparation method.The membrane dryer comprises a shell and a first cavity, a ceramic membrane tube is arranged in the first cavity, a second cavity is formed in the ceramic membrane tube, a second steam inlet is formed in the outer side of the shell, and a second steam outlet is formed in the outer side of the shell; the ceramic membrane tube is used for conveying a gaseous material to be dried to the first cavity, so that only water molecules are conveyed to the second cavity under the filtration of the ceramic membrane tube; a negative pressure environment is provided for the second cavity, a to-be-dried gaseous material is conveyed into the first cavity through a second steam inlet, only water molecules in the to-be-dried gaseous material are conveyed into the second cavity through filtration of the ceramic membrane tube under the driving of negative pressure power, and then the to-be-dried gaseous material is conveyed out of the membrane dryer. The method can be used for continuing to participate in dimethyl adipate synthesis reaction, and solves the problem that the conversion rate of adipic acid is influenced by water generated in the esterification process in the existing dimethyl adipate production method.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a membrane dryer, a batch esterification reaction system and a method for preparing dimethyl adipate. Background technique [0002] Dimethyl adipate (Dimethyl adipate, DMA), also known as dimethyl adipate and dimethyl fatty acid, is a colorless and transparent liquid, insoluble in water, soluble in alcohol and ether, and is mainly used in industry It is used as a raw material for synthesizing intermediates, medicines, and spices, as well as a plasticizer and a high-boiling solvent. [0003] Currently on the market, in the production of dimethyl adipate, the traditional method is to produce through continuous esterification, for example, using adipic acid and methanol as raw materials, using sulfuric acid as an esterification catalyst to complete, or, By adding methanol and a strong acid resin catalyst into the reaction kettle, adding solid adipic acid after the temperature of th...

Claims

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Application Information

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IPC IPC(8): B01J8/10B01J8/08B01J8/00B01D53/26B01D53/22C07C67/08C07C69/44
CPCB01J8/10B01J8/085B01J8/009B01D53/268B01D53/22C07C67/08B01D2053/223C07C69/44
Inventor 余珺
Owner 岳阳职业技术学院
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