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Esterification production technology of methyl acetoacetate

A technology for the production of methyl acetoacetate, applied in the preparation of carboxylic acid esters, organic chemistry, chemical instruments and methods, etc., can solve the problems of difficult control of reaction temperature, long reaction time, low conversion rate, etc., and achieve the goal of eliminating overheating Phenomenon, high synthesis rate, effect of increasing reaction temperature and pressure

Inactive Publication Date: 2018-09-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the shortcomings of long reaction time, low production capacity, low conversion rate and difficult control of reaction temperature in the one-pot reaction in the prior art, and provide a continuous production of methyl acetoacetate esterification reaction process

Method used

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  • Esterification production technology of methyl acetoacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Accurately add 29.2kg (36.804L) of methanol and 244g of triethylamine into the melting pot, and start the stirring pump. Open the feeding valve and send the mixed material in the melting tank to the high liquid level tank.

[0036] 2. Add 6.1g of p-toluenesulfonic acid into the high liquid level tank, mix well and send it into the mixer; 140 900m capillary tubes are used in the mixer.

[0037] 3. Accurately batch 64.956L diketene, open the feeding valve, send diketene into the mixer, and mix thoroughly.

[0038] 4. Turn on the circulating pump, and adjust the temperature of the constant temperature water in the spiral-wound microchannel reactor to 85°C. The mixture in the mixer was sent to a spiral-wound tube microchannel reactor for esterification reaction, and was retained for 10 min at a pressure of 3 MPa in the tube.

[0039] 5. After the reaction, put the material into the cooling kettle, open the brine to cool down to 40°C, and cool for 1 hour.

[0040] 6. S...

Embodiment 2

[0042] 1. Accurately add 73.608L of methanol and 488g of triethylamine into the melting pot, and start the stirring pump. Open the feeding valve and send the mixed material in the melting tank to the high liquid level tank.

[0043] 2. Add 12.2g of p-toluenesulfonic acid into the high liquid level tank, mix well and send it into the mixer; 160 900m capillary tubes are used in the mixer.

[0044] 3. Accurately batch 129.912L diketene, open the feeding valve, send diketene into the mixer, and mix thoroughly.

[0045] 4. Turn on the circulating pump, and adjust the temperature of the constant temperature water in the spiral-wound microchannel reactor to 80°C. The mixture in the mixer was sent to a spiral-wound tube microchannel reactor for esterification reaction, and was retained for 60 min at a pressure of 3 MPa in the tube.

[0046] 5. After the reaction, put the material into the cooling kettle, open the brine to cool down to 45°C, and cool for 4 hours.

[0047] 6. Send th...

Embodiment 3

[0049] 1. Accurately add 18.402L of methanol and 122g of triethylamine into the melting pot, and start the stirring pump. Open the feeding valve and send the mixed material in the melting tank to the high liquid level tank.

[0050] 2. Add 3.05g of p-toluenesulfonic acid into the high liquid level tank, mix well and send it into the mixer; 140 600m capillary tubes are used in the mixer.

[0051] 3. Accurately batch 32.478L diketene, open the feeding valve, send diketene into the mixer, and mix thoroughly.

[0052]4. Turn on the circulation pump, and adjust the temperature of the constant temperature water in the spiral-wound microchannel reactor to 100°C. The mixture in the mixer was sent to a spiral-wound tube microchannel reactor for esterification reaction, and was kept for 5 minutes under the pressure of 3 MPa in the tube.

[0053] 5. After the reaction, put the material into the cooling kettle, open the brine to cool down to 0°C, and cool for 30 minutes.

[0054] 6. Se...

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Abstract

The invention relates to an esterification reaction technology of methyl acetoacetate. The esterification reaction technology specifically comprises the following steps of adding methyl alcohol and triethylamine into a material melting kettle, and pumping a mixture into a high-liquid level tank; dripping a catalyst, fully mixing, and pumping into a mixer; pumping diketene into the mixer, fully mixing, performing esterification reaction on the mixture through a spiral winding pipe microchannel reactor, pumping into a cooling kettle to cool after reaction, and pumping into a rectification tower;rectifying, so as to obtain the methyl acetoacetate. The esterification reaction technology has the advantages that the continuity of production operation is realized, the stability in reaction is high, the problem of temperature rise due to failure to accurately control temperature by the control reactor is prevented, and the possibility of potential reactor explosion is troubleshot; the high flux, high heat transfer ability, high synthesizing rate and low processing cost of esterification reaction are realized, and the enterprise economic benefit is obviously increased.

Description

technical field [0001] The invention relates to a production process of methyl acetoacetate esterification. Background technique [0002] Methyl acetoacetate is the fungicide hymexazol / pymethimol / pyrimethol, the insecticide diazinon / masiaphos / pyrimidinox, the herbicide imazethapyr, rodenticide, coumatetate, and warfarin Intermediates of other substances. It can be used as a component of mixed solvents of cellulose ether esters, and can also be used in organic synthesis such as pesticides, medicines, dyes, pigments, and molecular stabilizers. [0003] In the prior art, diketene and methanol are used to generate methyl acetoacetate. In order to speed up the reaction, a catalyst needs to be added. However, the traditional method is to use concentrated sulfuric acid as a catalyst, but the use of concentrated sulfuric acid as a catalyst will corrode the equipment greatly, which is not conducive to long-term production, and the content and purity of methyl acetoacetate cannot be...

Claims

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Application Information

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IPC IPC(8): C07C67/46C07C67/54C07C69/72B01J19/00
CPCB01J19/0093C07C67/46C07C67/54B01J2219/00795B01J2219/00873C07C69/72
Inventor 凌祥周辉汤显王子来
Owner NANJING UNIV OF TECH
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