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Technology of direct production of 1,2,3-trimethoxybenzene from gallic acid

A technology of trimethoxybenzene and gallic acid, applied in the direction of organic chemistry, ether preparation, etc., can solve the problems of limited price resources, uneconomical economy, incompatibility with energy saving and emission reduction, etc., to save resources, reduce production costs, and be strong and practical. Value and effect of market application prospects

Active Publication Date: 2019-01-18
湖南棓雅生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing production process of 1,2,3-trimethoxybenzene mainly uses pyrogallic acid as raw material, which is obtained through methylation. Due to the high price of pyrogallic acid itself and limited resources, pyrogallic acid is used as the raw material. Using acid as raw material to synthesize 1,2,3-trimethoxybenzene is not only economically uneconomical, but also does not conform to my country's current energy-saving and emission-reduction policies

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0013] In a 2000L reaction tank, add 325 kg of gallic acid monohydrate, heat the temperature with heat transfer oil at 222°C, and carry out the decarboxylation reaction for 33 minutes. Observe that there are no bubbles on the liquid surface, indicating that the decarboxylation is complete; put the decarboxylation liquid into the reaction tank Cool down to 38 degrees, add catalyzer tetrabutylammonium bromide 2kg, carry out three methylation, one methylation is: dropwise add 200 liters of dimethyl sulfate and 200 liters of liquid caustic soda with a mass fraction of 33%, and the pH value is controlled at 8-8.5, the temperature is controlled at 40-45°C, the ph value remains unchanged and the temperature is kept for 9 minutes; Control at 60-65°C, keep the ph value unchanged for 9 minutes; the third methylation is: drop 50 liters of dimethyl sulfate and 70 liters of liquid caustic soda with a mass fraction of 33%, and control the ph value at 9.5-10. The temperature is controlled at...

Embodiment 2

[0015] In a 2000L reaction tank, pour 325kg of gallic acid monohydrate, heat the temperature with heat transfer oil at 237°C, and carry out the decarboxylation reaction for 47 minutes. Observe that there are no bubbles on the liquid surface, indicating that the decarboxylation is complete; put the decarboxylation liquid into the reaction tank Cool down to 42 degrees, add catalyzer tetrabutylammonium bromide 2kg, carry out three methylation, one methylation is: dropwise add 200 liters of dimethyl sulfate and 200 liters of liquid caustic soda with a mass fraction of 34%, and the pH value is controlled at 8-8.5, the temperature is controlled at 40-45°C, the ph value remains unchanged and the temperature is kept for 11 minutes; Control at 60-65°C, keep the ph value unchanged for 11 minutes; the third methylation is: drop 50 liters of dimethyl sulfate and 70 liters of liquid caustic soda with a mass fraction of 34%, and control the ph value at 9.5-10. The temperature is controlled ...

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Abstract

The invention discloses a process technology for producing 1,2,3-trimethoxybenzene directly from gallic acid. According to the process technology, 325 kg of gallic acid monohydrate is put in a 2,000-L reaction tank, conduction oil is used for heating, the temperature is controlled at 220-240 DEG C, a decarboxylation reaction is conducted for 30-35 minutes, and decarboxylation is completed when it is observed that no bubble is generated on the liquid level; decarboxylation liquid is put in a reaction tank, the temperature is dropped to 35-45 DEG C, 2 kg of the catalyst tetrabutylammonium bromide is added, 5 kg of activated carbon is added after methylation is conducted three times, filter-pressing is conducted after the temperature is kept for 20-40 min, and 1,2,3-trimethoxybenzene is obtained. By means of the process technology, resources are effectively saved, the yield of primary products is raised, production cost is lowered, the market competitiveness of the products is improved, economic benefits are increased, and high practical value and market application prospects are achieved.

Description

technical field [0001] The invention relates to a technology for directly producing 1,2,3-trimethoxybenzene from gallic acid. Background technique [0002] 1,2,3-Trimethoxybenzene (TMB) is a high value-added fine chemical product, which is widely used in medicine and pesticides, and can be used to synthesize trimethoxybenzazine (commonly known as Xinkangning) and Calcium ion antagonist lomerizine, and coronary artery vasodilator trimetazidine hydrochloride, etc. [0003] The existing production process of 1,2,3-trimethoxybenzene mainly uses pyrogallic acid as raw material, which is obtained through methylation. Due to the high price of pyrogallic acid itself and limited resources, pyrogallic acid is used as the raw material. Using acid as raw material to synthesize 1,2,3-trimethoxybenzene is not only economically uneconomical, but also not in line with my country's current energy-saving and emission-reduction policies. Contents of the invention [0004] In order to solve ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/01C07C43/205
CPCC07C41/01C07C43/2055
Inventor 王有朝
Owner 湖南棓雅生物科技有限公司
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