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A method and device for improving the synthesizing of 3,4-methylenedioxy mandelic acid through emulsification

A technology of methylenedioxybenzene and glycolic acid, applied in the field of chemical engineering, can solve the problems of insufficient reaction, low mass transfer efficiency, poor fluidity and the like, achieve simple and easy product separation process, and improve product purity and yield , the effect of improving the conversion rate and yield

Active Publication Date: 2020-03-06
山东天大泰泽环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to the high viscosity of the product 3,4-methylenedioxymandelic acid, the fluidity during the synthesis process is poor, the mass transfer efficiency is not high, and the piperonine and glyoxylic acid are immiscible, the two The contact area between the phases is small, so the reaction is insufficient, resulting in low yield, poor heat transfer effect, poor selectivity of reaction and many by-products.

Method used

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  • A method and device for improving the synthesizing of 3,4-methylenedioxy mandelic acid through emulsification
  • A method and device for improving the synthesizing of 3,4-methylenedioxy mandelic acid through emulsification
  • A method and device for improving the synthesizing of 3,4-methylenedioxy mandelic acid through emulsification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] A method for improving emulsification synthesis of 3,4-methylenedioxymandelic acid, carried out according to the following steps:

[0065] S1, the mixture of 10g of water and 160g of 50wt% glyoxylic acid aqueous solution was stirred at a constant temperature, the temperature of the constant temperature stirring was -25°C, and the stirring rate was 400rpm;

[0066] S2, after starting to stir, add 98wt% concentrated sulfuric acid dropwise to the mixture at a rate of 7g / min per minute, add 140g of the total amount of 98wt% concentrated sulfuric acid dropwise, the stirring temperature is -25°C, and the stirring rate is 400rpm;

[0067] S3, when all the 98wt% concentrated sulfuric acid is added dropwise, continue to stir for 30min, and the stirring temperature is -25°C;

[0068] S4, add 3,4-methylenedioxymandelic acid to the solution after S3, and add 4 g of 3,4-methylenedioxymandelic acid;

[0069] S5, the solution after S4 is emulsified, the emulsification speed is 12Kr / m...

Embodiment 2

[0076] A method for improving emulsification synthesis of 3,4-methylenedioxymandelic acid, carried out according to the following steps:

[0077] S1, the mixture of 10g of water and 160g of 50wt% glyoxylic acid aqueous solution was stirred at a constant temperature, the temperature of the constant temperature stirring was -25°C, and the stirring rate was 400rpm;

[0078] S2, after starting to stir, add 98wt% concentrated sulfuric acid dropwise to the mixture at a rate of 7g / min per minute, add 140g of the total amount of 98wt% concentrated sulfuric acid dropwise, the stirring temperature is -25°C, and the stirring rate is 400rpm;

[0079] S3, when all the 98wt% concentrated sulfuric acid is added dropwise, continue to stir for 30min, and the stirring temperature is -25°C;

[0080] S4, add 3,4-methylenedioxymandelic acid to the solution after S3, and add 4 g of 3,4-methylenedioxymandelic acid;

[0081] S5, the solution after S4 is emulsified, the emulsification speed is 12Kr / m...

Embodiment 3

[0088] A method for improving emulsification synthesis of 3,4-methylenedioxymandelic acid, carried out according to the following steps:

[0089] S1, the mixture of 10g of water and 160g of 50wt% glyoxylic acid aqueous solution was stirred at a constant temperature, the temperature of the constant temperature stirring was -25°C, and the stirring rate was 400rpm;

[0090] S2, after starting to stir, add 98wt% concentrated sulfuric acid dropwise to the mixture at a rate of 7g / min per minute, add 140g of the total amount of 98wt% concentrated sulfuric acid dropwise, the stirring temperature is -25°C, and the stirring rate is 400rpm;

[0091] S3, when all the 98wt% concentrated sulfuric acid is added dropwise, continue to stir for 30min, and the stirring temperature is -25°C;

[0092] S4, add 3,4-methylenedioxymandelic acid to the solution after S3, and add 4 g of 3,4-methylenedioxymandelic acid;

[0093] S5, the solution after S4 is emulsified, the emulsification speed is 12Kr / m...

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Abstract

The invention provides a method and device for improving the synthesizing of 3,4-methylenedioxy mandelic acid through emulsification. Based on the principle that 3,4-methylenedioxy mandelic acid has both lipophilic and hydrophilic groups, the method takes a resultant as an emulsifying agent so as to make the separating of a product simpler and easier; a water reducing agent is added during reaction and can be directionally adsorbed on the surfaces of oil phase droplets, so that the surfaces of the oil phase droplets can carry charges, electrostatic repulsion can be generated, and therefore, the dispersing effect of the water reducing agent can be achieved, the oil phase can be dispersed, and flowability can be increased; through the lubricating function of the water reducing agent, friction can be reduced by increasing the hydrophilic groups to form solvated water films, so that a 1,3-benzodioxole phase during the viscous stage of the product can be more dispersed, the lubricating function can be achieved by forming a water film form, the mass and heat transfer process of a reaction system can be uniformed, and the purity and yield of the product can be enhanced; and an inert solvent is dropwise added during reaction, so that the conversion rate of the reaction can be enhanced on the basis of increasing the flowability of the product, and the viscous problems of the product canbe solved. Thus, the device is provided for the above technologies.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a method and a device for improving emulsification synthesis of 3,4-methylenedioxymandelic acid. Background technique [0002] 3,4-Methylenedioxymandelic acid is an intermediate in the synthesis of piperonal. Piperonal is widely used in perfumes, spices, cherry and vanilla flavorings. It has a long lasting fragrance and is used as a flavoring agent and a deodorant. It is a safe fragrance approved by the American Spice Extract Manufacturing Association. It is widely used in indoor fragrances, soap flavors, food flavors and tobacco flavors. It can also be used in chemical biopharmaceuticals. It is one of the special commodities for which the country implements an export license. [0003] The traditional synthesis method of 3,4-methylenedioxymandelic acid is to use piperonylcycline and glyoxylic acid to synthesize under acidic conditions. Shan Shaojun et ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/60
CPCC07D317/60Y02A50/30
Inventor 那平鄂生平焦晗王淳
Owner 山东天大泰泽环保科技有限公司
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