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Method and device for synthesizing 3,4-dioxymethylene mandelic acid by enhanced emulsification

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

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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  • Method and device for synthesizing 3,4-dioxymethylene mandelic acid by enhanced emulsification
  • Method and device for synthesizing 3,4-dioxymethylene mandelic acid by enhanced emulsification
  • Method and device for synthesizing 3,4-dioxymethylene mandelic acid by enhanced emulsification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] A method for enhancing emulsification synthesis of 3,4-methylenedioxymandelic acid, carried out according to the following steps:

[0078] Step 1, 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;

[0079] Step 2, 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 ;

[0080] Step 3, when all the 98wt% concentrated sulfuric acid is added dropwise, continue to stir for 30 minutes, and the stirring temperature is -25°C;

[0081] Step 4, add 3,4-methylenedioxymandelic acid and benzyltriethylammonium chloride to the solution after step 3 is completed, add 4g of 3,4-methylenedioxymandelic acid , add the amou...

Embodiment 2

[0089] A method for enhancing emulsification synthesis of 3,4-methylenedioxymandelic acid, carried out according to the following steps:

[0090] Step 1, the mixture of 10g of water and 200g of 50wt% glyoxylic acid aqueous solution was stirred at a constant temperature, the temperature of the constant temperature stirring was -30°C, and the stirring rate was 430rpm;

[0091] Step 2, after starting to stir, add 98wt% concentrated sulfuric acid dropwise to the mixture at a rate of 9g / min per minute, add 150g of the total amount of 98wt% concentrated sulfuric acid dropwise, the stirring temperature is -28°C, and the stirring rate is 430rpm ;

[0092] Step 3, when all the 98wt% concentrated sulfuric acid is added dropwise, continue to stir for 30min, and the stirring temperature is -28°C;

[0093] Step 4, add 3,4-methylenedioxymandelic acid to the solution after step 3 is completed, and add 9 g of 3,4-methylenedioxymandelic acid;

[0094] Step 5, emulsify the solution after step...

Embodiment 3

[0101] A device for enhancing emulsification synthesis of 3,4-methylenedioxymandelic acid, comprising a jacketed distributor stirring tank, a sulfuric acid metering tank, a jacketed distributor emulsification tank, a jacketed distributor product stirring tank, Loop reactor with Venturi ejector, circulating suspended bed reactor, pepper ring metering tank, constant temperature tank, filtration equipment, feed pump, gas storage tank, filtrate tank, the outlet of the sulfuric acid metering tank is stirred with jacketed distributor The still pipes are connected, the sulfuric acid metering tank is arranged above the jacketed distributor stirring tank, and the outlet of the circulating liquid in the constant temperature tank is respectively connected to the jacket inlet and the jacket of the jacketed distributor stirring tank by pipelines. The jacket inlet of the emulsification kettle of the type distributor, the heat exchange medium inlet of the heat exchanger and the jacket inlet o...

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Abstract

The invention discloses a method for synthesizing 3,4-dioxymethylene mandelic acid by enhanced emulsification. According to the method, gas is introduced into a reaction system in mixed acid preparation and emulsification synthesis processes, so that a large quantity of bubbles are produced in the reaction system, the surface area of reactants is enlarged, the contact area between the reactants isincreased, and the reaction conversion rate and yield can be increased. By use of the homogenization effect of the emulsification process, 1,3-benzodioxole is uniformly dispersed in glyoxylic acid with tiny droplets, the contact efficiency of the reactants can be improved, and the product purity and yield can be increased. A product is used as an emulsifier, a stable emulsion system can be formedwhile no substances outside the reaction system are introduced, and the product separation process is simpler and easier. An emulsified solution is dispersed into tiny droplets by a loop reactor witha Venturi ejector and a circulating suspended bed reactor in the reaction process to form a microreaction system, the heat and mass transfer efficiency is improved, and the problem of production of byproducts due to non-uniform heat transfer is inhibited.

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 synthesizing 3,4-methylenedioxymandelic acid through enhanced emulsification. 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 Shao...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/60B01F5/04
CPCC07D317/60B01F25/312
Inventor 那平鄂生平王淳焦晗
Owner 山东天大泰泽环保科技有限公司
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