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
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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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