Process for preparing glyphosate by using glycine
A preparation process and glycine method technology, applied in the field of preparation technology, can solve the problems of complex reaction components, increase the ratio of raw materials, affect product quality, etc. Effect
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Embodiment 1
[0024] (1) Add 33.6g of paraformaldehyde, 168g of methanol and 40.3g of triethylamine into a three-necked flask with a reflux condenser, a thermometer and a stirring device, keep the reaction temperature at 30°C, and stir to obtain a transparent reaction solution;
[0025] (2) Add 33 g of glycine to the above reaction solution, keep the temperature at 30° C., stir and react for 1 h to obtain a condensation solution;
[0026] (3) Add 68.5 g of dimethyl phosphite to the condensation solution, keep the temperature at 30° C., stir and react for 1 hour to obtain an esterification solution;
[0027] (4) Adding 212 g of hydrochloric acid with a weight percent concentration of 10% to the esterification solution for acidification, keeping the temperature at 20° C., to obtain a hydrolysis solution;
[0028] (5) Under normal pressure conditions, control the temperature at 80°C to carry out desolvation and deacidification, then under a vacuum pressure of 0.2MPa, control the temperature at...
Embodiment 2
[0030] (1) Add 33.6g of paraformaldehyde, 195g of methanol and 52.2g of triethylamine into a three-necked flask equipped with a reflux condenser, a thermometer and a stirring device, keep the reaction temperature at 40°C, and stir to obtain a transparent reaction solution;
[0031] (2) Add 38.3 g of glycine to the above reaction solution, keep the temperature at 40° C., stir and react for 1.5 h to obtain a condensation solution;
[0032] (3) Add 72.1 g of dimethyl phosphite to the condensation solution, keep the temperature at 40° C., stir and react for 1.5 h to obtain an esterification solution;
[0033] (4) Adding 212 g of hydrochloric acid with a weight percent concentration of 30% to the esterification solution for acidification, keeping the temperature at 30° C., to obtain a hydrolysis solution;
[0034] (5) Under normal pressure conditions, control the temperature at 100°C to carry out desolvation and deacidification, then under the vacuum pressure of 0.3MPa, control the...
Embodiment 3
[0036] (1) Add 33.6g of paraformaldehyde, 201.6g of methanol and 67.2g of triethylamine into a three-necked flask equipped with a reflux condenser, a thermometer and a stirring device, keep the reaction temperature at 50°C, and stir to obtain a transparent reaction solution;
[0037] (2) Add 50.4 g of glycine to the above reaction solution, keep the temperature at 45° C., stir and react for 2 hours to obtain a condensation solution;
[0038] (3) Add 84 g of dimethyl phosphite to the condensation solution, keep the temperature at 60° C., stir and react for 1.5 h to obtain an esterification solution;
[0039] (4) Adding 228.5 g of hydrochloric acid with a weight percent concentration of 35% to the esterification solution for acidification, keeping the temperature at 40° C., to obtain a hydrolysis solution;
[0040] (5) Under normal pressure conditions, control the temperature at 100°C to carry out desolvation and deacidification, then under the vacuum pressure of 0.4MPa, control...
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