A kind of production method of powdery methionine hydroxy analogue with dispersion fluidity
A production method and fluidity technology are applied in the production field of methionine hydroxy analogues, which can solve the problems of affecting the use and long-term stability of addition, and achieve the effects of avoiding difficulty in mixing uniformity, simple production process and reducing nitrogen excretion.
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Embodiment 1
[0033] Add 160.00kg of 98% sulfuric acid (1600 moles) to the hydrolysis reactor, then slowly add 328.00kg of 80% 2-hydroxyl-4-methylsulfide to the reactor 2-hydroxy-4-methylthiobutyronitrile aqueous solution (2000 moles), control the addition speed, control the temperature of the reaction system at about 50 ° C, after the addition of 2-hydroxy-4-methylthio-butyronitrile aqueous solution, keep stirring at 50 ° C ~ 55 ° C After 30 minutes, its cyanohydrin was not detected by HPLC analysis. A 2-hydroxy-4-methylthiobutanamide sulfate aqueous solution was obtained, and the mass percentage of 2-hydroxy-4-methylthiobutanamide was 61.15%.
[0034] Add 485.33 kg of 99% isopropanol (8000 mol) by mass to the above reaction mixture, then raise the temperature to 95° C., stir and keep warm for 2 hours. After completion of the reaction, cool down to room temperature, add a total of 2100.00 kg of dichloromethane to the mixed solution obtained above in 3 times for extraction, and obtain dich...
Embodiment 2
[0037] Add 154.74kg of 95% sulfuric acid (1500 moles) in the hydrolysis reactor, then slowly add 336.41kg of 78% 2-hydroxyl-4-methylsulfide in the reactor Butyronitrile aqueous solution (2000 moles), control the addition speed, control the temperature of the reaction system at about 55°C, after adding 2-hydroxy-4-methylthiobutyronitrile aqueous solution, keep stirring at 55°C for 30 minutes, The cyanohydrin was not detected by HPLC analysis. A 2-hydroxy-4-methylthiobutyramide sulfate aqueous solution was obtained, and the mass percentage of 2-hydroxy-4-methylthiobutyramide was 60.76%.
[0038] Add 242.51 kg of 99% isopropanol (4000 mol) by mass to the above reaction mixture, then raise the temperature to 100° C., stir and keep warm for 2 hours. After completion of the reaction, cool down to room temperature, add 1538.24 kg of dichloromethane in total to the mixed solution obtained above in 3 times for extraction, and obtain dichloromethane containing 2-hydroxyl-4-methylthiobu...
Embodiment 3
[0041] Add 160.00kg of 98% sulfuric acid (1600 moles) to the hydrolysis reactor, then slowly add 328.00kg of 80% 2-hydroxyl-4-methylsulfide to the reactor 2-hydroxy-4-methylthiobutyronitrile aqueous solution (2000 moles), control the addition speed, control the temperature of the reaction system at about 50 ° C, after the addition of 2-hydroxy-4-methylthio-butyronitrile aqueous solution, keep stirring at 50 ° C ~ 55 ° C After 30 minutes, its cyanohydrin was not detected by HPLC analysis. A 2-hydroxy-4-methylthiobutanamide sulfate aqueous solution was obtained, and the mass percentage of 2-hydroxy-4-methylthiobutanamide was 61.15%.
[0042] Add 485.33 kg of 99% isopropanol (8000 mol) by mass to the above reaction mixture, then raise the temperature to 95° C., stir and keep warm for 2 hours. After completion of the reaction, cool down to room temperature, add a total of 2100.00 kg of dichloromethane to the mixed solution obtained above in 3 times for extraction, and obtain dich...
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