Preparation method of glycine
A technology of glycine and chloroacetic acid, which is applied in the field of chemical production, can solve the problems of yield and purity decline, cost increase, environmental pollution, etc., and achieve the effects of simple preparation method, production cost saving and environmental friendliness
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Embodiment 1
[0026] Add 192g of chloroacetic acid (content 98%) and 800g of methanol into a four-neck bottle, put in a magnet, install a thermometer and a reflux condenser, and after the chloroacetic acid is stirred and dissolved, start to pass ammonia, and control the temperature of ammonia flow at 10-30°C , Stop passing ammonia after the solution reaches alkaline pH=9. Add 72g of urotropine, raise the temperature to 66°C, start adding 204g of triethylamine dropwise, keep the temperature at 65-70°C, complete the dropwise addition within 1 hour, and keep warm for 0.5h after dropping. Cool down to 20-30°C, filter, rinse the filter cake with 92% methanol, filter, and dry to obtain 149.1 g of glycine with a purity of 97.8% and a molar yield of glycine based on chloroacetic acid of 97.6%. The filtered reaction solution was evaporated and concentrated at a temperature of 50°C and a vacuum pressure of -0.085MPa--0.095MPa. After 300mL of methanol was distilled off, the remaining mother liquor was...
Embodiment 2
[0028] Add 50g of chloroacetic acid (content 98%) and 200g of methanol evaporated in Example 1 into the beaker, after stirring and dissolving the chloroacetic acid, start passing ammonia, control the temperature of passing ammonia at 10-30°C, and make the solution reach alkaline pH=9 Then stop the ammonia. Add the reaction mother liquor that contains urotropine in the solution that has reacted and embodiment one in the four-neck bottle, the volume of the reaction mother liquor that contains urotropine among the described embodiment one is the volume of the reaction mother liquor that contains urotropine that implements one obtains 26% of the total volume of the reaction mother liquor, install a thermometer and a reflux condenser, raise the temperature to 66°C, start adding 52g of triethylamine dropwise, maintain the temperature at 65-70°C, complete the dropwise addition within 1h, and keep warm for 0.5h after dropping. Cool down to 20-30°C, filter, rinse the filter cake with 9...
Embodiment 3
[0031] Add 50g of chloroacetic acid (content 98%) and 200g of methanol evaporated in Example 2 into the beaker. After the chloroacetic acid is stirred and dissolved, start passing ammonia, and control the temperature of passing ammonia at 10-30°C, and the solution reaches alkaline pH=9 Then stop the ammonia. Add the reacted solution and the reaction mother liquor containing urotropine in Example 2 into a four-necked bottle, install a thermometer and a reflux condenser, raise the temperature to 66°C, start adding 52g of triethylamine dropwise, and maintain the temperature at 65- 70°C, the dropwise addition is completed within 1 hour, and the dropwise temperature is kept for 0.5 hour. Cool down to 20-30°C, filter, rinse the filter cake with 92% methanol, filter, and dry to obtain 38.8 g of glycine, with a purity of 98.0%, and a molar yield of glycine based on chloroacetic acid of 97.6%. The filtered reaction solution was evaporated and concentrated at a temperature of 50°C and ...
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