A kind of preparation method of glycyl-l-glutamine
A technology of glutamine and glycyl, which is applied in the field of preparation of glycyl-L-glutamine, can solve the problems of ammonium salt easily blocking a condenser, long concentration time, inconvenient production and the like, and achieves short concentration time, The effect of short reaction time and difficult removal
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Embodiment 1
[0026] (a) Preparation of crude glycyl-L-glutamine
[0027] In the plastic-lined high-pressure reactor, add 100kg of chloroacetyl-L-glutamine to dissolve it in 500kg of water, feed ammonia gas to 0.2~0.4Mpa, slowly raise the temperature to 42°C, at 42±1°C, 0.2~0.4 Stir under Mpa pressure for 5 hours; concentrate under reduced pressure, after 30 minutes, the temperature rises to 55~65°C, the vacuum is not higher than -0.09Mpa, concentrate until nearly dry, add 120kg of water, stir, heat to 52~56°C, add 2kg of activated carbon, Keep stirring for 25 minutes, filter out activated carbon, add 250kg methanol, keep stirring for 30 minutes, cool down to -4~-1°C, cool down and crystallize for 2~2.5 hours, centrifuge, and dry at 40~50°C for 8~10 hours to obtain off-white solid 82.8 kg, the liquid phase purity is not less than 97.8%;
[0028] (b) Glycyl-L-glutamine refining
[0029] Dissolve 82.5kg of crude product in 165kg of water, heat to 52~56℃, add 1.65kg of activated carbon,...
Embodiment 2
[0031] (a) Preparation of crude glycyl-L-glutamine
[0032] In the enamel reaction kettle, dissolve 200kg of chloroacetyl-L-glutamine in 1000kg of water, feed ammonia gas to 0.2~0.4Mpa, slowly raise the temperature to 42°C, and stir for 5 hours at 45°C under a pressure of 0.2~0.4Mpa; Concentrate under reduced pressure, after 30 minutes, the temperature rises to 55~65°C, the vacuum is not higher than -0.09Mpa, concentrate to nearly dry, add 240kg of water, stir, heat to 52~56°C, add 4kg of activated carbon, keep stirring for 25min, filter out the activated carbon , add 500kg of methanol, heat and stir for 30min, cool down to -4~-1°C, cool down and crystallize for 2~2.5 hours, shake off the material, dry at 40~50°C for 8~10 hours, and obtain 165.9kg of off-white solid. Less than 98.1%.
[0033] (b) Glycyl-L-glutamine refining
[0034] Dissolve 165kg of crude product in 330kg of water, heat to 52~56℃, add 3.3kg of activated carbon, keep stirring for 25min, filter out the activa...
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