Crystalline powder of L-lysine L-glutamate
A technology of crystalline powder and glutamate, applied in the field of L-lysine L-glutamate crystalline powder and its preparation, can solve the problems of high product viscosity, solvent residue, serious product agglomeration, etc. Less water content, less methanol residue and better tapped density
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Embodiment 1
[0043] Add 10g of L-lysine L-glutamate into 80g of pure water, fully stir and dissolve to form an aqueous solution of L-lysine L-glutamate, then transfer it to a 500mL crystallization tank, and control the temperature at 10°C , and then add 420mL of anhydrous methanol to it as an anti-solvent for crystallization. After the white crystal substance appears, put it in the tank and carry out solid-liquid separation by suction filtration. Wash the crystal with 40mL of 90vol.% ethanol, and then in 4 ° C , put the separated crystals into 90vol.% ethanol for stirring conversion, the mass ratio of crystals and ethanol is 0.1:10, after stirring for 10h, the crystals are separated from solid and liquid by suction filtration, and then drummed at 30°C Air-dried for 10 hours, L-lysine L-glutamate crystalline powder was obtained, wherein the product purity was 99.1%, and the yield was 78.8%.
Embodiment 2
[0045] Add 30g of L-lysine L-glutamate into 100g of pure water, fully stir and dissolve to form an aqueous solution of L-lysine L-glutamate, then transfer it to a 500mL crystallization tank, and control the temperature at 15°C , and then add 400mL of 90vol.% methanol as an anti-solvent to crystallize. After the white crystal material appears, put it in the tank and carry out solid-liquid separation by suction filtration. Wash the crystal with 60mL of 95vol.% ethanol, and then in 25 ℃ , the separated crystals were put into 95vol.% ethanol and stirred for transformation. The mass ratio of crystals and ethanol was 1:10. After stirring for 30 hours, the crystals were subjected to solid-liquid separation by means of suction filtration, and then the crystals were separated at 70°C Blow drying for 12 hours to obtain L-lysine L-glutamate crystalline powder, wherein the product purity is 99.2%, and the yield is 81.6%.
Embodiment 3
[0047] Add 50g of L-lysine L-glutamate into 100g of pure water, fully stir and dissolve to form an aqueous solution of L-lysine L-glutamate, then transfer it to a 500mL crystallization tank, and control the temperature at 20°C , then add 300mL of 80vol.% anhydrous methanol to it as anti-solvent to carry out crystallization, after the white crystal substance appears, go down the tank, carry out solid-liquid separation with the mode of suction filtration, wash crystal with 80mL of 98vol.% ethanol, then in At 35°C, put the separated crystals into 98vol.% ethanol for stirring transformation, the mass ratio of the crystals to ethanol is 1.5:10, after stirring for 60 hours, the crystals are separated from the solid and liquid by suction filtration, and then separated at 45 Blow drying at ℃ for 15 hours to obtain L-lysine L-glutamate crystalline powder, wherein the product purity is 99.5%, and the yield is 88.9%.
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