Preparation method for crystallization type L-arginine-malate
A technology of arginine and crystalline form, which is applied in the field of preparation of amino acid salts, can solve the problems of crystalline L-arginine-malate complex, unsuitable for industrial production, unsatisfactory, etc. The effect of easy transportation, use and operation
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Embodiment 1
[0025] A preparation method of crystalline L-arginine-malate: in a 500ml reaction bottle, add 70ml (69.6g) of a 25% (weight) L-arginine solution (equivalent to 0.1molL-arginine acid), stir, slowly add 13.3g (0.1mol) malic acid, react at room temperature for 10mins, completely dissolve, then concentrate under reduced pressure, water bath temperature 55°C, concentrate the total volume of the reaction solution to about 56ml, cool to 23°C, and stir Slowly add 95% ethanol dropwise until a small amount of crystals are precipitated, stir for 10mins, then continue to add 95% ethanol dropwise, the total amount of ethanol is 42ml, and the dropping time is 2hr, then lower the temperature of the crystallization solution to 5-10°C, and let it stand for 30mins , to make the crystal crystallization complete, filter, and wash the crystal with 95% ethanol, and vacuum-dry at 60° C. to obtain 25 g of white flaky crystal form L-arginine-malate, the yield is 81.4%, and the obtained purity is 99.8 ...
Embodiment 2
[0027] A preparation method of crystalline L-arginine-malate: in a 500ml reaction bottle, add 70ml (69.6g) content of 20% (weight) L-arginine solution (equivalent to 0.08molL-arginine acid), stir, slowly add 10.64g (0.08mol) L-malic acid, react at room temperature for 10mins, dissolve completely, then concentrate under reduced pressure, water bath temperature 50°C, concentrate the total volume of the reaction solution to about 28ml, cool to 20°C, and Slowly add anhydrous methanol dropwise while stirring until a small amount of crystals are precipitated, stir for 10mins, then continue to drop anhydrous methanol, the total amount of anhydrous methanol is 168ml, and the dropping time is 2.5hr, then lower the temperature of the crystallization solution to 5- Stand at 10°C for 30mins to completely crystallize the crystals, filter, wash the crystals with anhydrous methanol, and dry them in vacuum at 50°C to obtain white flaky crystals of L-arginine-L-malate (1:1) 19.7 g, the yield w...
Embodiment 3
[0029] A preparation method of crystalline L-arginine-malate: in a 500ml reaction bottle, add 70ml (69.6g) of 30% (weight) L-arginine solution (equivalent to 0.12molL-arginine acid), stir, slowly add 15.96g (0.12mol) DL-malic acid, react at room temperature for 10mins, dissolve completely, then concentrate under reduced pressure, water bath temperature 80°C, concentrate the total volume of the reaction solution to about 49ml, cool to 22°C, and Slowly add isobutanol dropwise while stirring until a small amount of crystals are precipitated, stir for 10mins, then continue to add isobutanol dropwise, the total amount of isobutanol is 63ml, and the dropping time is 2hr, then lower the temperature of the crystallization solution to 5-10 ℃, stand for 30mins to make the crystal crystallize completely, filter, wash the crystal with isobutanol, and dry it in vacuum at 70℃ to obtain 30.5g of white flaky crystal L-arginine-DL-malate (1:1) , the yield was 82.8%, and the obtained purity was...
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