A kind of drying method of citric acid monohydrate crystal and obtained citric acid crystal monohydrate
A drying method and technology of anhydrous citric acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve problems such as easy caking, poor appearance quality, and crystal detachment, so as to improve the color and enhance the combination The effect of improving crystallization water ability and anti-caking ability
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[0032] According to the drying method of the present invention, wherein, in step 1), the preparation method of the citric acid monohydrate crystal slurry can be prepared by methods known to those skilled in the art. Preferably, in order to obtain high crystallization rate and coarse, uniform citric acid monohydrate crystals, the following method is preferably used to prepare citric acid monohydrate crystal slurry, said method comprising:
[0033] (a) heating and concentrating the citric acid solution at 50-100°C until the citric acid concentration is 70-84% by weight to obtain a citric acid concentrate; (b) cooling the citric acid concentrate obtained in step (a) and Add anhydrous citric acid seed crystals to the citric acid concentrated solution when the citric acid concentrated solution is supersaturated. The temperature for adding anhydrous citric acid seed crystals is above 36.6°C; The temperature of the citric acid concentrate when adding the citric acid monohydrate seed ...
Embodiment 1
[0044] This embodiment is used to illustrate the drying method of citric acid monohydrate crystal provided by the present invention.
[0045] 1) (a) the concentration of citric acid is 38.7% by weight, the purity of citric acid is greater than 99% by weight, and the density is 1147kg / m 3 citric acid solution 5m 3 Heating and concentrating at 80° C. to a concentration of citric acid is 77.4% by weight to obtain a citric acid concentrate; (b) the above-mentioned citric acid concentrate is continuously sent into a crystallization tank, and the crystallization is carried out in the crystallization tank, and the concentrate is 10 When ℃ / h is cooled to 60 ℃ (supersaturation is 1.19), add particle size and be 85-150 purpose anhydrous citric acid seed crystal 50g (purity is 99.6% by weight); With the speed of 4 ℃ / h the temperature is reduced to Add 1.0 kg of citric acid monohydrate seed crystals with a particle size of 85-150 mesh at 36° C., and keep the temperature at this temperatu...
Embodiment 2
[0051] This embodiment is used to illustrate the drying method of citric acid monohydrate crystal provided by the present invention.
[0052] 1) (a) the concentration of citric acid is 38.1% by weight, the purity of citric acid is greater than 99% by weight, and the density is 1142kg / m 3 citric acid solution 5m 3 Heating and concentrating at 60° C. to a concentration of citric acid is 70% by weight to obtain a citric acid concentrate; (b) the citric acid concentrate enters a crystallization tank continuously, and crystallization is carried out in a crystallization tank, and the concentrate is heated at 10° C. / h When the temperature is lowered to 41°C (supersaturation is 1.14), add 50g of anhydrous citric acid seed crystals with a particle size of 85-150 mesh (purity is 99.8% by weight); when the temperature is reduced to 36°C at a speed of 6°C / h Add 0.78 kg of citric acid monohydrate seed crystals with a particle size of 85-150 mesh, and keep the temperature at this temperatu...
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