US 11,780,870 B2
Method for preparing crystalline D-psicose
Zhaobo Gan, Shandong (CN); Xianbao Shao, Shandong (CN); Fanghua Li, Shandong (CN); Qian Du, Shandong (CN); Xingjing Zhang, Shandong (CN); and Shuangshuang Liu, Shandong (CN)
Assigned to SHANDONG BAILONG CHUANGYUAN BIO-TECH CO., LTD., Shandong (CN)
Appl. No. 18/11,614
Filed by SHANDONG BAILONG CHUANGYUAN BIO-TECH CO., LTD., Shandong (CN)
PCT Filed Dec. 3, 2021, PCT No. PCT/CN2021/135345
§ 371(c)(1), (2) Date Dec. 20, 2022,
PCT Pub. No. WO2022/117074, PCT Pub. Date Jun. 9, 2022.
Claims priority of application No. 202011406639.1 (CN), filed on Dec. 4, 2020.
Prior Publication US 2023/0287026 A1, Sep. 14, 2023
Int. Cl. C07H 1/06 (2006.01); C07H 3/02 (2006.01)
CPC C07H 1/06 (2013.01) [C07H 3/02 (2013.01); C07B 2200/13 (2013.01)] 7 Claims
 
1. A preparation method of crystalline D-psicose, wherein, successively performing evaporative crystallization, crystal regulation, and cooling crystallization to obtain crystalline D-psicose;
said evaporative crystallization comprises adding crystal seeds when a solid mass content is 70˜75% to perform an evaporative crystallization;
said cooling crystallization is performed by applying a stepped cooling having a slow cooling rate in an initial stage and a rapid cooling rate in a later stage; wherein said stepped cooling has following operations: in a range of 50˜41° C., cooling at a rate of 0.1˜0.3° C. per hour; in a range of 41˜35° C., cooling at a rate of 0.4˜0.6° C. per hour; in a range of 35˜30° C., cooling at a rate of 0.9˜1.1° C. per hour; and the crystallization is finished when temperature is cooled to 30° C.; and said crystal regulation is carried out by adding water at the same time as an evaporative crystallization is performed, and a solid mass content is maintained constant during the crystal regulation process.