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1. 发明公开

EP3246310A1 METHOD FOR CONTINUOUS PREPARATION OF HIGH BULK DENSITY METHIONINE CRYSTAL 审中-公开
标题翻译：连续制备高密度蛋氨酸晶体的方法
公开(公告)号：EP3246310A1
公开(公告)日：2017-11-22
申请号：EP15881855.9
申请日：2015-12-23
申请人： Shandong Nhu Amino Acid Co., Ltd. , Zhejiang University , Zhejiang Nhu Co., Ltd.
发明人： CHEN, Zhirong , WANG, Zhixuan , CHEN, Cong , WANG, Zhengjiang , WANG, Cunchao , LI, Yin , ZHANG, Zhixiang
IPC分类号： C07C323/58 , C07C319/28 , B01D9/02
CPC分类号： B01D9/0036 , B01D9/0013 , B01D9/0027 , B01D9/0054 , B01D2009/0086 , C07C319/28 , C07C323/58
摘要： The present disclosure relates to a method for continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate solution, which is obtained from a reaction of 5- (β-methylmercaptoethyl) hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after being cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer and is sprayed in the form of liquid droplet or trickle into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the obtained mixture grows on fine crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a deposition area in the middle part of the crystallization region, the crystals having larger particle diameters deposits into an elutriation leg, while the fine crystals circulate with the external circulation material, and a part of the external circulation material is used to elutriate the crystals in the elutriation leg, while another part of the same is used to be mixed with the hydrolysate solution; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.
摘要翻译：本公开涉及用于连续制备高堆积密度甲硫氨酸晶体的方法。该方法的过程如下：将由5-（β-甲基巯基乙基）乙内酰脲和碳酸钾溶液反应获得的水解产物溶液与来自具有气相的DTB中和结晶器的外部循环物质混合中和部分; 冷却后，混合物进入结晶器上部的中和区的液体分配器，并以液滴或滴流形式喷入二氧化碳气体中进行中和反应，然后自然落入结晶器中的结晶区下部与该区域的材料混合; 所得混合物在体系中的细晶体上生长以形成具有较大粒径的晶体，同时形成新的晶核; 在结晶区域中部的沉积区域中，具有较大粒径的晶体沉积到淘析支路中，而细晶体与外循环材料一起循环，并且一部分外循环材料用于淘析晶体在淘洗支路中，另一部分用于与水解产物溶液混合; 并将淘洗腿中的晶体分离，洗涤并干燥以获得高堆积密度甲硫氨酸产品。

2. 发明授权

EP3246310B1 METHOD FOR CONTINUOUS PREPARATION OF HIGH BULK DENSITY METHIONINE CRYSTALS 有权
公开(公告)号：EP3246310B1
公开(公告)日：2019-08-07
申请号：EP15881855.9
申请日：2015-12-23
申请人： Shandong Nhu Amino Acid Co., Ltd. , Zhejiang University , Zhejiang Nhu Co., Ltd.
发明人： CHEN, Zhirong , WANG, Zhixuan , CHEN, Cong , WANG, Zhengjiang , WANG, Cunchao , LI, Yin , ZHANG, Zhixiang
IPC分类号： C07C323/58 , C07C319/28 , B01D9/02 , B01D9/00

3. 发明公开

EP3246310A4 METHOD FOR CONTINUOUS PREPARATION OF HIGH BULK DENSITY METHIONINE CRYSTAL 审中-公开
公开(公告)号：EP3246310A4
公开(公告)日：2018-01-10
申请号：EP15881855
申请日：2015-12-23
申请人： SHANDONG NHU AMINO ACID CO LTD , UNIV ZHEJIANG , ZHEJIANG NHU CO LTD
发明人： CHEN ZHIRONG , WANG ZHIXUAN , CHEN CONG , WANG ZHENGJIANG , WANG CUNCHAO , LI YIN , ZHANG ZHIXIANG
IPC分类号： C07C323/58 , B01D9/00 , B01D9/02 , C07C319/28
CPC分类号： B01D9/0054 , B01D9/0013 , B01D9/0027 , B01D9/0036 , C07C319/28 , C07C323/58
摘要： The present disclosure relates to a method for continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate solution, which is obtained from a reaction of 5- (²-methylmercaptoethyl) hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after being cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer and is sprayed in the form of liquid droplet or trickle into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the obtained mixture grows on fine crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a deposition area in the middle part of the crystallization region, the crystals having larger particle diameters deposits into an elutriation leg, while the fine crystals circulate with the external circulation material, and a part of the external circulation material is used to elutriate the crystals in the elutriation leg, while another part of the same is used to be mixed with the hydrolysate solution; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.

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