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公开(公告)号：US20180043281A1
公开(公告)日：2018-02-15
申请号：US15549833
申请日：2015-12-23
发明人： Zhirong Chen , Zhixuan Wang , Cong Chen , Zhengjiang Wang , Cunchao Wang , Yin Li , Zhixiang Zhang
IPC分类号： B01D9/00 , C07C319/28 , C07C323/58
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.
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公开(公告)号：US10293273B2
公开(公告)日：2019-05-21
申请号：US15549833
申请日：2015-12-23
发明人： Zhirong Chen , Zhixuan Wang , Cong Chen , Zhengjiang Wang , Cunchao Wang , Yin Li , Zhixiang Zhang
IPC分类号： B01D9/00 , 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.
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3.发明申请公开(公告)号：US20210147350A1
公开(公告)日：2021-05-20
申请号：US17263362
申请日：2019-08-27
发明人： Zhirong Chen , Hong Yin , Baishan Hu , Zhengjiang Wang , Zhixuan Wang , Cong Chen , Guisheng Qiu , Qichuan Li , Qingai Shi
IPC分类号： C07C319/20 , C07C319/28 , C07C323/52 , B01J19/24
摘要： Provided by the present disclosure are a method and a device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile. The method for preparing 2-hydroxy-4-methylthiobutyric acid provided by the present disclosure comprises: step (1), a step of reacting acrolein with methyl mercaptan to prepare 3-methylthiopropionaldehyde; step (2), a step of reacting 3-methylthiopropionaldehyde with hydrocyanic acid to prepare 2-hydroxy-4-methylthiobutyronitrile; and step (3), a step of hydrating 2-hydroxy-4-methylthiobutyronitrile by using sulfuric acid and then hydrolyzing to prepare 2-hydroxy-4-methylthiobutyric acid; wherein in steps (1), (2) and (3), the reaction status of the materials is detected online, and the proportions of the materials are controlled according to the detection results such that reactions are performed completely
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4.发明授权公开(公告)号：US11130732B2
公开(公告)日：2021-09-28
申请号：US17263362
申请日：2019-08-27
发明人： Zhirong Chen , Hong Yin , Baishan Hu , Zhengjiang Wang , Zhixuan Wang , Cong Chen , Guisheng Qiu , Qichuan Li , Qingai Shi
IPC分类号： C07C319/20 , C07C319/18 , B01J19/24 , C07C319/28 , C07C323/52
摘要： Provided by the present disclosure are a method and a device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile. The method for preparing 2-hydroxy-4-methylthiobutyric acid provided by the present disclosure comprises: step (1), a step of reacting acrolein with methyl mercaptan to prepare 3-methylthiopropionaldehyde; step (2), a step of reacting 3-methylthiopropionaldehyde with hydrocyanic acid to prepare 2-hydroxy-4-methylthiobutyronitrile; and step (3), a step of hydrating 2-hydroxy-4-methylthiobutyronitrile by using sulfuric acid and then hydrolyzing to prepare 2-hydroxy-4-methylthiobutyric acid; wherein in steps (1), (2) and (3), the reaction status of the materials is detected online, and the proportions of the materials are controlled according to the detection results such that reactions are performed completely.
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