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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. 发明授权

EP2894147B1 CLEAN METHOD FOR PREPARING D,L-METHIONINE 有权
公开(公告)号：EP2894147B1
公开(公告)日：2018-07-18
申请号：EP13833235.8
申请日：2013-01-06
申请人： Zhejiang Nhu Company Ltd , Zhejiang University
发明人： CHEN, Zhirong , WANG, Cunchao , ZHAO, Chuqiu , WANG, Sujuan , ZHANG, Chengfeng , LONG, Tao , LIU, Xinhong
IPC分类号： C07C323/58 , C07C319/20
CPC分类号： C07C319/20 , C07D207/38 , C07C323/58
摘要： The present invention discloses a clean method for preparing a D,L-methionine comprising the steps of: preparing a potassium cyanide solution using a crystallized mother solution containing potassium carbonate as an absorbing liquid to absorb hydrocyanic acid, then reacting the potassium cyanide solution with 3-methylthio propionaldehyde and an ammonium bicarbonate solution at 50-150°C for 3-15 minutes so as to obtain a 5-(²-methylthioethyl)glycolyurea solution, then bring the 5-(²-methylthioethyl)glycolyurea solution to a temperature of 140-220°C and subjecting to a saponification reaction for 2-5 minutes, after the completion of the saponification, reducing the temperature to 0-40°C, extracting with an organic solvent, neutralising the water phase with CO 2 and crystallizing, then filtering, washing, and drying to obtain an acceptable D,L-methionine product; bring the crystallized D,L-methionine mother solution from filtration to a temperature to 110-160°C to remove CO 2 , which are all then circulated and used as a hydrocyanic acid-absorbing liquid. The process route of the present invention is a route suitable for a continuous and clean production, substantially without producing waste water and waste gas.

4. 发明公开

EP2894147A1 CLEAN METHOD FOR PREPARING D,L-METHIONINE 有权
标题翻译： SAUBERES VERFAHREN ZUR HERSTELLUNG VON D，L-METHIONIN
公开(公告)号：EP2894147A1
公开(公告)日：2015-07-15
申请号：EP13833235.8
申请日：2013-01-06
申请人： Zhejiang Nhu Company Ltd , Zhejiang University
发明人： CHEN, Zhirong , WANG, Cunchao , ZHAO, Chuqiu , WANG, Sujuan , ZHANG, Chengfeng , LONG, Tao , LIU, Xinhong
IPC分类号： C07C323/58 , C07C319/20
CPC分类号： C07C319/20 , C07D207/38 , C07C323/58
摘要： The present invention discloses a clean method for preparing a D,L-methionine comprising the steps of: preparing a potassium cyanide solution using a crystallized mother solution containing potassium carbonate as an absorbing liquid to absorb hydrocyanic acid, then reacting the potassium cyanide solution with 3-methylthio propionaldehyde and an ammonium bicarbonate solution at 50-150°C for 3-15 minutes so as to obtain a 5-(β-methylthioethyl)glycolyurea solution, then bring the 5-(β-methylthioethyl)glycolyurea solution to a temperature of 140-220°C and subjecting to a saponification reaction for 2-5 minutes, after the completion of the saponification, reducing the temperature to 0-40°C, extracting with an organic solvent, neutralising the water phase with CO 2 and crystallizing, then filtering, washing, and drying to obtain an acceptable D,L-methionine product; bring the crystallized D,L-methionine mother solution from filtration to a temperature to 110-160°C to remove CO 2 , which are all then circulated and used as a hydrocyanic acid-absorbing liquid. The process route of the present invention is a route suitable for a continuous and clean production, substantially without producing waste water and waste gas.
摘要翻译：本发明公开了一种制备D，L-甲硫氨酸的清洁方法，包括以下步骤：使用含有碳酸钾的结晶母液作吸收液制备氰化钾溶液以吸收氢氰酸，然后使氰化钾溶液与3 - 甲硫基丙醛和碳酸氢铵溶液在50-150℃下反应3-15分钟，得到5-（2-甲硫基乙基）糖醇脲溶液，然后将5-（2-甲硫基乙基）糖醇脲溶液置于 140-220℃，皂化反应2-5分钟，皂化完成后，将温度降至0-40℃，用有机溶剂萃取，用CO 2中和水相并结晶，然后过滤，洗涤和干燥，得到可接受的D，L-甲硫氨酸产物; 将结晶的D，L-甲硫氨酸母液过滤至110-160℃，除去CO 2，然后将其循环并用作氢氰酸吸收液。本发明的工艺路线是适合连续清洁生产的路线，基本上不产生废水和废气。

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