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1. 发明授权

US09630942B2 Technological method for synthesis of optically pure L-/D-lactide catalyzed by biogenic guanidine 有权
公开(公告)号：US09630942B2
公开(公告)日：2017-04-25
申请号：US14782627
申请日：2013-08-17
申请人： Nanjing University
发明人： Hong Li , Quanxing Zhang , Na Cheng , Tianrong Zhang , Wei Jiang , Wei Huang , Bingcai Pan
IPC分类号： C07D319/12 , B01J31/02
CPC分类号： C07D319/12 , B01J31/0208 , B01J31/0241 , B01J31/0271 , B01J2231/34
摘要： A technological method for synthesizing optically pure L-/D-lactide by using a biogenic guanidine catalysis method. The method of the present invention comprises: by using biogenic guanidine creatinine (CR) as a catalyst and L-/D-lactic acid (90% of mass content) as a raw material, synthesizing optically pure L-/D-lactide by using a reactive reduced pressure distillation catalysis method. The method of the present invention has advantages that the used catalyst is biogenic guanidine creatinine and free of toxicity, metal, and cytotoxicity; the synthesized lactide is high in optical purity (the specific rotation of the L-lactide [α]25D=−276˜−280, and the specific rotation of the D-lactide [α]25D=280), and does not contain any metal; the amount of the catalyst used in reaction is low, the technological process is simplified (a process for rectifying and purifying a crude lactide product by using a conventional method is avoided); and the technological method is simple and convenient to operate and easy in industrial implementation.

2. 发明申请

US20160039782A1 TECHNOLOGICAL METHOD FOR SYNTHESIS OF OPTICALLY PURE L-/D-LACTIDE CATALYZED BY BIOGENIC GUANIDINE 有权
标题翻译：用于生物活性剂催化的光学纯化的L- / D-乳酸的合成方法
公开(公告)号：US20160039782A1
公开(公告)日：2016-02-11
申请号：US14782627
申请日：2013-08-17
申请人： Nanjing University
发明人： Hong Li , Quanxing Zhang , Na Cheng , Tianrong Zhang , Wei Jiang , Wei Huang , Bingcai Pan
IPC分类号： C07D319/12 , B01J31/02
CPC分类号： C07D319/12 , B01J31/0208 , B01J31/0241 , B01J31/0271 , B01J2231/34
摘要： A technological method for synthesizing optically pure L-/D-lactide by using a biogenic guanidine catalysis method. The method of the present invention comprises: by using biogenic guanidine creatinine (CR) as a catalyst and L-/D-lactic acid (90% of mass content) as a raw material, synthesizing optically pure L-/D-lactide by using a reactive reduced pressure distillation catalysis method. The method of the present invention has advantages that the used catalyst is biogenic guanidine creatinine and free of toxicity, metal, and cytotoxicity; the synthesized lactide is high in optical purity (the specific rotation of the L-lactide [α]25 D=−276˜−280, and the specific rotation of the D-lactide [α]25 D=280), and does not contain any metal; the amount of the catalyst used in reaction is low, the technological process is simplified (a process for rectifying and purifying a crude lactide product by using a conventional method is avoided); and the technological method is simple and convenient to operate and easy in industrial implementation.
摘要翻译：通过生物胍胍催化方法合成光学纯的L- / D-丙交酯的技术方法。本发明的方法包括：以生物胍胍肌酐（CR）为催化剂和L- / D-乳酸（90质量％）为原料，通过使用光学纯的L- / D-丙交酯一种反应性减压蒸馏催化方法。本发明的方法具有以下优点：所用催化剂是生物胍胍肌酐，无毒性，金属和细胞毒性; 合成的丙交酯的光学纯度高（L-丙交酯的比旋光度[α] 25 D = -276〜-280，D-丙交酯[α] 25 D = 280的比旋光度），不含有任何金属; 反应中使用的催化剂的量低，简化了工艺过程（避免了通过常规方法对粗制丙交酯产物进行精馏和纯化的方法）; 技术方法操作简便，工业实施方便。

3. 发明授权

US09469724B2 Method for synthesizing poly(butylene succinate-co-butylene adipate) 有权
标题翻译：聚（丁二酸丁二醇酯 - 己二酸丁二酯）
公开(公告)号：US09469724B2
公开(公告)日：2016-10-18
申请号：US14965873
申请日：2015-12-10
申请人： Nanjing University
发明人： Hong Li , Quanxing Zhang , Na Cheng , Tianrong Zhang , Wei Jiang , Bingcai Pan
IPC分类号： C08G63/02 , C08G63/16 , C08G63/85 , C08G63/87
CPC分类号： C08G63/16 , C08G63/85 , C08G63/87
摘要： A method for synthesizing poly(butylene succinate-co-butylene adipate) (PBSA), including: a) adding raw materials including succinic acid, adipic acid, and 1,4-butanediol into a reaction still; increasing the temperature in the reaction still to 130° C., and stirring the raw materials, then keeping the temperature in the reaction still at 170-200° C., and dehydrating for 1-3 hours at atmospheric pressure, to yield an oligomer of PBSA; and b) decreasing the temperature of the reaction still to 100° C., and adding a composite catalyst system, the total addition of the composite catalyst system accounting for one ten-thousandth to one ten-millionth of a total weight percentage of the raw materials; uniformly stiffing and mixing the composite catalyst system and reactants, slowly vacuum pumping the reaction still, heating the reaction still to a temperature of 200-240° C. and allowing the composite catalyst system and the reactants to react for 10-20 hrs.
摘要翻译：聚（丁二酸丁二酸酯 - 己二酸丁二酯）（PBSA）的合成方法，包括：a）将琥珀酸，己二酸和1,4-丁二醇的原料添加到反应釜中; 将反应温度升高至130℃，搅拌原料，然后将反应温度保持在170-200℃，并在大气压下脱水1-3小时，得到低聚物的PBSA; 和b）将反应温度降低至100℃，加入复合催化剂体系，复合催化剂体系的总添加量占原料总重量百分比的十万分之一到百万分之一材料; 均匀硬化和混合复合催化剂体系和反应物，缓慢抽真空反应，将反应物加热至200-240℃，使复合催化剂体系和反应物反应10-20小时。

4. 发明授权

US10570111B2 Method of purifying cyclic ester 有权
公开(公告)号：US10570111B2
公开(公告)日：2020-02-25
申请号：US16251047
申请日：2019-01-17
申请人： Nanjing University
发明人： Hong Li , Quanxing Zhang , Jiaye Sheng , Na Cheng , Wei Huang , Wei Jiang , Aimin Li
IPC分类号： C07D319/12
摘要： A method of purifying a cyclic ester, the method including: granulating a crude cyclic ester, an average particle size of resulting granules being 0.05-1.00 mm; adding the granules to 0-4° C. water to yield a mixture, a mass ratio of the water to the granules being (0.5-2):1; stirring the mixture, and performing solid-liquid separation on the mixture; repeating the stirring and solid-liquid separation for 1-4 times, to yield a purified cyclic ester; drying the purified cyclic ester at 0-4° C. and at an absolute pressure of less than or equal to 10 pascal for 4-6 hours, and continually drying the purified cyclic ester at 40-60° C. and at an absolute pressure of less than or equal to 5 pascal for 1-2 hours.

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