公开(公告)号：US08177881B2

公开(公告)日：2012-05-15

申请号：US12813698

申请日：2010-06-11

申请人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C22B3/16 ,  C22B59/00

CPC分类号： C22B59/00 ,  C22B3/0022 ,  Y02P10/234

摘要： Solvent extraction from an aqueous phase containing first and second rare earth elements is carried out by contacting an organic phase containing a diglycolamic acid as an extractant and a hydrocarbon or a low-polar alcohol as a solvent, with the aqueous phase below pH 3 for extracting the first rare earth element into the organic phase, back-extracting from the organic phase with an aqueous acid solution for recovering the first rare earth element, and recovering the second rare earth element which has not been extracted into the organic phase and has remained in the aqueous phase.

摘要翻译： 从含有第一和第二稀土元素的水相中的溶剂萃取通过使含有作为萃取剂的二甘醇酸的有机相和作为溶剂的烃或低极性醇接触，水相低于pH 3进行萃取 将第一稀土元素加入到有机相中，用用于回收第一稀土元素的酸性水溶液从有机相中回收，并回收未萃取到有机相中并保留在第二稀土元素中的第二稀土元素 水相。

公开(公告)号：US08802040B2

公开(公告)日：2014-08-12

申请号：US13530672

申请日：2012-06-22

申请人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa

发明人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa

IPC分类号： C22B59/00

CPC分类号： C01F17/0006 ,  C22B3/0022 ,  C22B59/00 ,  Y02P10/234

摘要： A target light rare earth element is separated from an aqueous solution containing two or more of La, Ce, Pr and Nd by contacting an organic phase containing an extractant with the aqueous solution in a counter-current flow multistage mixer-settler while adding an alkaline solution thereto, and contacting the organic phase with an acid aqueous solution for back-extracting the target element. The extractant is a dialkyl diglycol amic acid having formula: R1R2NCOCH2OCH2COOH wherein R1 and R2 are alkyl, at least one having at least 6 carbon atoms.

摘要翻译： 将含有萃取剂的有机相与逆流多级混合器 - 沉降器中的水溶液接触，同时加入碱性物质，将含有两种或多种La，Ce，Pr和Nd的水溶液与目标轻稀土元素分离。 并使有机相与酸性水溶液接触，用于反萃取目标元素。 萃取剂是具有式：R 1 R 2 NCOCH 2 OCH 2 COOH的二烷基二甘醇酰胺酸，其中R 1和R 2是烷基，至少有一个具有至少6个碳原子。

公开(公告)号：US20100319491A1

公开(公告)日：2010-12-23

申请号：US12813698

申请日：2010-06-11

申请人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C22B59/00

CPC分类号： C22B59/00 ,  C22B3/0022 ,  Y02P10/234

摘要： Solvent extraction from an aqueous phase containing first and second rare earth elements is carried out by contacting an organic phase containing a diglycolamic acid as an extractant and a hydrocarbon or a low-polar alcohol as a solvent, with the aqueous phase below pH 3 for extracting the first rare earth element into the organic phase, back-extracting from the organic phase with an aqueous acid solution for recovering the first rare earth element, and recovering the second rare earth element which has not been extracted into the organic phase and has remained in the aqueous phase.

摘要翻译： 从含有第一和第二稀土元素的水相中的溶剂萃取通过使含有作为萃取剂的二甘醇酸的有机相和作为溶剂的烃或低极性醇接触，水相低于pH 3进行萃取 将第一稀土元素加入到有机相中，用用于回收第一稀土元素的酸性水溶液从有机相中回收，并回收未萃取到有机相中并保留在第二稀土元素中的第二稀土元素 水相。

公开(公告)号：US20120328493A1

公开(公告)日：2012-12-27

申请号：US13530672

申请日：2012-06-22

申请人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa

发明人： Hiroto Sugahara ,  Kazuaki Sakaki ,  Takehisa Minowa

IPC分类号： C22B59/00

CPC分类号： C01F17/0006 ,  C22B3/0022 ,  C22B59/00 ,  Y02P10/234

摘要： A target light rare earth element is separated from an aqueous solution containing two or more of La, Ce, Pr and Nd by contacting an organic phase containing an extractant with the aqueous solution in a counter-current flow multistage mixer-settler while adding an alkaline solution thereto, and contacting the organic phase with an acid aqueous solution for back-extracting the target element. The extractant is a dialkyl diglycol amic acid having formula: R1R2NCOCH2OCH2COOH wherein R1 and R2 are alkyl, at least one having at least 6 carbon atoms.

摘要翻译： 将含有萃取剂的有机相与逆流多级混合器 - 沉降器中的水溶液接触，同时加入碱性物质，将含有两种或多种La，Ce，Pr和Nd的水溶液与目标轻稀土元素分离。 并使有机相与酸性水溶液接触，用于反萃取目标元素。 萃取剂是具有式：R 1 R 2 NCOCH 2 OCH 2 COOH的二烷基二甘醇酰胺酸，其中R 1和R 2是烷基，至少有一个具有至少6个碳原子。

公开(公告)号：US08841482B2

公开(公告)日：2014-09-23

申请号：US13807955

申请日：2011-07-01

申请人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C07C235/06 ,  C07C271/12 ,  C07C231/02 ,  C22B7/00 ,  C22B7/02 ,  C22B47/00 ,  C22B59/00 ,  C22B3/08 ,  C22B3/44 ,  C22B5/10 ,  C22B26/10

CPC分类号： C07C271/12 ,  C07C231/02 ,  C07C235/06 ,  C22B3/08 ,  C22B3/44 ,  C22B5/10 ,  C22B7/007 ,  C22B7/02 ,  C22B26/10 ,  C22B47/00 ,  C22B59/00 ,  Y02P10/234

摘要： A rare earth metal extractant containing, as the extractant component, dialkyldiglycol amide acid which is excellent in breaking down light rare earth elements is reacted in diglycolic acid (X mol) and an esterification agent (Y mol) at a reaction temperature of 70° C. or more and for a reaction time of one hour or more such that the mol ratio of Y/X is 2.5 or more, and is subjected to vacuum concentration. Subsequently, a reaction intermediate product is obtained by removing unreacted products and reaction residue, and an aprotic polar solvent is added as the reaction solvent. Then, the reaction intermediate product is reacted with dialkyl amine (Z mol) such that the mol ratio of Z/X is 0.9 or more and the aprotic polar solvent is removed. As a consequence, a rare earth metal extractant is efficiently synthesized at a low cost and at a high yield without having to use expensive diglycolic acid anhydride and harmful dichloromethane.

摘要翻译： 在二氯乙酸（X mol）和酯化剂（Y mol）中，在70℃的反应温度下，含有作为萃取剂成分的分解轻稀土元素的二烷基二乙二醇酰胺酸的稀土金属萃取剂 反应时间为1小时以上，Y / X的摩尔比为2.5以上，进行真空浓缩。 随后，通过除去未反应产物和反应残余物获得反应中间产物，并加入非质子极性溶剂作为反应溶剂。 然后，将反应中间产物与二烷基胺（Z mol）反应，使Z / X的摩尔比为0.9以上，去除非质子极性溶剂。 因此，稀土金属萃取剂以低成本和高收率有效地合成，而不必使用昂贵的二甘醇酸酐和有害的二氯甲烷。

公开(公告)号：US08519184B2

公开(公告)日：2013-08-27

申请号：US13176214

申请日：2011-07-05

申请人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Ohashi ,  Tetsuya Kume ,  Masahiko Ikka ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Ohashi ,  Tetsuya Kume ,  Masahiko Ikka ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C07C229/22

CPC分类号： C07C231/02 ,  C07C235/06

摘要： A rare earth metal extractant in the form of a dialkyl diglycol amic acid is synthesized by reacting diglycolic anhydride with a dialkylamine in a synthesis medium. A molar ratio (B/A) of dialkylamine (B) to diglycolic anhydride (A) is at least 1.0. A non-polar or low-polar solvent in which the dialkyl diglycol amic acid is dissolvable is used as the synthesis medium.

摘要翻译： 通过在合成介质中使二甘醇酸酐与二烷基胺反应合成二烷基二甘醇酰胺酸形式的稀土金属萃取剂。 二烷基胺（B）与二甘醇酸酐（A）的摩尔比（B / A）为至少1.0。 使用其中可溶解二烷基二甘醇酰胺酸的非极性或低极性溶剂作为合成介质。

公开(公告)号：US20120004458A1

公开(公告)日：2012-01-05

申请号：US13176214

申请日：2011-07-05

申请人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Ohashi ,  Tetsuya Kume ,  Masahiko Ikka ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Ohashi ,  Tetsuya Kume ,  Masahiko Ikka ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C07C231/02

CPC分类号： C07C231/02 ,  C07C235/06

摘要： A rare earth metal extractant in the form of a dialkyl diglycol amic acid is synthesized by reacting diglycolic anhydride with a dialkylamine in a synthesis medium. A molar ratio (B/A) of dialkylamine (B) to diglycolic anhydride (A) is at least 1.0. A non-polar or low-polar solvent in which the dialkyl diglycol amic acid is dissolvable is used as the synthesis medium.

摘要翻译： 通过在合成介质中使二甘醇酸酐与二烷基胺反应合成二烷基二甘醇酰胺酸形式的稀土金属萃取剂。 二烷基胺（B）与二甘醇酸酐（A）的摩尔比（B / A）为至少1.0。 使用其中可溶解二烷基二甘醇酰胺酸的非极性或低极性溶剂作为合成介质。

公开(公告)号：US20130102806A1

公开(公告)日：2013-04-25

申请号：US13807955

申请日：2011-07-01

申请人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C07C271/12

CPC分类号： C07C271/12 ,  C07C231/02 ,  C07C235/06 ,  C22B3/08 ,  C22B3/44 ,  C22B5/10 ,  C22B7/007 ,  C22B7/02 ,  C22B26/10 ,  C22B47/00 ,  C22B59/00 ,  Y02P10/234

摘要： A rare earth metal extractant containing, as the extractant component, dialkyldiglycol amide acid which is excellent in breaking down light rare earth elements is reacted in diglycolic acid (X mol) and an esterification agent (Y mol) at a reaction temperature of 70° C. or more and for a reaction time of one hour or more such that the mol ratio of Y/X is 2.5 or more, and is subjected to vacuum concentration. Subsequently, a reaction intermediate product is obtained by removing unreacted products and reaction residue, and an aprotic polar solvent is added as the reaction solvent. Then, the reaction intermediate product is reacted with dialkyl amine (Z mol) such that the mol ratio of Z/X is 0.9 or more and the aprotic polar solvent is removed. As a consequence, a rare earth metal extractant is efficiently synthesized at a low cost and at a high yield without having to use expensive diglycolic acid anhydride and harmful dichloromethane.

摘要翻译： 在二氯乙酸（X mol）和酯化剂（Y mol）中，在70℃的反应温度下，含有作为萃取剂成分的分解轻稀土元素的二烷基二乙二醇酰胺酸的稀土金属萃取剂 反应时间为1小时以上，Y / X的摩尔比为2.5以上，进行真空浓缩。 随后，通过除去未反应产物和反应残余物获得反应中间产物，并加入非质子极性溶剂作为反应溶剂。 然后，将反应中间产物与二烷基胺（Z mol）反应，使Z / X的摩尔比为0.9以上，去除非质子极性溶剂。 因此，稀土金属萃取剂以低成本和高收率有效地合成，而不必使用昂贵的二甘醇酸酐和有害的二氯甲烷。

公开(公告)号：US20130123534A1

公开(公告)日：2013-05-16

申请号：US13808220

申请日：2011-07-01

申请人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C07C231/02

CPC分类号： C07C231/02 ,  C07C235/06 ,  C22B3/08 ,  C22B3/44 ,  C22B47/00 ,  C22B59/00 ,  Y02P10/234 ,  Y02W30/54

摘要： A rare earth metal extractant containing, as the extractant component, dialkyldiglycol amide acid which is excellent in breaking down light rare earth elements is reacted in diglycolic acid (X mol) and an esterification agent (Y mol) at a reaction temperature of 70° C. or more and for a reaction time of one hour or more such that the mol ratio of Y/X is 2.5 or more, and is subjected to vacuum concentration. Subsequently, a reaction intermediate product is obtained by removing unreacted products and reaction residue. Then a nonpolar or low-polar solvent which is an organic solvent for forming an organic phase during solvent extraction of the rare earth metal and which is capable of dissolving dialkyldiglycol amide acid is added as the reaction solvent, and the reaction intermediate product is reacted with dialkyl amine (Z mol) such that the mol ratio of Z/X is 0.9 or more.

摘要翻译： 在二氯乙酸（X mol）和酯化剂（Y mol）中，在70℃的反应温度下，将分解轻稀土元素的二烷基二乙二醇酰胺酸作为萃取剂成分的稀土金属萃取剂反应 反应时间为1小时以上，Y / X的摩尔比为2.5以上，进行真空浓缩。 随后，通过除去未反应的产物和反应残余物获得反应中间产物。 然后加入作为在稀土金属溶剂萃取中形成有机相并能够溶解二烷基二乙酰胺酸的有机溶剂的非极性或低极性溶剂作为反应溶剂，将反应中间产物与 二烷基胺（Z摩尔），使Z / X的摩尔比为0.9以上。

公开(公告)号：US09133100B2

公开(公告)日：2015-09-15

申请号：US13808220

申请日：2011-07-01

申请人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

发明人： Kazuaki Sakaki ,  Hiroto Sugahara ,  Tetsuya Kume ,  Masaki Ohashi ,  Hirochika Naganawa ,  Kojiro Shimojo

IPC分类号： C07C229/00 ,  C07C231/02 ,  C07C235/06 ,  C22B47/00 ,  C22B59/00 ,  C22B3/08 ,  C22B3/44

CPC分类号： C07C231/02 ,  C07C235/06 ,  C22B3/08 ,  C22B3/44 ,  C22B47/00 ,  C22B59/00 ,  Y02P10/234 ,  Y02W30/54

摘要： A rare earth metal extractant containing, as the extractant component, dialkyldiglycol amide acid which is excellent in breaking down light rare earth elements is reacted in diglycolic acid (X mol) and an esterification agent (Y mol) at a reaction temperature of 70° C. or more and for a reaction time of one hour or more such that the mol ratio of Y/X is 2.5 or more, and is subjected to vacuum concentration. Subsequently, a reaction intermediate product is obtained by removing unreacted products and reaction residue. Then a nonpolar or low-polar solvent which is an organic solvent for forming an organic phase during solvent extraction of the rare earth metal and which is capable of dissolving dialkyldiglycol amide acid is added as the reaction solvent, and the reaction intermediate product is reacted with dialkyl amine (Z mol) such that the mol ratio of Z/X is 0.9 or more.

摘要翻译： 在二氯乙酸（X mol）和酯化剂（Y mol）中，在70℃的反应温度下，含有作为萃取剂成分的分解轻稀土元素的二烷基二乙二醇酰胺酸的稀土金属萃取剂 反应时间为1小时以上，Y / X的摩尔比为2.5以上，进行真空浓缩。 随后，通过除去未反应的产物和反应残余物获得反应中间产物。 然后加入作为在稀土金属溶剂萃取中形成有机相并能够溶解二烷基二乙酰胺酸的有机溶剂的非极性或低极性溶剂作为反应溶剂，将反应中间产物与 二烷基胺（Z摩尔），使Z / X的摩尔比为0.9以上。