公开(公告)号：US07253326B1

公开(公告)日：2007-08-07

申请号：US11401429

申请日：2006-04-10

申请人： Sung Shik Eom ,  Dong Hyun Ko ,  Ji Joong Moon ,  Jae Hoon Choe ,  Dae Sun Rew

发明人： Sung Shik Eom ,  Dong Hyun Ko ,  Ji Joong Moon ,  Jae Hoon Choe ,  Dae Sun Rew

IPC分类号： C07C31/22 ,  C07C29/38

CPC分类号： C07C29/38 ,  C07C31/22

摘要： The present invention relates to a method for preparing trimethylolpropane (TMP) comprising the steps of: 1) synthesizing trimethylolpropane by using n-butyl aldehyde, an aqueous solution of formaldehyde and an aqueous solution of alkali metal hydroxide through aldol condensation reaction and Cannizzaro reaction; 2) extracting trimethylolpropane from a resultant mixture of the step 1) by contacting the resultant mixture with an alcohol having 6 to 10 carbons; 3) removing alkali metal ion from a resultant extract of the step 2) by contacting the resultant extract with water; and 4) distilling the alkali metal ion-removed extract obtained from the step 3). According to the present invention, a separate formaldehyde recovery process can be omitted, the extraction efficiency of TMP can be maximized with using a relatively small amount of extraction solvent, the separation and recovery processes for extraction solvent can be simplified since a mixture of solvents is not used for TMP extraction, and the yield of TMP can be maximized while the amount of generated waste water can be minimized, thereby producing TMP economically with good efficiency.

摘要翻译： 本发明涉及一种制备三羟甲基丙烷（TMP）的方法，包括以下步骤：1）通过醛醇缩合反应和Cannizzaro反应，使用正丁醛，甲醛水溶液和碱金属氢氧化物水溶液合成三羟甲基丙烷; 2）通过使所得混合物与具有6至10个碳的醇接触，从步骤1）的所得混合物中提取三羟甲基丙烷; 3）通过使得到的提取物与水接触，从步骤2）的所得提取物中除去碱金属离子; 和4）蒸馏从步骤3）获得的碱金属离子去除的提取物。 根据本发明，可以省略单独的甲醛回收方法，使用相对少量的萃取溶剂可以最大限度地提高TMP的萃取效率，因为溶剂混合物的分离和回收方法可以简化，因此可以简化萃取溶剂的分离和回收过程 不用于TMP提取，并且可以最大限度地提高TMP的产率，同时可以最大限度地减少产生的废水量，从而以高效率经济地生产TMP。

公开(公告)号：US07453008B2

公开(公告)日：2008-11-18

申请号：US11209255

申请日：2005-08-23

申请人： Donghyun Ko ,  Kwang Ho Park ,  Sang Gi Lee ,  Jijoong Moon ,  Sungshik Eom ,  Dae Sun Rew

发明人： Donghyun Ko ,  Kwang Ho Park ,  Sang Gi Lee ,  Jijoong Moon ,  Sungshik Eom ,  Dae Sun Rew

IPC分类号： C07C67/02

CPC分类号： C07C67/08 ,  Y02P20/127 ,  C07C69/003 ,  C07C69/28

摘要： A method of synthesizing glycol diester by reacting a linear aliphatic carboxylic acid and a glycol monoester in the presence of a Lewis acid type catalyst is provided. In the method, after introducing the glycol monoester, the linear aliphatic carboxylic acid and the Lewis acid type catalyst into a reactor, the reaction occurs to produce reaction products and water in the reactor; an excess of the linear aliphatic carboxylic acid forms an azeotrope with water during the reaction to be sent to a condenser through a distillation column; the linear aliphatic carboxylic acid and water passed through the condenser are divided into an organic layer and an aqueous layer in an oil water separator; and the organic layer is returned to the distillation column through a material cycling line and water in the aqueous layer is removed through a water removal line. By utilizing reactive distillation technique, water produced during the reaction is rapidly removed, and thus the reaction time can be significantly reduced and the yield of the glycol diester can be maximized.

摘要翻译： 提供了在路易斯酸型催化剂存在下使直链脂族羧酸和二醇单酯反应合成二醇二酯的方法。 在该方法中，在将二醇单酯，直链脂肪族羧酸和路易斯酸型催化剂引入反应器中之后，发生反应以在反应器中产生反应产物和水; 过量的直链脂族羧酸在反应期间与水形成共沸物，通过蒸馏塔送至冷凝器; 将通过冷凝器的直链脂肪族羧酸和水分为油水分离器中的有机层和水层; 并且有机层通过材料循环管线返回到蒸馏塔中，水层中的水通过除水管线除去。 通过利用反应蒸馏技术，快速除去反应期间产生的水，从而可以显着降低反应时间，并使乙二醇二酯的产率最大化。

公开(公告)号：US07612228B2

公开(公告)日：2009-11-03

申请号：US12241521

申请日：2008-09-30

申请人： Donghyun Ko ,  Kwang Ho Park ,  Sang Gi Lee ,  Jijoong Moon ,  Sungshik Eom ,  Dae Sun Rew

发明人： Donghyun Ko ,  Kwang Ho Park ,  Sang Gi Lee ,  Jijoong Moon ,  Sungshik Eom ,  Dae Sun Rew

IPC分类号： C07C67/02

CPC分类号： C07C67/08 ,  Y02P20/127 ,  C07C69/003 ,  C07C69/28

摘要： A method of synthesizing glycol diester by reacting a linear aliphatic carboxylic acid and a glycol monoester in the presence of a Lewis acid type catalyst is provided. In the method, after introducing the glycol monoester, the linear aliphatic carboxylic acid and the Lewis acid type catalyst into a reactor, the reaction occurs to produce reaction products and water in the reactor; an excess of the linear aliphatic carboxylic acid forms an azeotrope with water during the reaction to be sent to a condenser through a distillation column; the linear aliphatic carboxylic acid and water passed through the condenser are divided into an organic layer and an aqueous layer in an oil water separator; and the organic layer is returned to the distillation column through a material cycling line and water in the aqueous layer is removed through a water removal line. By utilizing reactive distillation technique, water produced during the reaction is rapidly removed, and thus the reaction time can be significantly reduced and the yield of the glycol diester can be maximized.

摘要翻译： 提供了在路易斯酸型催化剂存在下使直链脂族羧酸和二醇单酯反应合成二醇二酯的方法。 在该方法中，在将二醇单酯，直链脂肪族羧酸和路易斯酸型催化剂引入反应器中之后，发生反应以在反应器中产生反应产物和水; 过量的直链脂族羧酸在反应期间与水形成共沸物，通过蒸馏塔送至冷凝器; 将通过冷凝器的直链脂肪族羧酸和水分为油水分离器中的有机层和水层; 并且有机层通过材料循环管线返回到蒸馏塔，水层中的水通过除水管线除去。 通过利用反应蒸馏技术，快速除去反应期间产生的水，从而可以显着降低反应时间，并使乙二醇二酯的产率最大化。

公开(公告)号：US20090023946A1

公开(公告)日：2009-01-22

申请号：US12241521

申请日：2008-09-30

申请人： Donghyun KO ,  Kwang Ho PARK ,  Sang Gi LEE ,  Jijoong MOON ,  Sungshik Eom ,  Dae Sun Rew

发明人： Donghyun KO ,  Kwang Ho PARK ,  Sang Gi LEE ,  Jijoong MOON ,  Sungshik Eom ,  Dae Sun Rew

IPC分类号： C07C69/34

CPC分类号： C07C67/08 ,  Y02P20/127 ,  C07C69/003 ,  C07C69/28

摘要： A method of synthesizing glycol diester by reacting a linear aliphatic carboxylic acid and a glycol monoester in the presence of a Lewis acid type catalyst is provided. In the method, after introducing the glycol monoester, the linear aliphatic carboxylic acid and the Lewis acid type catalyst into a reactor, the reaction occurs to produce reaction products and water in the reactor; an excess of the linear aliphatic carboxylic acid forms an azeotrope with water during the reaction to be sent to a condenser through a distillation column; the linear aliphatic carboxylic acid and water passed through the condenser are divided into an organic layer and an aqueous layer in an oil water separator; and the organic layer is returned to the distillation column through a material cycling line and water in the aqueous layer is removed through a water removal line. By utilizing reactive distillation technique, water produced during the reaction is rapidly removed, and thus the reaction time can be significantly reduced and the yield of the glycol diester can be maximized.

摘要翻译： 提供了在路易斯酸型催化剂存在下使直链脂族羧酸和二醇单酯反应合成二醇二酯的方法。 在该方法中，在将二醇单酯，直链脂肪族羧酸和路易斯酸型催化剂引入反应器中之后，发生反应以在反应器中产生反应产物和水; 过量的直链脂族羧酸在反应期间与水形成共沸物，通过蒸馏塔送至冷凝器; 将通过冷凝器的直链脂肪族羧酸和水分为油水分离器中的有机层和水层; 并且有机层通过材料循环管线返回到蒸馏塔，水层中的水通过除水管线除去。 通过利用反应蒸馏技术，快速除去反应期间产生的水，从而可以显着降低反应时间，并使乙二醇二酯的产率最大化。