公开(公告)号：US20120271066A1

公开(公告)日：2012-10-25

申请号：US13344995

申请日：2012-01-06

Applicant: Chien-Chang Chiang ,  Cheng-Fa Hsieh ,  Pin-To Yao ,  Shih-Yao Chao

Inventor： Chien-Chang Chiang ,  Cheng-Fa Hsieh ,  Pin-To Yao ,  Shih-Yao Chao

IPC: B01J21/06 ,  C07C249/04

CPC classification number: C01B37/005 ,  B01J29/035 ,  C07C249/04 ,  C07C251/44

Abstract: The present invention provides a method for preparing a titanium-silicalite molecular sieve, and a method for preparing cyclohexanone oxime using the titanium-silicalite molecular sieve. The method for preparing a titanium-silicalite molecular sieve includes the steps of preparing a mixture of a titanium source, a silicon source and a template agent, wherein the titanium source has a structure of formula (I); heating the mixture to form a gel mixture; mixing the gel mixture with water; heating the gel mixture mixed with the water in a water bathe; and calcining the gel mixture mixed with the water. The method using the titanium-silicalite molecular sieve for preparing cyclohexanone oxime results in high conversion rate and high selectivity.

Abstract translation: 本发明提供一种钛 - 硅沸石分子筛的制备方法，以及使用钛 - 硅沸石分子筛制备环己酮肟的方法。 制备钛 - 硅沸石分子筛的方法包括制备钛源，硅源和模板剂的混合物的步骤，其中钛源具有式（I）的结构; 加热混合物以形成凝胶混合物; 将凝胶混合物与水混合; 在水浴中加热与水混合的凝胶混合物; 并煅烧与水混合的凝胶混合物。 使用钛硅沸石分子筛制备环己酮肟的方法导致高转化率和高选择性。

公开(公告)号：US07417168B2

公开(公告)日：2008-08-26

申请号：US11732837

申请日：2007-04-05

Applicant: Pin-To Yao ,  Cheng-Fa Hsieh ,  Yuh-Ing Hwang

Inventor： Pin-To Yao ,  Cheng-Fa Hsieh ,  Yuh-Ing Hwang

IPC: C07C239/08

CPC classification number: C01B21/1418 ,  C01C3/11 ,  C01C3/12 ,  C01P2006/80

Abstract: A method for preparing hydroxylamine is provided that includes the steps of (i) pretreating an acidic buffer solution; and (ii) reducing nitrate ions in the acidic buffer solution with hydrogen to give hydroxylamine in the presence of catalysts, wherein the pretreatment is performed by adding a precipitant represented by formula (I) to the acidic buffer solution, [(A)aM(CN)6.xH2O]  (I) allowing the metal impurities in the acidic buffer solution to react with the precipitant to form metal complex, and then to remove the metal complex. The metal complex is formed and separated by pretreating the acidic buffer solution with a specific precipitant without adjusting pH and changing the composition of the acidic buffer solution prior to hydroxylamine synthesis, thus enhancing the selectivity of the hydroxylamine production.

Abstract translation: 提供了制备羟胺的方法，其包括以下步骤：（i）预处理酸性缓冲溶液; （ii）在催化剂存在下用氢还原酸性缓冲溶液中的硝酸根离子，得到羟胺，其中预处理是通过将由式（I）表示的沉淀剂加入到酸性缓冲溶液中， 公式描述=“在线公式”end =“lead”？> [（A）aM（CN）6 .XH （I）<？ -line-formula description =“In-line Formulas”end =“tail”？>使酸性缓冲溶液中的金属杂质与沉淀剂反应形成金属络合物，然后除去金属络合物。 通过用特定沉淀剂预处理酸性缓冲溶液而不调节pH并在羟胺合成之前改变酸性缓冲溶液的组成，形成和分离金属络合物，从而提高羟胺生产的选择性。

公开(公告)号：US20080015388A1

公开(公告)日：2008-01-17

申请号：US11732837

申请日：2007-04-05

Applicant: Pin-To Yao ,  Cheng-Fa Hsieh ,  Yuh-Ing Hwang

Inventor： Pin-To Yao ,  Cheng-Fa Hsieh ,  Yuh-Ing Hwang

IPC: C07C239/08

CPC classification number: C01B21/1418 ,  C01C3/11 ,  C01C3/12 ,  C01P2006/80

Abstract: A method for preparing hydroxylamine is provided that includes the steps of (i) pretreating an acidic buffer solution; and (ii) reducing nitrate ions in the acidic buffer solution with hydrogen to give hydroxylamine in the presence of catalysts, wherein the pretreatment is performed by adding a precipitant represented by formula (I) to the acidic buffer solution, [(A)aM(CN)6.xH2O]  (I) allowing the metal impurities in the acidic buffer solution to react with the precipitant to form metal complex, and then to remove the metal complex. The metal complex is formed and separated by pretreating the acidic buffer solution with a specific precipitant without adjusting pH and changing the composition of the acidic buffer solution prior to hydroxylamine synthesis, thus enhancing the selectivity of the hydroxylamine production.

Abstract translation: 提供了制备羟胺的方法，其包括以下步骤：（i）预处理酸性缓冲溶液; （ii）在催化剂存在下用氢还原酸性缓冲溶液中的硝酸根离子，得到羟胺，其中预处理是通过将由式（I）表示的沉淀剂加入到酸性缓冲溶液中， 公式描述=“在线公式”end =“lead”？> [（A）aM（CN）6 .XH （I）<？ -line-formula description =“In-line Formulas”end =“tail”？>使酸性缓冲溶液中的金属杂质与沉淀剂反应形成金属络合物，然后除去金属络合物。 通过用特定沉淀剂预处理酸性缓冲溶液而不调节pH并在羟胺合成之前改变酸性缓冲溶液的组成，形成和分离金属络合物，从而提高羟胺生产的选择性。

公开(公告)号：US09371238B2

公开(公告)日：2016-06-21

申请号：US13345089

申请日：2012-01-06

Applicant: Ya-Ping Chen ,  Cheng-Fa Hsieh ,  Pin-To Yao ,  Chien-Chang Chiang

Inventor： Ya-Ping Chen ,  Cheng-Fa Hsieh ,  Pin-To Yao ,  Chien-Chang Chiang

IPC: C01B37/00 ,  C01B39/08 ,  C07C249/04 ,  B01J29/89

CPC classification number: C01B37/005 ,  B01J29/89 ,  C01B39/085 ,  C01B39/087 ,  C07C249/04 ,  C07C251/44

Abstract: The present invention provides a titanium-silicalite molecular sieve and a method for preparing the same. The method includes the steps of preparing a mixture of a titanium source, a silicon source, a transition metal source, a template agent and water; heating the mixture to form a gel mixture; heating the gel mixture in a water bath; and calcining the gel mixture after the gel mixture in the water bath to form the titanium-silicalite molecular sieve. The present invention further provides a method for preparing cyclohexanone oxime by using the titanium-silicalite molecular sieve as the catalyst which results in high conversion rate, high selectivity and high usage efficiency of hydrogen peroxide.

Abstract translation: 本发明提供钛 - 硅沸石分子筛及其制备方法。 该方法包括制备钛源，硅源，过渡金属源，模板剂和水的混合物的步骤; 加热混合物以形成凝胶混合物; 在水浴中加热凝胶混合物; 并在凝胶混合物中在水浴中煅烧凝胶混合物以形成钛 - 硅沸石分子筛。 本发明还提供了通过使用钛 - 硅沸石分子筛作为催化剂制备环己酮肟的方法，其导致过氧化氢的高转化率，高选择性和高使用效率。

公开(公告)号：US08772194B2

公开(公告)日：2014-07-08

申请号：US13344869

申请日：2012-01-06

Applicant: Shih-Yao Chao ,  Cheng-Fa Hsieh ,  Chien-Chang Chiang ,  Ya-Ping Chen ,  Pin-To Yao

Inventor： Shih-Yao Chao ,  Cheng-Fa Hsieh ,  Chien-Chang Chiang ,  Ya-Ping Chen ,  Pin-To Yao

IPC: B01J29/89 ,  C07C249/04

CPC classification number: B01J29/89 ,  B01J35/023 ,  C01B37/005 ,  C07C249/04 ,  C07C251/44

Abstract: The present invention provides a method for preparing a large-sized titanium-silicalite molecular sieve, and a method for preparing cyclohexanone oxime using the large-sized titanium-silicalite molecular sieve. The method for preparing a large-sized titanium-silicalite molecular sieve includes preparing a mixture of a titanium source, a silicon source and a template agent; heating the mixture to form a gel mixture; mixing a colloidal silica with the gel mixture; heating the gel mixture mixed with the colloidal silica in a water bath; and calcining the gel mixture mixed with the colloidal silica. In the present invention, the average particle size of the large-sized titanium-silicalitem molecular sieve is more than 10 um, and the particle size distribution is centralized, so as to avoid the formation of titanium-oxygen-titanium bonding. The method for preparing cyclohexanone oxime using the large-sized titanium-silicalite molecular sieve results in high conversion rate, high selectivity and easy recovery.

Abstract translation: 本发明提供了制备大尺寸钛硅质分子筛的方法，以及使用大尺寸钛 - 硅沸石分子筛制备环己酮肟的方法。 制备大尺寸钛硅质岩分子筛的方法包括制备钛源，硅源和模板剂的混合物; 加热混合物以形成凝胶混合物; 将胶体二氧化硅与凝胶混合物混合; 在水浴中加热与胶体二氧化硅混合的凝胶混合物; 并煅烧与胶体二氧化硅混合的凝胶混合物。 在本发明中，大型钛硅分子筛的平均粒径为10μm以上，粒径分布集中，避免了钛 - 氧 - 钛键合的形成。 使用大尺寸钛 - 硅质分子筛制备环己酮肟的方法导致高转化率，高选择性和容易回收。

公开(公告)号：US20130041181A1

公开(公告)日：2013-02-14

申请号：US13350045

申请日：2012-01-13

Applicant: Ya-Ping Chen ,  Cheng-Fa Hsieh ,  Pin-To Yao ,  Chien-Chang Chiang

Inventor： Ya-Ping Chen ,  Cheng-Fa Hsieh ,  Pin-To Yao ,  Chien-Chang Chiang

IPC: B01J29/89 ,  C07C249/04

CPC classification number: C07C249/04 ,  B01J29/89 ,  B01J2229/183 ,  C01B37/005 ,  C07C2601/14 ,  C07C251/44

Abstract: The present invention provides a titanium-silicalite molecular sieve and a method for preparing the same. The method includes the steps of preparing a mixture of a titanium source, a silicon source, a metal source selected from IIA to IVA elements and a template agent; heating the mixture to form a gel mixture; heating the gel mixture in a water bath; and calcining the gel mixture after the gel mixture in the water bath to form the titanium-silicalite molecular sieve. The present invention further provides a method for preparing cyclohexanone oxime by using the titanium-silicalite molecular sieve as the catalyst which results in high conversion rate, high selectivity and high usage efficiency of hydrogen peroxide.

Abstract translation: 本发明提供钛 - 硅沸石分子筛及其制备方法。 该方法包括以下步骤：制备钛源，硅源，选自IIA至IVA元素的金属源和模板剂的混合物; 加热混合物以形成凝胶混合物; 在水浴中加热凝胶混合物; 并在凝胶混合物中在水浴中煅烧凝胶混合物以形成钛 - 硅沸石分子筛。 本发明还提供了通过使用钛 - 硅沸石分子筛作为催化剂制备环己酮肟的方法，其导致过氧化氢的高转化率，高选择性和高使用效率。

公开(公告)号：US20120209029A1

公开(公告)日：2012-08-16

申请号：US13344869

申请日：2012-01-06

Applicant: Shih-Yao CHAO ,  Cheng-Fa HSIEH ,  Chien-Chang CHIANG ,  Ya-Ping CHEN ,  Pin-To YAO

Inventor： Shih-Yao CHAO ,  Cheng-Fa HSIEH ,  Chien-Chang CHIANG ,  Ya-Ping CHEN ,  Pin-To YAO

IPC: B01J29/89 ,  C07C249/04

CPC classification number: B01J29/89 ,  B01J35/023 ,  C01B37/005 ,  C07C249/04 ,  C07C251/44

Abstract: The present invention provides a method for preparing a large-sized titanium-silicalite molecular sieve, and a method for preparing cyclohexanone oxime using the large-sized titanium-silicalite molecular sieve. The method for preparing a large-sized titanium-silicalite molecular sieve includes preparing a mixture of a titanium source, a silicon source and a template agent; heating the mixture to form a gel mixture; mixing a colloidal silica with the gel mixture; heating the gel mixture mixed with the colloidal silica in a water bathe; and calcining the gel mixture mixed with the colloidal silica. In the present invention, the average particle size of the large-sized titanium-silicalite molecular sieve is more than 10 um, and the particle size distribution is centralized, so as to avoid the formation of titanium-oxygen-titanium bonding. The method for preparing cyclohexanone oxime using the large-sized titanium-silicalite molecular sieve results in high conversion rate, high selectivity and easy recovery.

Abstract translation: 本发明提供了制备大尺寸钛硅质分子筛的方法，以及使用大尺寸钛 - 硅沸石分子筛制备环己酮肟的方法。 制备大尺寸钛硅质岩分子筛的方法包括制备钛源，硅源和模板剂的混合物; 加热混合物以形成凝胶混合物; 将胶体二氧化硅与凝胶混合物混合; 在水浴中加热与胶体二氧化硅混合的凝胶混合物; 并煅烧与胶体二氧化硅混合的凝胶混合物。 在本发明中，大型钛硅分子筛的平均粒径大于10μm，粒径分布集中，以避免钛 - 氧 - 钛键合的形成。 使用大尺寸钛 - 硅质分子筛制备环己酮肟的方法导致高转化率，高选择性和容易回收。