公开(公告)号：US08772194B2

公开(公告)日：2014-07-08

申请号：US13344869

申请日：2012-01-06

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

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

IPC分类号： B01J29/89 ,  C07C249/04

CPC分类号： B01J29/89 ,  B01J35/023 ,  C01B37/005 ,  C07C249/04 ,  C07C251/44

摘要： 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.

摘要翻译： 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：US08753998B2

公开(公告)日：2014-06-17

申请号：US13344995

申请日：2012-01-06

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

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

IPC分类号： B01J21/06 ,  C07C249/04

CPC分类号： C01B37/005 ,  B01J29/035 ,  C07C249/04 ,  C07C251/44

摘要： 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 bath; 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.

摘要翻译： 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：US20120271066A1

公开(公告)日：2012-10-25

申请号：US13344995

申请日：2012-01-06

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

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

IPC分类号： B01J21/06 ,  C07C249/04

CPC分类号： C01B37/005 ,  B01J29/035 ,  C07C249/04 ,  C07C251/44

摘要： 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.

摘要翻译： 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：US20120277468A1

公开(公告)日：2012-11-01

申请号：US13345089

申请日：2012-01-06

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

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

IPC分类号： B01J21/06 ,  C07C249/04

CPC分类号： C01B37/005 ,  B01J29/89 ,  C01B39/085 ,  C01B39/087 ,  C07C249/04 ,  C07C251/44

摘要： 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.

摘要翻译： 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：US09434683B2

公开(公告)日：2016-09-06

申请号：US13350045

申请日：2012-01-13

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

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

IPC分类号： C01B37/00 ,  C07C249/04 ,  B01J29/89

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

摘要： 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.

摘要翻译： 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，选自IIA至IVA元素的金属源和模板剂的混合物的步骤; 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：US09371238B2

公开(公告)日：2016-06-21

申请号：US13345089

申请日：2012-01-06

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

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

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

CPC分类号： C01B37/005 ,  B01J29/89 ,  C01B39/085 ,  C01B39/087 ,  C07C249/04 ,  C07C251/44

摘要： 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.

摘要翻译： 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：US20130041181A1

公开(公告)日：2013-02-14

申请号：US13350045

申请日：2012-01-13

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

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

IPC分类号： B01J29/89 ,  C07C249/04

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

摘要： 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.

摘要翻译： 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：US08540956B2

公开(公告)日：2013-09-24

申请号：US12748932

申请日：2010-03-29

申请人： Pin-To Yao ,  Cheng-Fa Hsieh ,  Shih-Yao Chao ,  Yang-Min Liang

发明人： Pin-To Yao ,  Cheng-Fa Hsieh ,  Shih-Yao Chao ,  Yang-Min Liang

IPC分类号： C01B39/02 ,  C01B39/04

CPC分类号： C01B39/023 ,  B01J29/405 ,  C01B37/005 ,  C01B39/04

摘要： The present invention provides a method for preparing large particles of titanium-silicalite molecular sieves. The method of the present invention includes the steps of preparing a dispersion solution of a primary crystalline molecular sieve; forming an aggregated particle solution by adding a flocculating agent and a coagulating agent into the dispersion solution; mixing the aggregated particle solution with a synthesis gel to form a mixture; and heat-treating the mixture. The average diameter of the titanium-silicalite molecular sieves in the present invention is more than 5 μm. In the preparation of cyclohexanone oxime using the molecular sieve of the present invention as the catalyst, the selectivity and conversion rate of cyclohexanone oxime are high, the usage of hydrogen peroxide is enhanced, and the catalyst is easy to be recovered.

摘要翻译： 本发明提供一种制备钛 - 硅沸石分子筛大颗粒的​​方法。 本发明的方法包括制备一级结晶分子筛的分散液的步骤; 通过向分散液中添加絮凝剂和凝结剂形成凝集颗粒溶液; 将聚集的颗粒溶液与合成凝胶混合以形成混合物; 并对该混合物进行热处理。 本发明中钛 - 硅沸石分子筛的平均直径大于5μm。 在使用本发明的分子筛作为催化剂的环己酮肟的制备中，环己酮肟的选择性和转化率高，过氧化氢的用途增加，催化剂容易回收。

公开(公告)号：US20110144328A1

公开(公告)日：2011-06-16

申请号：US12748932

申请日：2010-03-29

申请人： Pin-To Yao ,  Cheng-Fa Hsieh ,  Shih-Yao Chao ,  Yang-Min Liang

发明人： Pin-To Yao ,  Cheng-Fa Hsieh ,  Shih-Yao Chao ,  Yang-Min Liang

IPC分类号： C07D223/10 ,  B01J29/89

CPC分类号： C01B39/023 ,  B01J29/405 ,  C01B37/005 ,  C01B39/04

摘要： The present invention provides a method for preparing large particles of titanium-silicalite molecular sieves. The method of the present invention includes the steps of preparing a dispersion solution of a primary crystalline molecular sieve; forming an aggregated particle solution by adding a flocculating agent and a coagulating agent into the dispersion solution; mixing the aggregated particle solution with a synthesis gel to form a mixture; and heat-treating the mixture. The average diameter of the titanium-silicalite molecular sieves in the present invention is more than 5 μm. In the preparation of cyclohexanone oxime using the molecular sieve of the present invention as the catalyst, the selectivity and conversion rate of cyclohexanone oxime are high, the usage of hydrogen peroxide is enhanced, and the catalyst is easy to be recovered.

摘要翻译： 本发明提供一种制备钛 - 硅沸石分子筛大颗粒的​​方法。 本发明的方法包括制备一级结晶分子筛的分散液的步骤; 通过向分散液中添加絮凝剂和凝结剂形成凝集颗粒溶液; 将聚集的颗粒溶液与合成凝胶混合以形成混合物; 并对该混合物进行热处理。 本发明中钛 - 硅沸石分子筛的平均直径大于5μm。 在使用本发明的分子筛作为催化剂的环己酮肟的制备中，环己酮肟的选择性和转化率高，过氧化氢的用途增加，催化剂容易回收。

公开(公告)号：US08524895B2

公开(公告)日：2013-09-03

申请号：US12501699

申请日：2009-07-13

申请人： Tung-Han Tsai ,  Pin-To Yao ,  Cheng-Fa Hsieh

发明人： Tung-Han Tsai ,  Pin-To Yao ,  Cheng-Fa Hsieh

IPC分类号： C07D201/04 ,  C07D223/10

CPC分类号： C07D201/04 ,  C07D223/10

摘要： The present invention provides a method for preparing amides, in which an amino acid ionic liquid is used as both a reaction medium and a catalyst to catalyze Beckman rearrangement of a ketoxime, so as to produce an amide. In the method, the rearrangement is conducted by catalyzing a ketoxime with an amino acid ionic liquid having the asymmetric property at a moderate reaction temperature during a short reaction time, so as to produce an amide without adding other catalysts such as concentrate sulfuric acid. The method has advantages such as avoiding corrosion in equipments with pipelines, the high conversion rate of ketoximes and the high selectivity of amides.

摘要翻译： 本发明提供了一种制备酰胺的方法，其中使用氨基酸离子液体作为反应介质和催化贝克曼重排酮肟的催化剂，以产生酰胺。 在该方法中，通过在短的反应时间内在适度的反应温度下用具有不对称性质的氨基酸离子液体催化酮肟进行重排，从而在不加入其它催化剂如浓硫酸的情况下生成酰胺。 该方法具有避免管道设备腐蚀，酮肟转化率高，酰胺选择性高等优点。