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1. 发明授权

US08673073B2 Methods for purifying metallurgical silicon 有权
标题翻译：纯化冶金硅的方法
公开(公告)号：US08673073B2
公开(公告)日：2014-03-18
申请号：US13541319
申请日：2012-07-03
申请人： Masahiro Hoshino , Cheng C. Kao
发明人： Masahiro Hoshino , Cheng C. Kao
IPC分类号： C30B28/04
CPC分类号： C01B33/037 , H01L31/182 , Y02E10/546 , Y02P70/521
摘要： A method for purifying silicon bearing materials for photovoltaic applications includes providing metallurgical silicon into a crucible apparatus. The metallurgical silicon is subjected to at least a thermal process to cause the metallurgical silicon to change in state from a first state to a second state, the second stage being a molten state not exceeding 1500 Degrees Celsius. At least a first portion of impurities is caused to be removed from the metallurgical silicon in the molten state. The molten metallurgical silicon is cooled from a lower region to an upper region to cause the lower region to solidify while a second portion of impurities segregate and accumulate in a liquid state region. The liquid state region is solidified to form a resulting silicon structure having a purified region and an impurity region. The purified region is characterized by a purity of greater than 99.9999%.
摘要翻译：用于光电应用的用于纯化硅轴承材料的方法包括将冶金硅提供到坩埚装置中。对冶金硅进行至少一个热处理，使冶金硅从第一状态转变到第二状态，第二阶段是不超过1500摄氏度的熔融状态。使至少第一部分杂质从熔融状态的冶金硅中除去。熔融冶金硅从下部区域冷却到上部区域，导致下部区域固化，而第二部分杂质在液态区域中分离并积聚。液态区域被固化，形成具有纯化区域和杂质区域的所得硅结构。纯化区的特征在于纯度大于99.9999％。

2. 发明授权

US08501140B2 Method and apparatus for purifying metallurgical silicon for solar cells 有权
标题翻译：用于净化太阳能电池的冶金硅的方法和装置
公开(公告)号：US08501140B2
公开(公告)日：2013-08-06
申请号：US13536919
申请日：2012-06-28
申请人： Masahiro Hoshino , Cheng C. Kao
发明人： Masahiro Hoshino , Cheng C. Kao
IPC分类号： C01B33/021
CPC分类号： C01B33/037 , H01L31/182 , Y02E10/546 , Y02P70/521
摘要： A method improves yield of an upgraded metallurgical-grade (UMG) silicon purification process. In the UMG silicon purification process, in a reaction chamber, purification is performed on a silicon melt therein by one, all or a plurality of the following techniques in the same apparatus at the same time. The techniques includes a crucible ratio approach, the addition of water-soluble substances, the control of power, the control of vacuum pressure, the upward venting of exhaust, isolation by high-pressure gas jet, and carbon removal by sandblasting, thereby reducing oxygen, carbon and other impurities in the silicon melt, meeting a high-purity silicon standard of solar cells, increasing yield while maintaining low cost, and avoiding EMF reduction over time. An exhaust venting device for the purification process allows exhaust to be vented from the top of the reactor chamber, thereby avoiding backflow of exhaust into the silicon melt and erosion of the reactor.
摘要翻译：一种方法提高了升级冶金级（UMG）硅纯化工艺的产量。在UMG硅纯化方法中，在反应室中，在同一装置中同时进行一种，全部或多种以下技术的硅熔体的纯化。该技术包括坩埚比方法，水溶性物质的添加，功率的控制，真空压力的控制，排气的向上排气，高压气体喷射的隔离以及通过喷砂除碳，从而减少氧气，硅熔体中的碳和其他杂质，满足太阳能电池的高纯硅标准，提高产量，同时保持低成本，并避免随着时间的推移EMF减少。用于净化过程的排气装置允许排气从反应器室的顶部排出，从而避免排入硅熔体的回流和反应器的侵蚀。

3. 发明申请

US20120275985A1 METHOD FOR PURIFYING METALLURGICAL SILICON FOR SOLAR CELLS 有权
标题翻译：纯化用于太阳能电池的冶金硅的方法
公开(公告)号：US20120275985A1
公开(公告)日：2012-11-01
申请号：US13539183
申请日：2012-06-29
申请人： Masahiro HOSHINO , Cheng C. KAO
发明人： Masahiro HOSHINO , Cheng C. KAO
IPC分类号： C01B33/037
CPC分类号： C01B33/037 , C30B11/002 , C30B11/003 , C30B29/06 , F27B14/06 , F27B14/14 , H05B7/18
摘要： A method includes transferring a raw silicon material in a crucible and subjecting the raw silicon material in the crucible to thermal energy to form a melted silicon material at a temperature of less than 1400 Degrees Celsius, the melted silicon material having an exposed region bounded by an interior region of the crucible, subjecting an exposed inner region of the melted silicon material to an energy source to include an arc heater configured above the exposed region and to be spaced by a gap between the exposed region and a muzzle region of the arc heater to form a determined temperature profile within a vicinity of an inner region of the exposed melted silicon material while maintaining outer regions of the melted silicon material at a temperature below a melting point of the crucible, and removing impurities from the melted silicon material to form higher purity silicon.
摘要翻译：一种方法包括将原料硅材料转移到坩埚中，并使坩埚中的原料硅材料在低于1400摄氏度的温度下进行热能以形成熔融的硅材料，熔融的硅材料具有由坩埚的内部区域，将熔融的硅材料的暴露的内部区域经受能量源包括配置在暴露区域之上的电弧加热器，并且被间隔开，该电弧加热器暴露区域与电弧加热器的枪口区域之间的间隙在暴露的熔融硅材料的内部区域的附近形成确定的温度曲线，同时保持熔融的硅材料的外部区域处于低于坩埚的熔点的温度，并且从熔融的硅材料中除去杂质以形成更高的纯度硅。

4. 发明授权

US08257492B2 Methods for purifying metallurgical silicon 有权
标题翻译：纯化冶金硅的方法
公开(公告)号：US08257492B2
公开(公告)日：2012-09-04
申请号：US12947777
申请日：2010-11-16
申请人： Masahiro Hoshino , Cheng C. Kao
发明人： Masahiro Hoshino , Cheng C. Kao
IPC分类号： C30B28/00
CPC分类号： C01B33/037 , H01L31/182 , Y02E10/546 , Y02P70/521
摘要： A method for purifying silicon bearing materials for photovoltaic applications includes providing metallurgical silicon into a crucible apparatus. The metallurgical silicon is subjected to at least a thermal process to cause the metallurgical silicon to change in state from a first state to a second state, the second stage being a molten state not exceeding 1500 Degrees Celsius. At least a first portion of impurities is caused to be removed from the metallurgical silicon in the molten state. The molten metallurgical silicon is cooled from a lower region to an upper region to cause the lower region to solidify while a second portion of impurities segregate and accumulate in a liquid state region. The liquid state region is solidified to form a resulting silicon structure having a purified region and an impurity region. The purified region is characterized by a purity of greater than 99.9999%.
摘要翻译：用于光电应用的用于纯化硅轴承材料的方法包括将冶金硅提供到坩埚装置中。对冶金硅进行至少一个热处理，使冶金硅从第一状态转变到第二状态，第二阶段是不超过1500摄氏度的熔融状态。使至少第一部分杂质从熔融状态的冶金硅中除去。熔融冶金硅从下部区域冷却到上部区域，导致下部区域固化，而第二部分杂质在液态区域中分离并积聚。液态区域被固化，形成具有纯化区域和杂质区域的所得硅结构。纯化区的特征在于纯度大于99.9999％。

5. 发明授权

US08236265B2 Method for purifying metallurgical silicon for solar cells 有权
标题翻译：纯化太阳能电池冶金硅的方法
公开(公告)号：US08236265B2
公开(公告)日：2012-08-07
申请号：US13024292
申请日：2011-02-09
申请人： Masahiro Hoshino , Cheng C. Kao
发明人： Masahiro Hoshino , Cheng C. Kao
IPC分类号： C01B33/02 , C01B33/021
CPC分类号： C01B33/037 , C30B11/002 , C30B11/003 , C30B29/06 , F27B14/06 , F27B14/14 , H05B7/18
摘要： The present invention provides a method for forming high quality silicon material, e.g., polysilicon. The method includes transferring a raw silicon material in a crucible having an interior region. The crucible is made of a quartz or other suitable material, which is capable of withstanding a temperature of at least 1400 Degrees Celsius. The method includes subjecting the raw silicon material in the crucible to thermal energy to cause the raw silicon material to be melted into a liquid state to form a melted material at a temperature of less than about 1400 Degrees Celsius. Preferably, the melted material has an exposed region bounded by the interior region of the crucible. The method also includes subjecting an exposed inner region of the melted material to an energy source comprising an arc heater configured above the exposed region and spaced by a gap between the exposed region and a muzzle region of the arc heater to cause formation of determined temperature profile within a vicinity of an inner region of the exposed melted material while maintaining outer regions of the melted material at a temperature below a melting point of the quartz material of the crucible. Preferably, the method removes one or more impurities from the melted material to form a higher purity silicon material in the crucible.
摘要翻译：本发明提供了形成高质量硅材料（例如多晶硅）的方法。该方法包括将原料硅转移到具有内部区域的坩埚中。坩埚由石英或其他合适的材料制成，其能够承受至少1400摄氏度的温度。该方法包括使坩埚中的原料硅经受热能，使原料硅熔化成液态，以在小于约1400摄氏度的温度下形成熔融材料。优选地，熔融的材料具有由坩埚的内部区域限定的暴露区域。该方法还包括使熔融材料的暴露的内部区域经受能量源，该能量源包括配置在暴露区域之上并由暴露区域和电弧加热器的枪口区域之间的间隙隔开的电弧加热器以形成确定的温度曲线在暴露的熔融材料的内部区域的附近，同时保持熔融材料的外部区域处于低于坩埚的石英材料的熔点的温度。优选地，该方法从熔融材料中除去一种或多种杂质，以在坩埚中形成更高纯度的硅材料。

6. 发明授权

US07709685B2 Method for producing cycloalkanol and/or cycloalkanone 失效
标题翻译：环烷醇和/或环烷酮的制备方法
公开(公告)号：US07709685B2
公开(公告)日：2010-05-04
申请号：US12048258
申请日：2008-03-14
申请人： Masahiro Hoshino , Tatsuya Suzuki , Hajime Ishida
发明人： Masahiro Hoshino , Tatsuya Suzuki , Hajime Ishida
IPC分类号： C07C45/32 , C07C35/08
CPC分类号： C07C29/50 , B01J23/22 , B01J23/26 , B01J23/34 , B01J23/44 , B01J23/462 , B01J23/745 , B01J23/75 , B01J29/0308 , B01J29/041 , B01J37/0209 , B01J2229/32 , C07C45/33 , C07C2601/14 , C07C49/403 , C07C35/08
摘要： An object of the present invention is to provide a method capable of producing cycloalkanol and/or cycloalkanone with a favorable selectivity by oxidizing cycloalkane with a favorable conversion.A cycloalkanol and/or cycloalkanone are produced by oxidizing cycloalkane with oxygen in the presence of mesoporous silica which contains at least one metal selected from metals of Groups 5 to 10 of the Periodic Table and which is also subjected to a contact treatment with an organosilicon compound. The metal is preferably at least one metal selected from the group consisting of vanadium, chromium, manganese, iron, cobalt, ruthenium and palladium, and the mesoporous silica is preferably MCM-41 type mesoporous silica.
摘要翻译：本发明的目的是提供一种通过以良好的转化率氧化环烷烃，以良好的选择性制备环烷醇和/或环烷酮的方法。在含有至少一种选自元素周期表第5至10族金属的金属的介孔二氧化硅的存在下，用氧氧化环烷烃并且还与有机硅化合物进行接触处理来制备环烷醇和/或环烷酮。金属优选为选自钒，铬，锰，铁，钴，钌和钯中的至少一种金属，并且介孔二氧化硅优选为MCM-41型中孔二氧化硅。

7. 发明申请

US20090227814A1 METHOD FOR PRODUCING CYCLOALKANOL AND/OR CYCLOALKANONE 失效
标题翻译：生产环烷醇和/或环烷酮的方法
公开(公告)号：US20090227814A1
公开(公告)日：2009-09-10
申请号：US12392122
申请日：2009-02-25
申请人： Masahiro HOSHINO , Nobufumi Watanabe , Keisuke Sugita
发明人： Masahiro HOSHINO , Nobufumi Watanabe , Keisuke Sugita
IPC分类号： C07C35/08 , C07C45/33
CPC分类号： B01J35/1061 , B01J23/38 , B01J23/70 , B01J23/75 , B01J29/0308 , B01J35/1023 , B01J35/1028 , B01J37/0018 , B01J37/033 , B01J37/10 , B01J2229/32 , C07C29/50 , C07C45/33 , C07C2601/14 , C07C35/08 , C07C49/403
摘要： An object of the present invention is to provide a method capable of producing a cycloalkanol and/or a cycloalkanone with a favorable selectivity coefficient by oxidizing a cycloalkane with a favorable conversion ratio.Disclosed is a method for producing a cycloalkanol and/or a cycloalkanone, which comprises oxidizing a cycloalkane with oxygen in the presence of a mesoporous silica which contains at least one transition metal and has been also subjected to contact treatment with an amine and/or ammonia. Preferably, a crystal obtained by mixing a compound containing the metal, a silicon compound, a structure-directing agent and water is subjected to contact treatment with an amine and/or ammonia and then fired to obtain a mesoporous silica, and a cycloalkane is oxidized with oxygen in the presence of the mesoporous silica.
摘要翻译：本发明的目的是提供一种通过以良好的转化率氧化环烷烃，能够制备具有良好选择性系数的环烷醇和/或环烷酮的方法。公开了一种制备环烷醇和/或环烷酮的方法，其包括在含有至少一种过渡金属的介孔二氧化硅的存在下用氧氧化环烷烃，并且还已经用胺和/或氨进行接触处理。优选将通过混合含有金属，硅化合物，结构导向剂和水的化合物得到的晶体与胺和/或氨进行接触处理，然后烧制以获得介孔二氧化硅，并且环烷烃被氧化在介孔二氧化硅存在下用氧气。

8. 发明申请

US20090036714A1 PROCESS FOR PRODUCING CYCLOALKANOL AND/OR CYCLOALKANONE 失效
标题翻译：生产环烷醇和/或环烷酮的方法
公开(公告)号：US20090036714A1
公开(公告)日：2009-02-05
申请号：US12184461
申请日：2008-08-01
申请人： Masahiro HOSHINO , Nobufumi Watanabe
发明人： Masahiro HOSHINO , Nobufumi Watanabe
IPC分类号： C07C45/27 , C07C35/08
CPC分类号： C07C29/50 , B01J29/0333 , B01J35/0066 , B01J2229/32 , C07C45/33 , C07C2601/14 , C12C11/02 , C07C35/08 , C07C49/403
摘要： An object of the present invention is to provide a process capable of producing cycloalkanol and/or cycloalkanone with a favorable selectivity by oxidizing cycloalkane with a favorable conversion.Disclosed is a process for producing cycloalkanol and/or cycloalkanone, which comprises oxidizing cycloalkane with oxygen in the presence of mesoporous silica, wherein (1) the mesoporous silica contains at least one transition metal, and (2) a ratio of total volume of mesoporous silica particles having a particle diameter of 20 μm or less to total volume of entire mesoporous silica particles is 25% or more in the mesoporous silica.
摘要翻译：本发明的目的是提供一种通过以良好的转化率氧化环烷烃，以良好的选择性制备环烷醇和/或环烷酮的方法。公开了一种制备环烷醇和/或环烷酮的方法，其包括在介孔二氧化硅存在下用氧氧化环烷烃，其中（1）介孔二氧化硅含有至少一种过渡金属，和（2）介孔中的总体积比在介孔二氧化硅中，粒径为20μm以下的二氧化硅粒子的总体积的总体积为25％以上。

9. 发明申请

US20080228007A1 METHOD FOR PRODUCING CYCLOALKANOL AND/OR CYCLOALKANONE 失效
标题翻译：生产环烷醇和/或环烷酮的方法
公开(公告)号：US20080228007A1
公开(公告)日：2008-09-18
申请号：US12048258
申请日：2008-03-14
申请人： Masahiro HOSHINO , Tatsuya Suzuki , Hajime Ishida
发明人： Masahiro HOSHINO , Tatsuya Suzuki , Hajime Ishida
IPC分类号： C07C45/32
CPC分类号： C07C29/50 , B01J23/22 , B01J23/26 , B01J23/34 , B01J23/44 , B01J23/462 , B01J23/745 , B01J23/75 , B01J29/0308 , B01J29/041 , B01J37/0209 , B01J2229/32 , C07C45/33 , C07C2601/14 , C07C49/403 , C07C35/08
摘要： An object of the present invention is to provide a method capable of producing cycloalkanol and/or cycloalkanone with a favorable selectivity by oxidizing cycloalkane with a favorable conversion.A cycloalkanol and/or cycloalkanone are produced by oxidizing cycloalkane with oxygen in the presence of mesoporous silica which contains at least one metal selected from metals of Groups 5 to 10 of the Periodic Table and which is also subjected to a contact treatment with an organosilicon compound. The metal is preferably at least one metal selected from the group consisting of vanadium, chromium, manganese, iron, cobalt, ruthenium and palladium, and the mesoporous silica is preferably MCM-41 type mesoporous silica.
摘要翻译：本发明的目的是提供一种通过以良好的转化率氧化环烷烃，以良好的选择性制备环烷醇和/或环烷酮的方法。在含有至少一种选自元素周期表第5至10族金属的金属的介孔二氧化硅的存在下，用氧氧化环烷烃并且还与有机硅化合物进行接触处理来制备环烷醇和/或环烷酮。金属优选为选自钒，铬，锰，铁，钴，钌和钯中的至少一种金属，并且介孔二氧化硅优选为MCM-41型介孔二氧化硅。

10. 发明申请

US20060004194A1 Method for manufacturing zeolite and method for manufacturing epsilon-caprolatam 失效
标题翻译：制造沸石的方法和制备ε-caprolatam的方法
公开(公告)号：US20060004194A1
公开(公告)日：2006-01-05
申请号：US11165538
申请日：2005-06-24
申请人： Masahiro Hoshino , Masaru Kitamura , Keisuke Sugita
发明人： Masahiro Hoshino , Masaru Kitamura , Keisuke Sugita
IPC分类号： B01J29/40 , C07D201/04
CPC分类号： C07D201/04 , B01J29/035 , B01J37/06 , B01J2229/38 , B01J2229/40 , C01B37/02
摘要： The present invention provides a method for manufacturing a zeolite comprising following steps of: (1): calcining crystals obtained by hydrothermal synthesis reaction of a silicon compound; (2): contact treating a calcined product obtained by the step (1) with an aqueous solution including an amine and/or a quaternary ammonium compound; (3): calcining a treated product obtained by the step (2); and (4): contact treating the calcined product obtained by the step (3) with an aqueous solution including ammonia and/or an ammonium salt. According to the present invention, a method is also provided wherein ε-caprolactam is manufactured by Beckmann rearrangement reaction of cyclohexanone oxime in a gaseous phase in the presence of the zeolite manufactured by the above-described method.
摘要翻译：本发明提供一种制造沸石的方法，包括以下步骤：（1）：煅烧通过硅化合物的水热合成反应获得的晶体; （2）：用包含胺和/或季铵化合物的水溶液接触步骤（1）得到的煅烧产物; （3）：煅烧通过工序（2）得到的处理物; 和（4）：用包含氨和/或铵盐的水溶液接触处理由步骤（3）获得的煅烧产物。根据本发明，还提供了一种方法，其中ε-己内酰胺通过在通过上述方法制造的沸石存在下，在气相中通过环己酮肟的贝克曼重排反应制造。

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