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    Lithium-porous metal oxide compositions and lithium reagent-porous metal compositions
    1.
    发明授权
    Lithium-porous metal oxide compositions and lithium reagent-porous metal compositions 有权
    锂多孔金属氧化物组合物和锂试剂多孔金属组合物

    公开(公告)号：US08197707B2

    公开(公告)日：2012-06-12

    申请号：US11852820

    申请日：2007-09-10

    申请人： Michael Lefenfeld ,  James L. Dye ,  Partha Nandi ,  James Jackson

    发明人： Michael Lefenfeld ,  James L. Dye ,  Partha Nandi ,  James Jackson

    IPC分类号： H01M4/58 ,  B05D5/12

    CPC分类号： C07F1/02 ,  C01C1/026 ,  C01D15/00 ,  C01P2002/86 ,  C01P2002/87 ,  C01P2002/89 ,  C01P2006/16 ,  Y02P20/52

    摘要： The invention relates to lithium metal/porous metal oxide compositions. These lithium metal compositions are prepared by mixing liquid lithium metal with a porous metal oxide in an inert atmosphere under exothermic conditions sufficient to absorb the liquid lithium metal into the porous metal oxide pores. The lithium metal/porous metal oxide compositions of the invention are preferably loaded with lithium metal up to about 40% by weight, with about 20% to 40% by weight being the most preferred loading. The invention also relates to lithium reagent-porous metal oxide compositions having RLi absorbed into a porous oxide. The preparation and use of these compositions are also described.

    摘要翻译： 本发明涉及锂金属/多孔金属氧化物组合物。 这些锂金属组合物通过在惰性气氛中将液态锂金属与多孔金属氧化物混合，在足以将液态锂金属吸收到多孔金属氧化物孔中的放热条件下来制备。 本发明的锂金属/多孔金属氧化物组合物优选负载高达约40重量％的锂金属，其中最优选的负载量为约20重量％至40重量％。 本发明还涉及具有吸收到多孔氧化物中的RLi的锂试剂多孔金属氧化物组合物。 还描述了这些组合物的制备和用途。

    Silicide compositions containing alkali metals and methods of making the same
    2.
    发明授权
    Silicide compositions containing alkali metals and methods of making the same 有权
    含有碱金属的硅化物组合物及其制备方法

    公开(公告)号：US08986643B2

    公开(公告)日：2015-03-24

    申请号：US13445557

    申请日：2012-04-12

    申请人： Michael Lefenfeld ,  James L. Dye

    发明人： Michael Lefenfeld ,  James L. Dye

    IPC分类号： C01B3/06 ,  C01B3/08 ,  C01B33/06

    CPC分类号： C11D7/04 ,  C01B3/06 ,  C01B3/08 ,  C01B33/06 ,  C11D17/042 ,  F24V30/00 ,  Y02E60/364

    摘要： The invention relates to a method of making alkali metal silicide compositions, and the compositions resulting from the method, comprising mixing an alkali metal with silicon and heating the resulting mixture to a temperature below about 475° C. The resulting compositions do not react with dry O2. Also, the invention relates to sodium silicide compositions having a powder X-ray diffraction pattern comprising at least three peaks with 2Theta angles selected from about 18.2, 28.5, 29.5, 33.7, 41.2, 47.4, and 56.2 and a solid state 23Na MAS NMR spectra peak at about 18 ppm. Moreover, the invention relates to methods of removing a volatile or flammable substance in a controlled manner. Furthermore, the alkali metal silicide compositions of the invention react with water to produce hydrogen gas.

    摘要翻译： 本发明涉及一种制备碱金属硅化物组合物的方法和由该方法得到的组合物，其包括将碱金属与硅混合并将所得混合物加热至低于约475℃的温度。所得组合物不与干 O2。 此外，本发明涉及具有粉末X射线衍射图的硅化钠组合物，其包含至少三个具有选自约18.2,28.5,29.5,33.7,41.2,47.4和56.2的2θ角的峰和固态23Na MAS NMR光谱 峰值约为18ppm。 此外，本发明涉及以受控方式除去挥发性或易燃物质的方法。 此外，本发明的碱金属硅化物组合物与水反应产生氢气。

    SILICA GEL COMPOSITIONS CONTAINING ALKALI METALS AND ALKALI METAL ALLOYS
    3.
    发明申请
    SILICA GEL COMPOSITIONS CONTAINING ALKALI METALS AND ALKALI METAL ALLOYS 有权
    含有碱金属和碱金属合金的二氧化硅凝胶组合物

    公开(公告)号：US20100166648A1

    公开(公告)日：2010-07-01

    申请号：US12723588

    申请日：2010-03-12

    申请人： Michael LEFENFELD ,  James L. Dye

    发明人： Michael LEFENFELD ,  James L. Dye

    IPC分类号： C01B3/08 ,  C07C15/28 ,  C07C1/00

    CPC分类号： B01J35/002 ,  B01J20/02 ,  B01J20/103 ,  B01J20/28047 ,  B01J20/28078 ,  B01J20/28097 ,  B01J20/281 ,  B01J20/291 ,  B01J20/3078 ,  B01J20/3204 ,  B01J20/3236 ,  B01J23/04 ,  B01J37/023 ,  B01J37/08 ,  B01J2220/42 ,  B01J2220/54 ,  B01J2220/56 ,  B01J2220/58 ,  C01B3/001 ,  C01B3/06 ,  C07C2/861 ,  C07C2/868 ,  C07D333/76 ,  Y02E60/324 ,  Y02E60/36 ,  C07C15/18 ,  C07C15/14

    摘要： The invention relates to Group 1 metal/silica gel compositions comprising silica gel and an alkali metal or alloy, wherein Group 1 metals or alloys are absorbed into the silica gel pores. The invention relates to producing hydrogen gas comprising contacting a Group 1 metal/silica gel composition with water, and further relates to an alkali metal reduction of an organic compound, the improvement comprising contacting the organic compound with a Group 1 metal/silica gel composition. In these embodiments, the Group 1 metal/silica gel composition reacts with dry O2. The invention also relates to producing hydrogen gas comprising contacting a Group 1 metal/silica gel composition with water, and further relates to an alkali metal reduction of an organic compound, the improvement comprising contacting the organic compound with a Group 1 metal/silica gel composition. In these embodiments, the Group 1 metal/silica gel composition produced does not react with dry O2.

    摘要翻译： 本发明涉及包含硅胶和碱金属或合金的第1族金属/硅胶组合物，其中第1族金属或合金被吸收到硅胶孔中。 本发明涉及生产氢气，包括使第1族金属/硅胶组合物与水接触，还涉及有机化合物的碱金属还原，其改进包括使有机化合物与第1族金属/硅胶组合物接触。 在这些实施方案中，第1族金属/硅胶组合物与干燥的O 2反应。 本发明还涉及生产氢气，包括使第1族金属/硅胶组合物与水接触，还涉及有机化合物的碱金属还原，其改进包括使有机化合物与第1族金属/硅胶组合物 。 在这些实施方案中，所生产的第1族金属/硅胶组合物不与干燥的O 2反应。

    Silicide compositions containing alkali metals and methods of making the same
    5.
    发明授权
    Silicide compositions containing alkali metals and methods of making the same 有权

    公开(公告)号：US08372371B2

    公开(公告)日：2013-02-12

    申请号：US12854510

    申请日：2010-08-11

    申请人： Michael Lefenfeld ,  James L. Dye

    发明人： Michael Lefenfeld ,  James L. Dye

    IPC分类号： C01B33/06 ,  B01J21/00

    CPC分类号： C11D7/04 ,  C01B3/06 ,  C01B3/08 ,  C01B33/06 ,  C11D17/042 ,  F24V30/00 ,  Y02E60/364

    摘要： The invention relates to a method of making alkali metal silicide compositions, and the compositions resulting from the method, comprising mixing an alkali metal with silicon and heating the resulting mixture to a temperature below about 475° C. The resulting compositions do not react with dry O2. Also, the invention relates to sodium silicide compositions having a powder X-ray diffraction pattern comprising at least three peaks with 2Theta angles selected from about 18.2, 28.5, 29.5, 33.7, 41.2, 47.4, and 56.2 and a solid state 23Na MAS NMR spectra peak at about 18 ppm. Moreover, the invention relates to methods of removing a volatile or flammable substance in a controlled manner. Furthermore, the alkali metal silicide compositions of the invention react with water to produce hydrogen gas.

    Titanium oxide and alumina alkali metal compositions
    6.
    发明授权
    Titanium oxide and alumina alkali metal compositions 有权
    氧化钛和氧化铝碱金属组合物

    公开(公告)号：US07820061B2

    公开(公告)日：2010-10-26

    申请号：US12499608

    申请日：2009-07-08

    申请人： Michael Lefenfeld ,  James L. Dye

    发明人： Michael Lefenfeld ,  James L. Dye

    IPC分类号： C01G23/00 ,  C01G23/047 ,  C07C15/02 ,  C07C403/00 ,  C07C1/20 ,  B01J23/00 ,  B01J21/00 ,  B01J20/00 ,  B01J29/00 ,  B01J37/00 ,  C02F1/70

    CPC分类号： C01G23/00 ,  B01J21/04 ,  B01J21/063 ,  B01J23/04 ,  B01J35/1061 ,  B01J35/1066 ,  B01J37/0081 ,  B01J37/0201 ,  B01J37/023 ,  B01J37/08 ,  C01B3/042 ,  C01B3/065 ,  C01B3/08 ,  C01P2006/16 ,  C07C1/26 ,  C07C2/861 ,  C07C5/324 ,  C07C17/23 ,  C07C2521/04 ,  C07C2521/06 ,  C07C2523/04 ,  Y02E60/362 ,  Y02E60/364 ,  C07C15/18 ,  C07C15/20

    摘要： The invention relates to Group 1 metal/porous metal oxide compositions comprising porous metal oxide selected from porous titanium oxide and porous alumina and an alkali metal or an alkali metal alloy. The compositions of the inventions are described as Stage 0 and I materials. These materials differ in their preparation and chemical reactivity. Each successive stage may be prepared directly using the methods described below or from an earlier stage material. Stage 0 materials may, for example, be prepared using liquid alloys of Na and K which are rapidly absorbed by porous metal oxide under isothermal conditions, preferably at or just above room temperature, to form loose black powders that retain much of the reducing ability of the parent metals. When the low melting Group 1 metals are absorbed into the porous metal oxide at about 150° C., an exothermic reaction produces Stage I material, loose black powders that are stable in dry air. Further heating forms higher stage materials of unknown composition. It is believed that Stage I higher materials represent reductions of the porous metal oxide after absorption of the Group 1 metal. Preferred Group 1 metal/porous metal oxide compositions of the invention are those containing sodium, potassium, or sodium-potassium alloys with sodium and sodium-potassium alloys being most preferred. Each stage of the Group 1 metal/porous metal oxide composition of the invention may be used as a reducing agent reacting with a number of reducible organic materials in the same manner known for alkali metals and their alloys.

    摘要翻译： 本发明涉及包含选自多孔氧化钛和多孔氧化铝的多孔金属氧化物和碱金属或碱金属合金的第1族金属/多孔金属氧化物组合物。 本发明的组合物被描述为阶段0和I材料。 这些材料的制备和化学反应性不同。 可以使用下述方法或从较早阶段的材料直接制备每个连续阶段。 阶段0材料可以例如使用Na和K的液体合金制备，其在等温条件下优选在或刚好高于室温下被多孔金属氧化物快速吸收，形成松散的黑色粉末，其保留大量的还原能力 母体金属。 当低熔点的第1族金属在约150℃下被吸收到多孔金属氧化物中时，放热反应产生阶段I材料，在干燥空气中稳定的松散的黑色粉末。 进一步加热形成未知组成的较高级材料。 据信，第一阶段较高的材料表示吸收第1族金属后多孔金属氧化物的减少。 优选的本发明的第1族金属/多孔金属氧化物组合物是含有钠，钾或钠 - 钾合金的那些，其中钠和钠 - 钾合金是最优选的。 本发明的第1族金属/多孔金属氧化物组合物的每个阶段可以以与碱金属及其合金已知的相同方式用作与许多可还原的有机材料反应的还原剂。

    Silica gel compositions containing alkali metals and alkali metal alloys
    7.
    发明授权
    Silica gel compositions containing alkali metals and alkali metal alloys 有权
    含有碱金属和碱金属合金的硅胶组合物

    公开(公告)号：US07709410B2

    公开(公告)日：2010-05-04

    申请号：US12222533

    申请日：2008-08-11

    申请人： Michael Lefenfeld ,  James L. Dye

    发明人： Michael Lefenfeld ,  James L. Dye

    IPC分类号： B01J23/02 ,  B01J21/00 ,  B01J20/00

    CPC分类号： B01J35/002 ,  B01J20/02 ,  B01J20/103 ,  B01J20/28047 ,  B01J20/28078 ,  B01J20/28097 ,  B01J20/281 ,  B01J20/291 ,  B01J20/3078 ,  B01J20/3204 ,  B01J20/3236 ,  B01J23/04 ,  B01J37/023 ,  B01J37/08 ,  B01J2220/42 ,  B01J2220/54 ,  B01J2220/56 ,  B01J2220/58 ,  C01B3/001 ,  C01B3/06 ,  C07C2/861 ,  C07C2/868 ,  C07D333/76 ,  Y02E60/324 ,  Y02E60/36 ,  C07C15/18 ,  C07C15/14

    摘要： The invention relates to Group 1 metal/silica gel compositions comprising silica gel and an alkali metal or an alkali metal alloy. The compositions of the inventions are described as Stage 0, I, II, and III materials. These materials differ in their preparation and chemical reactivity. Each successive stage may be prepared directly using the methods described below or from an earlier stage material. Stage 0 materials may, for example, be prepared using liquid alloys of Na and K which are rapidly absorbed by silica gel (porous SiO2) under isothermal conditions, preferably at or just above room temperature, to form loose black powders that retain much of the reducing ability of the parent metals. When the low melting Group 1 metals are absorbed into the silica gel, a mild exothermic reaction produces Stage I material, loose black powders that are indefinitely stable in dry air. Subsequent heating to 400° C. produces Stage II materials, which are also loose black powders. Further heating above 400° C. forms Stage III material with release of some Group 1 metal. It is believed that Stage I, H and III materials represent reductions of the silica gel after absorption of the Group 1 metal. Preferred Group 1 metal/silica gel compositions of the invention are those containing sodium, potassium, or sodium-potassium alloys with sodium and sodium-potassium alloys being most preferred. Each stage of the Group 1 metal/silica gel composition of the invention may be used as a reducing agent reacting with a number of reducible organic materials in the same manner known for alkali metals and their alloys.

    摘要翻译： 本发明涉及包含硅胶和碱金属或碱金属合金的第1族金属/硅胶组合物。 本发明的组合物被描述为阶段0，I，II和III材料。 这些材料的制备和化学反应性不同。 可以使用下述方法或从较早阶段的材料直接制备每个连续阶段。 例如，可以使用在等温条件下，优选在或高于室温的硅胶（多孔SiO 2）快速吸收的Na和K的液体合金来制备阶段0材料，以形成松散的黑色粉末，其保留大部分 降低母体金属的能力。 当低熔点的第1族金属被吸收到硅胶中时，温和的放热反应产生阶段I材料，在干燥空气中无限稳定的松散的黑色粉末。 随后加热至400°C，产生阶段II材料，它们也是松散的黑色粉末。 在400℃以上进一步加热，形成具有一些第1组金属释放的III级材料。 据信阶段I，H和III材料表示吸收第1族金属后的硅胶的减少。 本发明优选的第1族金属/硅胶组合物是含有钠，钾或钠 - 钾合金的那些，其中钠和钠 - 钾合金是最优选的。 本发明的第1族金属/硅胶组合物的每个阶段可以以与碱金属及其合金已知的相同的方式用作与许多可还原的有机材料反应的还原剂。

    TITANIUM OXIDE AND ALUMINA ALKALI METAL COMPOSITIONS
    8.
    发明申请
    TITANIUM OXIDE AND ALUMINA ALKALI METAL COMPOSITIONS 有权
    氧化钛和氧化铝碱金属组合物

    公开(公告)号：US20090266771A1

    公开(公告)日：2009-10-29

    申请号：US12499608

    申请日：2009-07-08

    申请人： Michael Lefenfeld ,  James L. Dye

    发明人： Michael Lefenfeld ,  James L. Dye

    IPC分类号： B01J19/00 ,  C09K3/00

    CPC分类号： C01G23/00 ,  B01J21/04 ,  B01J21/063 ,  B01J23/04 ,  B01J35/1061 ,  B01J35/1066 ,  B01J37/0081 ,  B01J37/0201 ,  B01J37/023 ,  B01J37/08 ,  C01B3/042 ,  C01B3/065 ,  C01B3/08 ,  C01P2006/16 ,  C07C1/26 ,  C07C2/861 ,  C07C5/324 ,  C07C17/23 ,  C07C2521/04 ,  C07C2521/06 ,  C07C2523/04 ,  Y02E60/362 ,  Y02E60/364 ,  C07C15/18 ,  C07C15/20

    摘要： The invention relates to Group 1 metal/porous metal oxide compositions comprising porous metal oxide selected from porous titanium oxide and porous alumina and an alkali metal or an alkali metal alloy. The compositions of the inventions are described as Stage 0 and I materials. These materials differ in their preparation and chemical reactivity. Each successive stage may be prepared directly using the methods described below or from an earlier stage material. Stage 0 materials may, for example, be prepared using liquid alloys of Na and K which are rapidly absorbed by porous metal oxide under isothermal conditions, preferably at or just above room temperature, to form loose black powders that retain much of the reducing ability of the parent metals. When the low melting Group 1 metals are absorbed into the porous metal oxide at about 150° C., an exothermic reaction produces Stage I material, loose black powders that are stable in dry air. Further heating forms higher stage materials of unknown composition. It is believed that Stage I higher materials represent reductions of the porous metal oxide after absorption of the Group 1 metal. Preferred Group 1 metal/porous metal oxide compositions of the invention are those containing sodium, potassium, or sodium-potassium alloys with sodium and sodium-potassium alloys being most preferred. Each stage of the Group 1 metal/porous metal oxide composition of the invention may be used as a reducing agent reacting with a number of reducible organic materials in the same manner known for alkali metals and their alloys.

    摘要翻译： 本发明涉及包含选自多孔氧化钛和多孔氧化铝的多孔金属氧化物和碱金属或碱金属合金的第1族金属/多孔金属氧化物组合物。 本发明的组合物被描述为阶段0和I材料。 这些材料的制备和化学反应性不同。 可以使用下述方法或从较早阶段的材料直接制备每个连续阶段。 阶段0材料可以例如使用Na和K的液体合金制备，其在等温条件下优选在或刚好高于室温下被多孔金属氧化物快速吸收，形成松散的黑色粉末，其保留大量的还原能力 母体金属。 当低熔点的第1族金属在约150℃下被吸收到多孔金属氧化物中时，放热反应产生阶段I材料，在干燥空气中稳定的松散的黑色粉末。 进一步加热形成未知组成的较高级材料。 据信，第一阶段较高的材料表示吸收第1族金属后多孔金属氧化物的减少。 优选的本发明的第1族金属/多孔金属氧化物组合物是含有钠，钾或钠 - 钾合金的那些，其中钠和钠 - 钾合金是最优选的。 本发明的第1族金属/多孔金属氧化物组合物的每个阶段可以以与碱金属及其合金已知的相同方式用作与许多可还原的有机材料反应的还原剂。

    Method for deprotecting aryl or alkyl sulfonamides of primary or secondary amines
    9.
    发明授权
    Method for deprotecting aryl or alkyl sulfonamides of primary or secondary amines 有权
    伯胺或仲胺芳基或烷基磺酰胺脱保护方法

    公开(公告)号：US08263808B2

    公开(公告)日：2012-09-11

    申请号：US12300409

    申请日：2007-02-13

    申请人： Michael Lefenfeld ,  James L. Dye ,  Partha Nandi ,  James Jackson

    发明人： Michael Lefenfeld ,  James L. Dye ,  Partha Nandi ,  James Jackson

    IPC分类号： C07C209/00

    CPC分类号： C07D211/96 ,  C07C209/62 ,  C07C213/08 ,  C07C2601/14 ,  Y02P20/55 ,  C07C211/35 ,  C07C211/40 ,  C07C211/45 ,  C07C217/08

    摘要： The invention relates to a method for removing an alkyl sulfonyl or aryl sulfonyl protecting group from a primary or secondary amine by contacting an alkyl sulfonamide or an aryl sulfonamide with a Stage 0 or Stage I alkali metal-silica gel material in the presence of a solid proton source under conditions sufficient to form the corresponding amine. The invention also relates to a method for removing an alkyl sulfonyl or aryl sulfonyl protecting group from a primary or secondary amine by a) reacting an alkyl sulfonamide or an aryl sulfonamide with a Stage 0 or Stage I alkali metal-silica gel material, and b) subsequently reacting the reaction product from step a) with an electrophile or a proton source. Preferred Stage 0 or Stage I alkali metal-silica gel materials include Na, K2Na, and Na2K.

    摘要翻译： 本发明涉及通过在固体存在下使烷基磺酰胺或芳基磺酰胺与阶段0或阶段I碱金属 - 硅胶材料接触来从伯胺或仲胺除去烷基磺酰基或芳基磺酰基保护基的方法 质子源在足以形成相应胺的条件下。 本发明还涉及通过以下步骤从伯胺或仲胺除去烷基磺酰基或芳基磺酰基保护基的方法：a）使烷基磺酰胺或芳基磺酰胺与阶段0或阶段I碱金属 - 硅胶材料反应，b ）随后使来自步骤a）的反应产物与亲电试剂或质子源反应。 优选的阶段0或阶段I碱金属 - 硅胶材料包括Na，K 2 Na和Na 2 K。