Patents Assigned to SIGNa Chemistry, LLC
  • Patent number: 8986643
    Abstract: 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.
    Type: Grant
    Filed: April 12, 2012
    Date of Patent: March 24, 2015
    Assignees: Signa Chemistry, LLC, The Board of Trustees of Michigan State University
    Inventors: Michael Lefenfeld, James L. Dye
  • Patent number: 8197707
    Abstract: 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.
    Type: Grant
    Filed: September 10, 2007
    Date of Patent: June 12, 2012
    Assignee: Signa Chemistry LLC
    Inventors: Michael Lefenfeld, James L. Dye, Partha Nandi, James Jackson
  • Publication number: 20090306391
    Abstract: 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.
    Type: Application
    Filed: February 13, 2007
    Publication date: December 10, 2009
    Applicant: SIGNA CHEMISTRY, LLC
    Inventors: Michael Lefenfeld, James L. Dye, Partha Nandi, James Jackson
  • Patent number: 7410567
    Abstract: 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.
    Type: Grant
    Filed: March 28, 2007
    Date of Patent: August 12, 2008
    Assignees: SiGNa Chemistry, LLC, Board of Trustees of Michigan State University
    Inventors: Michael Lefenfeld, James L. Dye
  • Publication number: 20080111104
    Abstract: 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. In formula RLi, R is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group, or an NR1R2 group; R1 is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group; and R2 is hydrogen, an alkyl group, an alkenyl group, an alkynyl group, an aryl group, and an alkaryl group. The preparation and use of these compositions are also described.
    Type: Application
    Filed: September 10, 2007
    Publication date: May 15, 2008
    Applicant: SiGNA Chemistry, LLC
    Inventors: Michael LEFENFELD, James L. DYE, Partha NANDI, James JACKSON
  • Publication number: 20080063596
    Abstract: 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.
    Type: Application
    Filed: August 16, 2007
    Publication date: March 13, 2008
    Applicant: SIGNA CHEMISTRY LLC
    Inventors: Michael Lefenfeld, James Dye
  • Patent number: 7259128
    Abstract: 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.
    Type: Grant
    Filed: September 22, 2005
    Date of Patent: August 21, 2007
    Assignees: SiGNa Chemistry, LLC, Board of Trustees of Michigan State University
    Inventors: Michael Lefenfeld, James L. Dye
  • Publication number: 20070167317
    Abstract: 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.
    Type: Application
    Filed: March 28, 2007
    Publication date: July 19, 2007
    Applicants: SIGNA CHEMISTRY, LLC, BOARD OF TRUSTEES OF MICHIGAN STATE UNIVERSITY
    Inventors: Michael LEFENFELD, James DYE
  • Patent number: 7211539
    Abstract: 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.
    Type: Grant
    Filed: November 24, 2004
    Date of Patent: May 1, 2007
    Assignees: SIGNa Chemistry, LLC, Board of Trustees of Michigan State University
    Inventors: Michael Lefenfeld, James L. Dye
  • Publication number: 20060073968
    Abstract: 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.
    Type: Application
    Filed: September 22, 2005
    Publication date: April 6, 2006
    Applicants: SIGNA Chemistry LLC, MICHIGAN STATE UNIVERSITY
    Inventors: Michael Lefenfeld, James Dye