Hydrogen Containing Patents (Class 423/294)
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Patent number: 10731080Abstract: Systems and methods for recycling waste plastics are provided, including a system for recovering styrene monomer from waste polystyrene.Type: GrantFiled: April 18, 2019Date of Patent: August 4, 2020
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Patent number: 10059599Abstract: The present invention is directed to a process for the synthesis of alkali metal tetrahydroborates-10B and amine borane-10B precursors, such as sodium tetrahydroborate-10B and triethylamine borane-10B.Type: GrantFiled: February 3, 2015Date of Patent: August 28, 2018Assignee: THE CURATORS OF THE UNIVERSITY OF MISSOURIInventors: Alexander Valentinovich Safronov, Satish Subray Jalisatgi, Marion Frederick Hawthorne
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Patent number: 9598352Abstract: The present invention provides methods and devices for producing polyhedral boron compounds. The process is generally an anhydrous, one-pot process that comprises a pyrolytic reaction of a tetraborohydride with a quaternary amine salt to form the polyhedral borane. In another aspect of the present invention, polyhedral boranes are produced, without isolation of the Lewis base-borane complex.Type: GrantFiled: November 16, 2012Date of Patent: March 21, 2017Assignee: The Curators of the University of MissouriInventors: Mark Wayne Lee, Marion Frederick Hawthorne
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Publication number: 20150034500Abstract: A metal organic framework (MOF) includes a coordination product of a metal ion and an at least bidentate organic ligand, where the metal ion and the organic ligand are selected to provide a deliverable adsorption capacity of at least 70 g/l for an electronic gas. A porous organic polymer (POP) includes polymerization product from at least a plurality of organic monomers, where the organic monomers are selected to provide a deliverable adsorption capacity of at least 70 g/l for an electronic gas.Type: ApplicationFiled: August 4, 2014Publication date: February 5, 2015Inventors: Han Sung KIM, Mitchell Hugh WESTON, Patrick FULLER, Paul Wai-Man SIU
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Patent number: 8864857Abstract: An apparatus for generating hydrogen gas from a replaceable aluminum pack comprising an aluminum and hydride mixture encased in a breathable membrane that is raised and lowered into a fluid contained within an enclosed tank wherein contact with the fluid releases hydrogen gas from the aluminum. A pressure transducer and microprocessor chip are provided for monitoring and regulating the rate of hydrogen production by engaging and disengaging a reversible motor that raises and lowers an inner tray on which the aluminum pack resides accordingly.Type: GrantFiled: July 26, 2011Date of Patent: October 21, 2014Inventor: Harlo Mayne
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Patent number: 8753600Abstract: New methods are provided for synthesis of ClusterBoron® (B18H22). Preferred methods of the invention include generation of the conjugate acid of B20H182? and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: GrantFiled: January 18, 2011Date of Patent: June 17, 2014Assignee: SemEquip, Inc.Inventors: Kevin S. Cook, Mark Oxford
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Publication number: 20140113811Abstract: Provided are methods for storing gases on porous adsorbents, methods for optimizing the storage of gases on porous adsorbents, methods of making porous adsorbents, and methods of gas storage of optimized compositions, as in systems containing porous adsorbents and gas adsorbed on the surface of the porous adsorbent. The disclosed methods and systems feature a constant or increasing isosteric enthalpy of adsorption as a function of uptake of the gas onto the exposed surface of a porous adsorbent. Adsorbents with a porous geometry and surface dimensions suited to a particular adsorbate are exposed to the gas at elevated pressures in the specific regime where n/V (density) is larger than predicted by the ideal gas law by more than several percent.Type: ApplicationFiled: October 10, 2013Publication date: April 24, 2014Inventors: Nicholas P. STADIE, Brent T. FULTZ, Channing AHN, Maxwell MURIALDO
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Patent number: 8673251Abstract: The invention provides new methods for synthesis of ClusterBoron® (B18H22). Preferred methods of the invention include generation of the conjugate acid of B20H182? and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: GrantFiled: November 3, 2008Date of Patent: March 18, 2014Assignee: SemEquip, Inc.Inventors: Kevin S. Cook, Mark Oxford
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Patent number: 8623309Abstract: The invention provides new methods for synthesis of ClusterBoron (B18H22). Preferred methods of the invention include in situ generation of the conjugate acid of B20H182? and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B)18H22 and 11B18H22.Type: GrantFiled: November 3, 2008Date of Patent: January 7, 2014Assignee: SemEquip, Inc.Inventor: Kevin S. Cook
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Publication number: 20130236384Abstract: New methods are provided for synthesis of ClusterBoron® (B18H22). Preferred methods of the invention include generation of the conjugate acid of B20H182? and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: ApplicationFiled: January 18, 2011Publication date: September 12, 2013Applicant: SEMEQUIP, INC.Inventors: Kevin S. Cook, Mark Oxford
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Patent number: 8465715Abstract: The present invention describes the synthesis of a family of metal bis(borano) hypophosphite complexes. One procedure described in detail is the syntheses of complexes beginning from phosphorus trichloride and sodium borohydride. Temperature, solvent, concentration, and atmosphere are all critical to ensure product formation. In the case of sodium bis(borano) hypophosphite, hydrogen gas was evolved upon heating at temperatures above 150° C. Included in this family of materials are the salts of the alkali metals Li, Na and K, and those of the alkaline earth metals Mg and Ca. Hydrogen storage materials are possible. In particular the lithium salt, Li[PH2(BH3)2], theoretically would contain nearly 12 wt % hydrogen. Analytical data for product characterization and thermal properties are given.Type: GrantFiled: July 2, 2010Date of Patent: June 18, 2013Assignee: Sandia CorporationInventor: Joseph G. Cordaro
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Patent number: 8329131Abstract: The invention provides new methods for synthesis of large boron hydride clusters, e.g., boron hydride molecules of the formula BnHm where 5?n?96 and m?n+8, wherein m and n satisfy the electron counting rules of macropolyhedral boranes. The invention is particularly useful for synthesis of octadecaborane (B18H22). Preferred methods of the invention include iteratively generating a conjugate acid from a salt of the [BaHb]c? or [Bn+2Hm?4]2? anion followed by degradation under conditions conducive to concentrating and drying of the conjugate acid to provide a borane BnHm and residual salt of the [BaHb]c? or [Bn+2Hm?4]2? anion which is reused in the method of synthesis. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: GrantFiled: May 17, 2011Date of Patent: December 11, 2012Assignee: SemEquip, Inc.Inventors: Bernard Spielvogel, Kevin S. Cook
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Patent number: 8083996Abstract: Provided are a thermal siphon reactor and a hydrogen generator including the same. The hydrogen generator including the thermal siphon reactor includes: a housing; a reaction source container disposed in the housing; a reactor tube connected to the reaction source container in which a catalytic reaction of a reaction source provided from the reaction source container occurs; a catalyst layer which is porous, facilitates gas generation by being contacted with the reaction source, and is disposed in the reactor tube; and a product container which is connected to the reactor tube and collects a reaction product generated in the reactor tube, wherein in the reactor tube, a convection channel through which the reaction product is discharged passes through the reactor tube in the lengthwise direction of the reactor tube. The thermal siphon reactor and the hydrogen generator including the same have a self-operating ability, operate at low costs, and have small installment volume.Type: GrantFiled: January 23, 2007Date of Patent: December 27, 2011Assignee: Samsung Engineering Co., Ltd.Inventors: Myong Hoon Lim, Tae Hee Park, Jae Hoi Gu, Yongho Yu
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Patent number: 8084007Abstract: The invention provides new methods for the synthesis of isotopically enriched metal borohydrides, metal tetrahydroundecaborate salts, and decaborane from isotopically enriched 10B-boric acid or 11B-boric acid. The invention is particularly useful for synthesis of isotopically enriched sodium or lithium borohydride, MB11H14 (where M is Li, Na, K, or alkylammonium), and decaborane.Type: GrantFiled: December 31, 2009Date of Patent: December 27, 2011Assignee: SemEquip Inc.Inventors: Bernard Spielvogel, Kevin S. Cook
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Publication number: 20110217223Abstract: The invention provides new methods for synthesis of large boron hydride clusters, e.g., boron hydride molecules of the formula BnHm where 5?n?96 and m?n+8, wherein m and n satisfy the electron counting rules of macropolyhedral boranes. The invention is particularly useful for synthesis of octadecaborane (B18H22). Preferred methods of the invention include iteratively generating a conjugate acid from a salt of the [BaHb]c? or [Bn+2Hm?4]2? anion followed by degradation under conditions conducive to concentrating and drying of the conjugate acid to provide a borane BnHm and residual salt of the [BaHb]c? or [Bn+2Hm?4]2? anion which is reused in the method of synthesis. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: ApplicationFiled: May 17, 2011Publication date: September 8, 2011Applicant: SEMEQUIP, INC.Inventors: Bernard Spielvogel, Kevin Cook
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Publication number: 20110195009Abstract: The invention provides new methods for synthesis of ClusterBoron (B18H22). Preferred methods of the invention include in situ generation of the conjugate acid of B20H182? and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B)18H22 and 11B18H22.Type: ApplicationFiled: November 3, 2008Publication date: August 11, 2011Applicant: SemEquip, Inc.Inventor: Kevin S. Cook
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Publication number: 20110165053Abstract: The invention provides new methods for synthesis of ClusterBoron® (B18H22). Preferred methods of the invention include generation of the conjugate acid of B20H182? and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: ApplicationFiled: November 3, 2008Publication date: July 7, 2011Inventors: Kevin S. Cook, Mark Oxford
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Patent number: 7955580Abstract: The invention provides new methods for synthesis of large boron hydride clusters e.g., boron hydride molecules of the formula BnHm where 5?n?96 and m?n+8, wherein m and n satisfy the electron counting rules of macropolyhedral boranes. The invention is particularly useful for synthesis of octadecaborane (B18H22). Preferred methods of the invention include iteratively generating a conjugate acid from a salt of the [BaHb]c? or [Bn+2Hm?4]2? anion followed by degradation under conditions conducive to concentrating and drying of the conjugate acid to provide a borane BnHm and residual salt of the [BaHb]c? or [Bn+2Hm?4]2? anion which is reused in the method of synthesis. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: GrantFiled: January 21, 2005Date of Patent: June 7, 2011Assignee: SemEquip, Inc.Inventors: Bernard Spielvogel, Kevin Cook
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Patent number: 7837852Abstract: The reaction of halo-boron compounds (B—X compounds, compounds having one or more boron-halogen bonds) with silanes provides boranes (B—H compounds, compounds having one or more B—H bonds) and halosilanes. Inorganic hydrides, such as surface-bound silane hydrides (Si—H) react with B—X compounds to form B—H compounds and surface-bound halosilanes. The surface bound halosilanes are converted back to surface-bound silanes electrochemically. Halo-boron compounds react with stannanes (tin compounds having a Sn—H bond) to form boranes and halostannanes (tin compounds having a Sn—X bond). The halostannanes are converted back to stannanes electrochemically or by the thermolysis of Sn-formate compounds. When the halo-boron compound is BCl3, the B—H compound is B2H6, and where the reducing potential is provided electrochemically or by the thermolysis of formate.Type: GrantFiled: July 31, 2009Date of Patent: November 23, 2010Assignee: Los Alamos National Security, LLCInventors: David L. Thorn, William Tumas, Daniel E. Schwarz, Anthony K. Burrell
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Patent number: 7718154Abstract: This idea relates to the synthesis of salts of dodecahydrododecaborate B12H12 (2-). In the proposed process a metal hydride is reacted with an alkyl borate in the presence of a Lewis base to produce Lewis base-borane compex, which is thermally decomposed to produce salts of B12H12 (2-), while alkyl borare is recovered from the reaction by-product and is recycled.Type: GrantFiled: June 7, 2006Date of Patent: May 18, 2010Assignee: Air Products and Chemicals, Inc.Inventors: Sergei Vladimirovich Ivanov, Baldomero Casas
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Patent number: 7641879Abstract: The invention provides new methods for the synthesis of isotopically enriched metal borohydrides, metal tetrahydroundecaborate salts, and decaborane from isotopically enriched 10B-boric acid or 11B-boric acid. The invention is particularly useful for synthesis of isotopically enriched sodium or lithium borohydride, MB11H14 (where M is Li, Na, K, or alkylammonium), and decaborane.Type: GrantFiled: January 28, 2005Date of Patent: January 5, 2010Assignee: SemEquip Inc.Inventors: Bernard Spielvogel, Kevin Cook
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Publication number: 20090317317Abstract: A method of storing and dispensing a fluid includes providing a vessel configured for selective dispensing of the fluid therefrom. A solvent mixture comprising an ionic liquid and a cosolvent is provided within the vessel. The fluid is contacted with the solvent mixture for take-up of the fluid by the solvent mixture. The fluid is released from the ionic liquid and dispensed from the vessel.Type: ApplicationFiled: September 1, 2009Publication date: December 24, 2009Applicant: Matheson Tri-Gas, Inc.Inventors: Carrie L. Wyse, Robert Torres, JR., Joseph V. Vininski
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Patent number: 7524477Abstract: The invention provides new methods for synthesis of B9H9?, B10H102?, B11H14?, and B12H122? salts, particularly alkylammonium salts of B9H9?, B10H102?, B11H14?, and B12H122?. More particularly, the invention provides methods of preparing tetraalkylamronium salts of B9H9?, B10H102?, B11H14?, and B12H122? by pyrolysis of tetraalkylammonium borohydrides under controlled conditions. The invention additionally provides methods of preparing, in an atom efficient process, octadecaborane from the tetraalkylammonium salts of the invention. Preferred methods of the invention are suitable for preparation of isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.Type: GrantFiled: February 2, 2005Date of Patent: April 28, 2009Assignee: SemEquip Inc.Inventors: Bernard Spielvogel, Kevin Cook
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Publication number: 20080305026Abstract: A method for producing a borohydride is described and which includes the steps of providing a source of borate; providing a material which chemically reduces the source of the borate to produce a borohydride; and reacting the source of borate and the material by supplying heat at a temperature which substantially effects the production of the borohydride.Type: ApplicationFiled: August 21, 2008Publication date: December 11, 2008Inventor: Peter C. Kong
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Patent number: 7397048Abstract: A technique for boron implantation is disclosed. In one particular exemplary embodiment, the technique may be realized by an apparatus for boron implantation. The apparatus may comprise a reaction chamber. The apparatus may also comprise a source of pentaborane coupled to the reaction chamber, wherein the source is capable of supplying a substantially pure form of pentaborane into the reaction chamber. The apparatus may further comprise a power supply that is configured to energize the pentaborane in the reaction chamber sufficiently to produce a plasma discharge having boron-bearing ions.Type: GrantFiled: September 16, 2005Date of Patent: July 8, 2008Assignee: Varian Semiconductor Equipment Associates, Inc.Inventors: Vikram Singh, Edmund J. Winder, Harold M. Persing, Timothy Jerome Miller, Ziwei Fang, Atul Gupta
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Patent number: 6660238Abstract: BF3CO2 or both are removed from a mixture containing these gases with B2H6 by contacting the mixture with an inorganic hydroxide such as LiOH. B2H6 is synthesized by contacting BF3 with KBH4.Type: GrantFiled: December 12, 2002Date of Patent: December 9, 2003Assignee: Honeywell Intellectual Properties, Inc.Inventor: Dalbir S. Rajoria
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Patent number: 6517796Abstract: BF3, CO2 or both are removed from a mixture containing these gases with B2H6 by contacting the mixture with an inorganic hydroxide such as LiOH. B2H6 is synthesized by contacting BF3 with KBH4.Type: GrantFiled: September 14, 2000Date of Patent: February 11, 2003Assignee: Honeywell Intellectual Properties Inc.Inventor: Dalbir S. Rajoria
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Patent number: 6165434Abstract: BF.sub.3, CO.sub.2 or both are removed from a mixture containing these gases with B.sub.2 H.sub.6 by contacting the mixture with an inorganic hydroxide such as LiOH. B.sub.2 H.sub.6 is synthesized by contacting BF.sub.3 with KBH.sub.4.Type: GrantFiled: April 9, 1999Date of Patent: December 26, 2000Assignee: UHP Materials, IncInventor: Dalbir S. Rajoria
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Patent number: 6086837Abstract: A method is described for synthesizing decaborane wherein at least about 90% of the boron atoms in the decaborane are the .sup.10 B isotope, comprising the steps of: (a) reacting boric acid with a C.sub.1 to C.sub.10 alkanol to form a .sup.10 B-alkyl borate wherein at least about 90% of the boron atoms in the boric acid are the .sup.10 B isotope; (b) reducing the .sup.10 B-alkyl borate to form an alkali metal .sup.10 B-borohydride; (c) converting the alkali metal .sup.10 B-borohydride to a .sup.10 B-tetradecahydroundecaborate ion; and (d) converting the .sup.10 B-tetradecahydroundecaborate ion to .sup.10 B-decaborane. Methods of preparing tetradecahydroundecaborate ions and decaborane from alkali metal borohydrides are also described.Type: GrantFiled: April 24, 1997Date of Patent: July 11, 2000Assignee: Bechtel BWXT Idaho, LLCInventors: Robert L. Cowan, Daniel M. Ginosar, Gary B. Dunks
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Patent number: 6048985Abstract: A method of stabilizing borane-tetrahydrofuran complex comprises the step of maintaining the temperature of the borane-tetrahydrofuran complex at or below 20.degree. C. A method of reacting a borane reagent with a substrate comprises the steps of heating the borane reagent and the substrate in a reaction vessel and preventing escape of evolved diborane from the reaction vessel. Preferably, a reaction vessel containing a borane reagent and a substrate is maintained under at greater than atmospheric pressure with back-pressure regulation.Type: GrantFiled: December 22, 1998Date of Patent: April 11, 2000Assignee: Mine Safety Appliances CompanyInventors: Elizabeth R. Burkhardt, Joseph A. Corella, II
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Patent number: 5993766Abstract: A system for the storage and delivery of a sorbable fluid, comprising a storage and dispensing vessel containing a sorbent material having sorptive affinity for the sorbable fluid, and from which the fluid is desorbable by pressure-mediated and/or thermally-mediated desorption, wherein the sorbent material is functionally enhanced by a reagent which alters the binding energy of the fluid to the sorbent. In a preferred aspect, the system is arranged for storage and delivery of B.sub.2 H.sub.6, in which the sorbent material has sorptive affinity for B.sub.2 H.sub.6 and is effective when B.sub.2 H.sub.6 is contacted with the sorbent to convert B.sub.2 H.sub.6 to a sorbed .BH.sub.3 form, which is desorbable by pressure-mediated desorption and/or thermally-mediated desorption to release B.sub.2 H.sub.6 from the sorbent, and means for selectively discharging desorbed B.sub.2 H.sub.Type: GrantFiled: May 20, 1997Date of Patent: November 30, 1999Assignee: Advanced Technology Materials, Inc.Inventors: Glenn M. Tom, James V. McManus
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Patent number: 5938969Abstract: A fire suppressant powder with particle sizes less than 5 .mu.m is made by a chemical reaction between a gas or vapour of a first material and a vapour or an aerosol of a second material. For example an aerosol of sodium hydroxide droplets may be reacted with carbon dioxide gas to produce sodium bicarbonate powder; or boron halide vapour may be reacted with steam to form boric acid powder The powder may be used in fire extinguishers either on its own, or combined with other ingredients such as silica and/or alumina, and calcium stearate.Type: GrantFiled: December 3, 1997Date of Patent: August 17, 1999Assignee: AEA Technology plcInventor: David Alexander Vodden Morton
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Patent number: 5543127Abstract: A solution of hydride in liquid nitrogen, the hydride being one that is in gaseous phase at atmospheric pressure and ambient temperature. The concentration of hydride in the liquid nitrogen is comprised between 0.05 and 10 mol %, preferably between 0.05 and 2 mol %, and more preferably between 0.1 and 0.3 mol %. The hydride is selected from the group consisting of arsine, germane, phosphine (PH.sub.3), diborane and silane (SiH.sub.4) and is preferably silane. Atmospheres prepared from these solutions are useful in the thermal treatment of metals, or for surface treatment, particularly of polymeric or metallic surfaces.Type: GrantFiled: March 3, 1994Date of Patent: August 6, 1996Assignee: L'Air Liquide, Societe Anonyme pour l'Etude et l'Exploitation des Procedes Georges ClaudeInventors: Pierre Karinthi, Bernard Jamonet
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Patent number: 5264783Abstract: An electrical power controller includes an integrated circuit having a Hall element, a Hall voltage amplifier, a ramp signal generator, and a voltage comparator. The output of the ramp generator is connected to one input of the voltage comparator and the output of the Hall voltage amplifier is connected to the outer comparator input. During intervals when the amplified Hall voltage exceeds the ramp voltage, the output of the comparator changes from one binary state to the other such that a stream of pulses is generated at the output of the comparator. Thus as a magnetic field at the Hall element increases, the Hall voltage increases and the width of each pulse in the stream of pulses grows proportionally. Mechanical means is provided for manually moving and guiding the pole of a magnet along a path toward the integrated circuit. Constructions of such controllers adapted for use as lamp dimmers and DC motor speed controllers are described.Type: GrantFiled: January 21, 1992Date of Patent: November 23, 1993Assignee: Allegro Microsystems, Inc.Inventors: Ravi Vig, Mark C. Hopkins, Jay M. Towne
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Patent number: 5026809Abstract: Preceramic polymers formed by reacting B.sub.10 H.sub.14-n R.sub.n, (where R is a lower alkyl group having from 1 to about 8 carbon atoms, a substituted or unsubstituted cycloalkyl group having from 3 to about 8 carbon atoms, a substituted or unsubstituted lower alkenyl group having from 2 to about 8 carbon atoms, or a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, and n is a number from zero to about six) with a diamine of the formulaR.sup.1 R.sup.2 N--(E).sub.q --NR.sup.4 R.sup.5,where R.sup.1, R.sup.2, R.sup.4 and R.sup.Type: GrantFiled: June 2, 1989Date of Patent: June 25, 1991Assignee: Massachusetts Institute of TechnologyInventors: Seyferth Dietmar, William S. Rees, Jr.
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Patent number: 4976942Abstract: A method for purifying a gaseous hydride, which comprises bringing a crude gaseous hydride into contact with at least one material from nickel arsenides, nickel phosphides, nickel silicides, nickel selenides, or nickel borides to remove oxygen contained in the crude gaseous hydride.Type: GrantFiled: September 26, 1989Date of Patent: December 11, 1990Assignee: Japan Pionics, Ltd.Inventors: Koichi Kitahara, Takashi Shimada, Keiichi Iwata, Noboru Akita
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Patent number: 4970095Abstract: A method of producing coatings of boron nitride on substrates by the application of solutions containing boron compounds.Type: GrantFiled: December 30, 1988Date of Patent: November 13, 1990Assignee: E. I. du Pont de Nemours and CompanyInventors: John D. Bolt, Frederick N. Tebbe
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Patent number: 4871826Abstract: New soluble preceramic polymers formed by reacting B.sub.10 H.sub.14-n R.sub.n, (where R is a lower alkyl group having from 1 to about 8 carbon atoms, a substituted or unsubstituted cycloalkyl group having from 3 to about 8 carbon atoms, a substituted or unsubstituted lower alkenyl group having from 2 to about 8 carbon atoms, or a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, and n is a number from zero to about six) with a diamine in an organic solvent are disclosed. Preferably the diamine has the formulaR.sup.1 R.sup.2 N-R.sup.3 -NR.sup.4 R.sup.5where R.sup.1, R.sup.2, R.sup.4 and R.sup.5 are H, a lower alkyl group having from 1 to about 8 carbon atoms, a substituted or unsubstituted cycloalkyl group having from 3 to about 8 carbon atoms, a substituted or unsubstituted lower alkenyl group having from 2 to about 8 carbon atoms, a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, or a di- or triorganosilyl. R.sup.Type: GrantFiled: June 22, 1987Date of Patent: October 3, 1989Assignee: Massachusetts Institute of TechnologyInventors: Dietmar Seyferth, William S. Rees, Jr.
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Patent number: 4338289Abstract: Disclosed is a method for the preparation of decaborane-14(B.sub.10 H.sub) in high yields from B.sub.5 H.sub.9 which involve three basic procedure steps as follows:(1) conversion of B.sub.5 H.sub.9 to a solid, [N(CH.sub.3).sub.4 ][B.sub.9 H.sub.14 ], by reacting NaH in a tetrahydrofuran (THF) solution in the presence of [N(CH.sub.3).sub.4 ][Cl];(2) performing a hydride abstraction on the solid after removal of THF by reacting, while stirring, a boron trihalide selected from BBr.sub.3 and BCl.sub.3 to form B.sub.10 H.sub.14 ; and,(3) separating the B.sub.10 H.sub.14 from the solid reaction mixture by a sublimation procedure.Type: GrantFiled: August 10, 1981Date of Patent: July 6, 1982Assignee: The United States of America as represented by the Secretary of the ArmyInventors: Sheldon G. Shore, Mark A. Toft, Francis L. Himpsl
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Patent number: 4320027Abstract: A process which comprises heating a stabilized solution of borane in tetrahydrofuran containing an organic sulfide and finely divided particles of sodium fluoroborate at an elevated temperature for a period of time sufficient to convert the sodium fluoroborate particles to a form which permits them to be readily removed from the solution such as by settling, filtration or centrifugation.Type: GrantFiled: May 2, 1980Date of Patent: March 16, 1982Assignee: Aldrich-Boranes, Inc.Inventor: Herbert C. Brown
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Patent number: 4115520Abstract: Tetradecahydroundecaborate compounds, MB.sub.11 H.sub.14, wherein M represents a monovalent cation are prepared by the reaction of the corresponding octahydroborate compounds, MB.sub.3 H.sub.8, with boron trifluoride. The reaction is carried out at a temperature of 100.degree. C. to 120.degree. C., preferably in an inert solvent medium.Type: GrantFiled: September 29, 1977Date of Patent: September 19, 1978Assignee: Union Carbide CorporationInventors: Gary Burr Dunks, Kathy Palmer Ordonez
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Patent number: 4115521Abstract: Decaborane (14) is prepared by the chemical oxidation of the tetradecahydroundecaborate (-1) ion with an oxidant having an electrode potential (E.degree.) of at least +0.6 volts.Type: GrantFiled: July 5, 1977Date of Patent: September 19, 1978Assignee: Union Carbide CorporationInventors: Gary Burr Dunks, Kathy Palmer Ordonez
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Patent number: 4026993Abstract: A method for preparing a mixture of decaborane-14 and an alkyl-substituted ecaborane-14 which comprises admixing an ethereal solution of nonaborane-14 ions with an alkaliboron halide at a temperature from 20.degree. C to 30.degree. C and at pressure from atmospheric pressure to 400 psig and a method of preparing decaborane-14 which comprises preparing an ethereal solution of nonaborane-14 by a reaction in an ethereal solution of an alkali metal borohydride with an excess of pentaborane-9 at temperature from 20.degree. C to 30.degree. C and admixing this ethereal solution of nonaborane-14 ions with diborane-6 at a temperature from 20.degree. C to 30.degree. C and at a pressure of at least 50 psig. Such compounds are useful as precursor compounds for the synthesis of important carborane derivatives, such as n-hexylcarborane (a catalyst for rocket propellants) and high-temperature-resistant carborane/siloxane polymers.Type: GrantFiled: August 23, 1976Date of Patent: May 31, 1977Assignee: The United States of America as represented by the Secretary of the NavyInventors: Jerome F. Ditter, Eugene B. Klusmann