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(12) United States Patent (10) Patent No.: US 8,007,762 B2 Lefenfeld Et Al

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(12) United States Patent (10) Patent No.: US 8,007,762 B2 Lefenfeld Et Al USO08007762B2 (12) United States Patent (10) Patent No.: US 8,007,762 B2 Lefenfeld et al. (45) Date of Patent: *Aug. 30, 2011 (54) SILICA GEL COMPOSITIONS CONTAINING (58) Field of Classification Search .................. 423/657; ALKAL METALS AND ALKAL METAL 585/400, 469; 502/233,237, 343, 344, 407, ALLOYS 502/411,439 (75) Inventors: Michael Lefenfeld, New York, NY (US); See application file for complete search history. James L. Dye, East Lansing, MI (US) (56) References Cited (73) Assignees: SiGNa Chemistry, Inc., New York, NY (US); Board of Trustees of Michigan State University, East Lansing, MI (US) us. PATENT DOCUMENTS (*) Notice: Subject to any disclaimer, the term of this 1,665,264 A 48,issass et al. patent is extended or adjusted under 35 U.S.C. 154(b) by 0 days. FOREIGN PATENT DOCUMENTS This patent is subject to a terminal dis- JP O9-141097 6, 1997 claimer. (Continue 3 (21) Appl. No.: 12/723,588 OTHER PUBLICATIONS (22) Filed: Mar 12, 2010 (65) Prior Publication Data K.M. Unruh. T.E. Huber, and C.A. Huber, "Melting and freezing behavior of indium metal in porous glasses.” Physical Review B, Sep. US 2010/0166648 A1 Jul. 1, 2010 15, 1993, pp. 9021-9027, vol. 48, No. 12, The American Physical Related U.S. Application Data Society. (60) Continuation of application No. 12/222,533, filed on (Continued) conunuauon(i. R OI applicauonI R N No. 779:...is 89), Illed on a Primary Examiner — Cam N. Nguyen Mar. 28, 2007, now Pat. No. 7,410,567, which is a Sattorney Agent, or Firm — J.A. Lindeman & Co., division of application No. 10/995.327, filed on Nov. 24, 2004, now Pat. No. 7,211,539. (57) ABSTRACT (60) Provisional application No. 60/524,038, filed on Nov. The invention relates to Group 1 metal/silica gel composi 24, 2003, provisional application No. 60/561,886, tions comprising silica gel and an alkali metal or alloy, filed on Apr. 14, 2004, provisional application No. wherein Group 1 metals or alloys are absorbed into the silica 60/578,818, filed on Jun. 14, 2004, provisional gel pores. The invention relates to producing hydrogen gas application No. 60/611,701, filed on Sep. 22, 2004, comprising contacting a Group 1 metal/silica gel composition provisional application No. 60/61 1,700, filed on Sep. with water, and further relates to an alkali metal reduction of 22, 2004. an organic compound, the improvement comprising contact (51) Int. Cl. ing the organic compound with a Group 1 metal/silica gel COIB 3/08 (2006.01) composition. In these embodiments, the Group 1 metal/silica C07C 15/02 (2006.01) gel composition reacts with dry O. The invention also relates CD7C 403/00 (2006.01) to producing hydrogen gas comprising contacting a Group 1 C07C I/20 (2006.01) metal/silicag1/silica gel compositionpost with water, andc. further relates to BOI. 23/00 (2006.01) improvementan alkali metal comprising reduction contacting of an organic the organic compound, compound the BOI 2L/00 (2006.01) with a Group 1 metal/silica gel composition. In these embodi BOI 20/00 (2006.01) ments, the Group 1 metal/silica gel composition produced (52) U.S. Cl. ........ 423/657; 585/400:585/469; 502/233; does not react with dry O. 502/237; 502/343; 502/344: 502/.407: 502/411; 20 Claims, 9 Drawing Sheets O - Z-N w -2 - -60 -40 -20 0 -- - O 100 200 300 400 500 600 Temperature (C) US 8,007,762 B2 Page 2 U.S. PATENT DOCUMENTS FOREIGN PATENT DOCUMENTS 1939,647 A * 12/1933 Arnold et al. WO O3,0558O2 A1 T 2003 2,337.419 A * 12, 1943 Sensel 2,378,290 A * 6/1945 Drake et al. 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