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(12) United States Patent (10) Patent No.: US 9.249,480 B2 Sepeur Et Al

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(12) United States Patent (10) Patent No.: US 9.249,480 B2 Sepeur Et Al USOO924.948OB2 (12) United States Patent (10) Patent No.: US 9.249,480 B2 Sepeur et al. (45) Date of Patent: Feb. 2, 2016 (54) METHOD FOR PRODUCING ALKALIAND (58) Field of Classification Search ALKALINE EARTH ALLOYS AND USE OF CPC ................................. C22C 24/00; B01J 23/04 THE ALKALIAND ALKALINE EARTH USPC ....................................................... 427/376.1 ALLOYS See application file for complete search history. (75) Inventors: Stefan Sepeur, Wadgassen (DE); (56) References Cited Gerald Frenzer, Saarbruecken (DE); U.S. PATENT DOCUMENTS Stefan Huefner, Saarbruecken (DE); Frank Mueller, Saarbruecken (DE) 2,171.439 A 8/1939 von Zeppelin 3,469,729 A * 9/1969 Grekila et al. ............. 220/2.3 R (73) Assignees: NANO-X GmbH, Saarbruecken (DE); Elringklinger AG, Dettingen an der (Continued) Erms (DE), part interest FOREIGN PATENT DOCUMENTS (*) Notice: Subject to any disclaimer, the term of this CH 216 205 8, 1941 patent is extended or adjusted under 35 CH 219713 2, 1942 U.S.C. 154(b) by 81 days. (Continued) (21) Appl. No.: 13/138,373 OTHER PUBLICATIONS (22) PCT Filed: Feb. 9, 2010 International Search Report of PCT/DE2010/0750 13, Aug. 11, 2010. (86). PCT No.: PCT/DE2010/075O13 (Continued) S371 (c)(1), Primary Examiner —Nathan Empie (2), (4) Date: Sep. 13, 2011 (74) Attorney, Agent, or Firm — Collard & Roe, P.C. (57) ABSTRACT (87) PCT Pub. No.: WO2010/088902 A method for producing alkali and alkaline earth alloys. It PCT Pub. Date: Aug. 12, 2010 also relates to the use of the alkali and alkaline earth compo sitions. In order to create a novel method for producing alkali (65) Prior Publication Data and alkaline earth alloys, it is proposed within the context of US 2012/O156379 A1 Jun. 21, 2012 the invention that salts, hydroxides, alkoxides or oxides of alkali or alkaline earth compounds be mixed with salts, (30) Foreign Application Priority Data hydroxides, alkoxides or oxides of semi-metals, nonmetals or metals and then heated to at least 100° C., the salts, hydrox Feb. 9, 2009 (DE) ......................... 10 2009 OO8144 ides, alkoxides or oxides of alkali or alkaline earth metals (51) Int. Cl. being present in a molar ratio of 1:1 or in excess thereof in B05D3/02 (2006.01) relation to the salts, hydroxide, alkoxides or oxides of the C22C I/00 (2006.01) semi-metals, nonmetals or metal. Surprisingly, it was found within the context of the invention that by mixing salts, (Continued) hydroxides, alkoxides or oxides of alkali or alkaline earth (52) U.S. Cl. compounds with salts, hydroxides, alkoxides or oxides of CPC ................. C22C I/00 (2013.01); B01J 21/063 semi-metals or metals from the 3rd or 4th main group and (2013.01); B01J 23/02 (2013.01); B01J 23/04 Subsequent heating, alkali or alkaline earth alloys can be (2013.01); produced. (Continued) 9 Claims, 1 Drawing Sheet Surface (>0.1mm) Surface (-0.1 nm) b c E15 sists 3X as 28 as 23 23 St SS S3 s as as 28 as Binding energy (eV) Binding energy (ew) sia M2 Surface (>0.1 mrin) Surface (-0.1 nm) 12 1 0 3 & 78 8 & 23 0 13s 9x 80 0 88 88 Binding energy (ew) Binding energy (ew) Photoelectron spectroscopy for a catalytically active coaling. US 9.249.480 B2 Page 2 (51) Int. Cl. FOREIGN PATENT DOCUMENTS BOI 2/06 (2006.01) DE 10 2005 O21 658 1, 2006 BOI. 23/02 (2006.01) DE 10 2005 O27 789 12/2006 BOI. 23/04 (2006.01) DE 10 2007 O16 946 10, 2008 WO WO 89,04716 6, 1989 BOI 35/00 (2006.01) WO WOO2,5O191 6, 2002 BOI. 37/02 (2006.01) WO WO 2006/036697 4/2006 WO WO 2007/095276 8, 2007 C22C 24/00 (2006.01) WO WO 2008/031101 3, 2008 (52) U.S. Cl. WO WO 2008/122266 10, 2008 WO WO 2008/131270 10, 2008 CPC ............ B01J 35/002 (2013.01); B01J 37/0215 OTHER PUBLICATIONS (2013.01); C22C 24/00 (2013.01); B01D 2255/202 (2013.01); B01D 2255/204 (2013.01); English translation of the International Preliminary Report on Pat BOID 2255/2027 (2013.01); B01D 2255/2045 entability for PCT/DE2010/0750 13, Aug. 11, 2011. Vorlow, S. et al., “The catalytic activity and selectivity of supported (2013.01); B01D 2255/2092 (2013.01); B01D vanadia catalysts doped with alkali metal Sulphates. I. Structural 2255/30 (2013.01); B01D 2258/012 (2013.01) re-organisations during pre-treatment and use. Applied Catalysis, 17(1), pp. 87-101, CODEN: APCADI; ISSN: 0166-9834, 1985, (56) References Cited XP002592568. (ISR) (Spec, p. 1-see Preliminary Amendment). Vorlow, S. et al., “The catalytic activity and selectivity of supported U.S. PATENT DOCUMENTS vanadia catalysts doped with alkali metal sulphates. III. The effect of variation in the chemical nature of the alkali metal.” Applied Cataly 3.996,335 A * 12, 1976 Wolk ..................... BO1D 53/52 sis, 17(1), pp. 115-125, (1985). 423,210.5 Reddy et al., “Influence of alkaline earth metal on acid-base charac 4,939,310 A * 7/1990 Wade ............................ 585,500 teristics of VOs/Mo TiO, (M=Ca,Sr and Ba) catalysts,” Journal of 5,011,548 A 4, 1991 Dean ............................... 148.27 Molecular Catalysis. A. Chemical, Elsevier, Amsterdam, NL, 5,068.483. A 11, 1991 Barthomeufetal. LNKD-DOI: 10.1016/J.MOLCATA2007.07.018, vol. 276, No. 1-2, 5,478,672 A * 12/1995 Mitate ........................... 429,224 Sep. 14, 2007, pp. 197-204, XP022248081, ISSN: 1381-1169. (ISR) 5,739,076 A * 4/1998 Huybrechts et al. ....... 562,512.4 (Spec, p. 1-see Preliminary Amendment). 6,245.306 B1* 6/2001 Miyazaki ............. BO1D 53,945 Zhao et al., “Effect of alkaline earth metals on catalytic performance 423,213.5 of HY zeolite for alkylation of O-methylnaphthalene with long-chain 7,247,350 B2 7/2007 Sepeur et al. olefins.” Microporous and Mesoporous Materials, Elsevier Science 2003/O103886 A1* 6/2003 Dou ................... BOD 53,8628 Publishing, New York, US, LNKD-DOI: 10.1016/J.MICROMESO. 423,239.1 2006.03.028, vol. 94, No. 1-3, Sep. 8, 2006, pp. 105-112, 2005/O151278 A1 7/2005 Lefenfeld et al. XP00560 1295, ISSN: 1387-1811. (ISR). 2009, 0238986 A1 9, 2009 Gross et al. 2010.0081569 A1 4/2010 Sepeur et al. * cited by examiner U.S. Patent Feb. 2, 2016 US 9.249,480 B2 Surface (> 0.1 nm) Surface (~ 0.1 nm) C 1s 150 6OO b) 140 550 K2p 30 SOO 120 450 11 O 400 ( 90100. 350 80 3OO 70 250 60 200 SO 150 OO Sz 2O 50 10 O O 310 305 300 295 290 285 280 275 310 305 300 295 290 28S 280 275 Binding energy (eV) Binding energy (eV) (Si2p) Na2s (sl2p) (Na2s) 450 Surface (>0.1 nm) Surface (~ 0.1 nm) 90 120 110 100 90 BO 70 60 SO 120 110 100 90 80 70 60 50 Binding energy (eV) Binding energy (eV) Photoelectron spectroscopy for a catalytically active coating. US 9.249,480 B2 1. 2 METHOD FOR PRODUCING ALKALIAND mixing salts, hydroxides, alkoxides or oxides of alkali or ALKALINE EARTHALLOYS AND USE OF alkaline earth compounds with salts, hydroxides, alkoxides or THE ALKALIAND ALKALINE EARTH oxides of semi-metals, non-metals or metals and Subsequent ALLOYS heating. The salts, hydroxides or alkoxides of alkali and alkaline CROSS REFERENCE TO RELATED earth compounds are preferably selected from the group con APPLICATIONS sisting of lithium nitrate, lithium formiate, lithium carbonate, lithium oxalate, lithium oxide, lithium hydroxide, lithium This application is the National Stage of PCT/DE2010/ alkoxide, lithium fluoride, lithium chloride, lithium bromide, 075013 filed on Feb. 9, 2010, which claims priority under 35 10 lithium iodide, lithium sulphate, lithium sulphite, lithium U.S.C. S 119 of German Application No. 10 2009 008 144.5 Sulphonate, lithium nitrite, lithium phosphite, lithium phos filed on Feb. 9, 2009, the disclosure of which is incorporated phate, lithium acetate, sodium nitrate, sodium formiate, by reference. The international application under PCT article Sodium carbonate, Sodium oxalate, sodium oxide, Sodium 21(2) was not published in English. hydroxide, Sodium alkoxide, Sodium fluoride, sodium chlo The invention relates to a method for producing alkali and 15 ride, Sodium bromide, sodium iodide, sodium Sulphate, alkaline earth alloys. It also relates to the use of the alkali and Sodium Sulphite, Sodium Sulphonate, sodium nitrite, Sodium alkaline earth compositions. phosphite, sodium phosphate, sodium acetate, potassium WO 2007/095276 A1 describes a method of removing nitrate, potassium formiate, potassium carbonate; potassium protective alkyl- or arylsulfonyl groups from a primary or oxalate, potassium oxide, potassium hydroxide, potassium secondary amine, wherein an alkyl- or arylsulfonamide is 20 alkoxid, potassium fluoride, potassium chloride, potassium preferably contacted with Na, KNa or KNa in the presence bromide, potassium iodide, potassium Sulphate, potassium of a proton source and under conditions that suffice for the Sulphite, potassium Sulphonate, potassium nitrite, potassium formation of the corresponding amine. phosphite, potassium phosphate, potassium acetate, rubidium WO 2008/031101A2 relates to lithium metal-porous oxide nitrate, rubidium formiate, rubidium carbonate, rubidium compositions (also termed “Group I metal/porous oxide com- 25 oxalate, rubidium oxide, rubidium hydroxide, rubidium positions”) prepared by mixing liquid lithium metal with a alkoxide, rubidium fluoride, rubidium chloride, rubidium porous metal oxide in an inert atmosphere under Sufficiently bromide, rubidium iodide, rubidium sulphate, rubidium sul exothermic conditions to enable the liquid lithium metal to be phite, rubidium sulphonate, rubidium nitrite, rubidium phos absorbed into the pores of the porous metal oxide. These phite, rubidium phosphate, rubidium acetate, caesium nitrate, compositions are used in organic reactions such as the 0 30 caesium formiate, caesium carbonate, caesium oxalate, cae synthesis.
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