Process and device for the production of polyhedral boranes
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C07F-005/02
C07C-211/63
C01B-035/02
출원번호
US-0357684
(2012-11-16)
등록번호
US-9598352
(2017-03-21)
국제출원번호
PCT/US2012/065495
(2012-11-16)
국제공개번호
WO2013/115889
(2013-08-08)
발명자
/ 주소
Lee, Mark Wayne
Hawthorne, Marion Frederick
출원인 / 주소
The Curators of the University of Missouri
대리인 / 주소
Polsinelli PC
인용정보
피인용 횟수 :
0인용 특허 :
9
초록▼
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 i
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.
대표청구항▼
1. A process for the production of a polyhedral borane in an amount greater than one kilogram, wherein the process comprises a solid-phase, anhydrous, one-pot reaction of a tetraborohydride and a quaternary amine salt under anhydrous pyrolytic reaction conditions without solvent, resulting in the fo
1. A process for the production of a polyhedral borane in an amount greater than one kilogram, wherein the process comprises a solid-phase, anhydrous, one-pot reaction of a tetraborohydride and a quaternary amine salt under anhydrous pyrolytic reaction conditions without solvent, resulting in the formation of the polyhedral borane. 2. The process of claim 1, wherein the tetraborohydride is chosen from sodium borohydride, potassium borohydride, and lithium borohydride. 3. The process of claim 1, wherein the quaternary amine salt of Formula (I), wherein L1-4are independently chosen from hydrogen, hydrocarbyl, and substituted hydrocarbyl, and X−is chosen from F−, Cl−, Br−, I−, and OH− 4. The process of claim 1, wherein the quaternary amine salt is tetraethyl ammonium chloride. 5. The process of claim 1, wherein the pyrolytic conditions comprise a temperature of at least 180° C., and a pressure of at least 0.5 atmospheres. 6. The process of claim 1, wherein the reaction time is at least 5 hours. 7. The process of claim 1, wherein the polyhedral borane is a borane anion. 8. The process of claim 7, wherein the borane anion is B10H102−or B12H122−. 9. The process of claim 1, wherein the reaction occurs in the presence of a catalyst. 10. The process of claim 9, wherein the catalyst is a Lewis acid in a ratio of about 0.1 to about 5 mol% of the tetraborohydride. 11. The process of claim 1, wherein the tetraborohydride and the quaternary amine salt are present in a ratio between 1:1.3 to 1:1.5. 12. The process of claim 1, wherein B10H102−is selectively produced in a yield of at least about 40%. 13. The process of claim 1, wherein B12H122−is selectively produced in a yield of at least about 50%. 14. The process of claim 1, wherein the pyrolytic reaction occurs in a milling reactor. 15. A process for the selective formation of B12H122−over B10H102−in an amount greater than one kilogram, the process comprising (a) combining a borohydride with a quaternary amine salt to form an anhydrous reaction mixture; and (b) subjecting the anhydrous reaction mixture to solid-phase, anhydrous pyrolytic reaction conditions without solvent, comprising at least a temperature of 180° C. for at least 12 hours such that the majority of the borohydride is converted to B12H122−. 16. The process of claim 15, further comprising the steps of: (a) quenching the pyrolytic reaction with a quench reagent, and(b) purifying the resultant reaction mixture to isolate one or more polyhedral boranes. 17. The process of claim 16, wherein the quench reagent is selected from weak acids and bases. 18. The process of claim 17, wherein the quench reagent is acetic acid. 19. The process of claim 16, wherein purification is accomplished by washing the reaction mixture with an alcohol chosen from methanol, ethanol, propanol, allyl alcohol, and butanol. 20. The process of claim 19, wherein the alcohol is methanol.
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이 특허에 인용된 특허 (9)
Hawthorne, M. Frederick; Peymann, Toralf; Maderna, Andreas, Ether and ester derivatives of the perborate icosahedron.
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