Method for producing perhalogenated hexasilane anion and method for producing a cyclic silane compound
The present invention relates to a process for the production of perhalogenated hexasilane anion by reacting halogenated monosilane in the presence of organosubstituted ammonium and/or phosphonium halide at temperatures in a range from 100 to 120° C., wherein no solvent is used, and a process for the production of a cyclic silane compound of the formula Si 6 R 12 , by reacting [X] 2 [Si 6 Cl 14 ] with AlR 3 in at least one organic solvent, wherein R is chlorine or methyl and X, the same or different, is a counter-cation and is preferably selected from organosubstituted ammonium, organosubstituted phosphonium, alkali metal ions and [(PEDETA)(H 2 SiCl)]+.
1. A process for the production of perhalogenated hexasilane anion by reacting halogenated monosilane in the presence of organosubstituted ammonium and/or phosphonium halide at temperatures in a range from 100 to 120° C., followed by removal of by-products comprising hydrogen by raising and releasing pressure, wherein no solvent is used,
wherein said organosubsitutued ammonium and/or phosphonium halide is substituted with at least one substituent selected from the group consisting of aryl, alkyl and alkenyl.
2. The process for the production of perhalogenated hexasilane anion as claimed in claim 1 , wherein the halogenated monosilane is trichlorosilane or dichlorosilane.
3. The process for the production of perhalogenated hexasilane anion as claimed in claim 1 , wherein no additional Lewis base is added.
4. The process for the production of perhalogenated hexasilane anion as claimed in claim 1 , wherein the reaction time is 12 to 96 hours.
5. The process for the production of perhalogenated hexasilane anion as claimed in claim 1 , wherein the weight ratio of halogenated monosilane to organosubstituted ammonium and/or phosphonium halide is 3:1 to 50:1.
6. The process for the production of perhalogenated hexasilane anion as claimed in claim 1 , wherein the organosubstituted ammonium and/or phosphonium halide is selected from [nBu 4 N]Cl, [Et 4 N]Cl, [Ph 4 P]Cl and [nBu 4 P]Cl.
7. A process for the production of a cyclic silane compound of the formula Si 6 R 12 where R is a halogen, comprising:
producing perhalogenated hexasilane anion by reacting halogenated monosilane in the presence of organosubstituted ammonium and/or phosphonium halide at temperatures in a range from 100 to 120° C., followed by removal of by-products comprising hydrogen by raising and releasing pressure, wherein no solvent is used,
wherein said organosubsitutued ammonium and/or phosphonium halide is substituted with at least one substituent selected from the group consisting of aryl, alkyl and alkenyl, and reacting said perhalogenated hexasilane anion with AlR′ 3 in at least one organic solvent, wherein R′ is chlorine or methyl.
8. The process for the production of a cyclic silane compound as claimed in claim 7 , wherein the organic solvent is selected from benzene, cyclohexane, n-hexane, n-heptane, chloroform and dichloromethane.
9. The process for the production of a cyclic silane compound as claimed in claim 7 , wherein the process is carried out in a temperature range from 20° C. to 120° C.
10. The process for the production of a cyclic silane compound as claimed in claim 7 , wherein the weight ratio of perhalogenated hexasilane anion to AlR′ 3 lies in a range of 5:1 to 1:10.
11. The process as claimed in claim 7 , wherein the Si 6 Cl 12 obtained is cleaved in a subsequent reaction.