IP Library Granted Patent US 8,722,913
Granted Patent B2
US 8,722,913 · App. 12/524,371 · Granted May 13, 2014

Method for producing higher silanes

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Quick Facts
Patent No.
US 8,722,913
App. No.
12/524,371
Granted
May 13, 2014
Kind
B2
Abstract

The invention relates to a method for producing dimeric and/or trimeric silicon compounds, in particular silicon halogen compounds. The claimed method is also suitable for producing corresponding germanium compounds. The invention also relates to a device for carrying out said method to the use of the produced silicon compounds.

Claims (50)

1. A process, comprising:

reacting, in a nonthermal plasma, a silicon compound represented by formula (IIa) or a germanium compound represented by formula (IIb)

to obtain a silicon compound represented by formula (Ia) or a germanium compound represented by formula (Ib)

and, thereafter

recovering said compound represented by formula (Ia) or said compound represented by formula (Ib) from a phase that comprises said compound represented by formula (Ia) or said compound represented by formula (Ib),

wherein

each R1 to R8 radical is independently a hydrogen or a halogen selected from the group consisting of chlorine, bromine and iodine, with the proviso that at least one of the R1 to R8 radicals is a halogen, and n=0 or 1,

each R9 to R12 is independently a hydrogen; an organyl, where the organyl comprises a linear, branched or cyclic alkyl having 1 to 18 carbon atoms, linear, branched or cyclic alkenyl having 2 to 8 carbon atoms, unsubstituted or substituted aryl and/or corresponding benzyl; or a halogen selected from the group consisting of chlorine, bromine and iodine, and n=1 or 2,

said reacting of the silicon compound of formula (IIa) is carried out in the presence of at least one compound represented by formula (IIIa)

or

and said reacting of the germanium compound of formula (IIb) is carried out in the presence of at least one compound represented by formula (IIIb)

where each R13 to R16 radical is independently a hydrogen; an organyl, where the organyl comprises a linear, branched or cyclic alkyl having 1 to 18 carbon atoms, linear, branched or cyclic alkenyl having 2 to 8 carbon atoms, unsubstituted or substituted aryl or corresponding benzyl; or a halogen selected from the group consisting of chlorine, bromine and iodine, n=1 or 2, and

wherein said reacting is carried out in the absence of a reducing agent.

2. The process as claimed in claim 1 , wherein said recovering comprises distilling said compound represented by formula (Ia) or said compound represented formula (Ib) from the phase that comprises said compound represented by formula (Ia) or said compound represented by formula (Ib).

3. The process as claimed in claim 1 , said process comprising reacting, in a nonthermal plasma, a silicon tetrachloride compound represented by formula (IIa), where R9 to R12=chlorine and n=1, and at least one further hydrogen-containing compound represented by formula (IIIa).

4. The process as claimed in claim 3 , wherein

the hydrogen-containing compound represented by formula (IIIa) is at least one compound selected from the group consisting of methyltrichlorosilane, trichlorosilane, dichlorosilane, monochlorosilane, monosilane and dimethyldichlorosilane.

5. The process as claimed in claim 1 , wherein at least one of said reacting and said recovering occurs continuously.

6. The process as claimed in claim 1 , wherein

said reacting is carried out in an apparatus comprising a collecting vessel, and said

silicon compound represented by formula (Ia) obtained from said recovering is isolated to said collecting vessel.

7. The process as claimed in claim 1 , wherein

said recovering is carried out in a continuous process regime and effected by distillation in a column system comprising at least two columns, and in a batchwise process regime with at least one column.

8. The process as claimed in claim 2 , wherein

said distilling is carried out under standard pressure, reduced pressure or elevated pressure.

9. The process as claimed in claim 2 , wherein

said distilling is carried out at a pressure in the range from 1 to 1500 mbar abs .

10. The process as claimed in claim 2 , wherein

said distilling is a distillation of the silicon compound of the formula (Ia), which occurs at top temperatures in the range from 40 to 250° C.

11. The process as claimed in claim 1 , wherein

said reacting occurs at pressures in the range from 1 to 1000 mbar abs .

12. The process as claimed in claim 1 , wherein

the silicon compound represented by formula (Ia) is at least one of hexachlorodisilane and octachlorotrisilane.

13. The process as claimed in claim 1 , wherein

the silicon compound of formula (Ia) has at least a purity in the ppb range.

14. The process according to claim 1 , wherein at least one compound represented by Formula (IIIa), at least one compound represented by Formula (IIIb), or a combination thereof, is a hydrogen-containing compound.

15. The process as claimed in claim 1 , wherein the silicon compound of formula (Ia) has a purity in the ppt range.

16. A process, comprising:

reacting, in a nonthermal plasma, a silicon compound represented by formula (IIa) or a germanium compound represented by formula (IIb)

to obtain a silicon compound represented by formula (Ia) or a germanium compound represented by formula (Ib)

and, thereafter

recovering said compound represented by formula (Ia) or said compound represented by formula (Ib) from a phase that comprises said compound represented by formula (Ia) or said compound represented by formula (Ib),

wherein

each R1 to R8 radical is independently a hydrogen or a halogen selected from the group consisting of chlorine, bromine and iodine, with the proviso that at least one of the R1 to R8 radicals is a halogen, and n=0 or 1,

each R9 to R12 is independently a hydrogen; an organyl, where the organyl comprises a linear, branched or cyclic alkyl having 1 to 18 carbon atoms, linear, branched or cyclic alkenyl having 2 to 8 carbon atoms, unsubstituted or substituted aryl and/or corresponding benzyl; or a halogen selected from the group consisting of chlorine, bromine and iodine, and n=1 or 2,

said reacting of the silicon compound of formula (IIa) is carried out in the presence of at least one compound represented by formula (IIIa)

or

and said reacting of the germanium compound of formula (IIb) is carried out in the presence of at least one compound represented by formula (IIIb)

where each R13 to R16 radical is independently a hydrogen; an organyl, where the organyl comprises a linear, branched or cyclic alkyl having 1 to 18 carbon atoms, linear, branched or cyclic alkenyl having 2 to 8 carbon atoms, unsubstituted or substituted aryl or corresponding benzyl; or a halogen selected from the group consisting of chlorine, bromine and iodine, n=1 or 2, and

wherein said reacting is carried out in the absence of hydrogen.

Assignments (2)
CHANGE OF NAME Recorded Jan 31, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051765/0166 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 30, 2009
From: LANG, JUERGEN ERWIN; RAULEDER, HARTWIG; MUEH, EKKEHARD
To: EVONIK DEGUSSA GMBH
Reel/Frame 023026/0313 →