Process and use of amino-functional resins for dismutating halosilanes and for removing extraneous metals

Patent metadata

Field	Value
Publication number	US-9908781-B2
Application number	US-201013383681-A
Country	US
Kind code	B2
Filing date	May 18, 2010
Priority date	Jul 15, 2009
Publication date	Mar 6, 2018
Grant date	Mar 6, 2018

Abstract

The invention relates to a process for dismutating at least one halosilane and reducing the content of extraneous metal and/or a compound containing extraneous metal in the at least one halosilane and in the at least one silane obtained, by contacting at least one halosilane of the general formula I, H n SiCl m (I), where n and m are integers and n=1, 2 or 3 and m=1, 2 or 3 and n+m=4, with a particulate, organic, amino-functional resin to obtain at least one silane of the general formula II, H a SiCl b (II), where a and b are integers and a=0, 2, 3 or 4 and b=0, 1, 2 or 4 where a+b=4, in one step, in which the content of extraneous metal and/or compounds containing extraneous metal has been reduced compared to the halosilane of the formula I. The invention further provides for the use of this resin for dismutating halosilanes and as an absorbent of extraneous metals or compounds containing extraneous metal in a process for preparing monosilane.

First claim

The invention claimed is:

1. A process for dismutating a trichlorosilane, the process comprising:
first washing a particulate, organic, amino-functional resin with deionized water, the resin comprising a dialkylamino- or dialkylaminomethylene-functionalized divinylbenzene-styrene copolymer or trialkylammonium- or trialkylammoniummethylene-functionalized divinylbenzene-styrene copolymer, to obtain a water-containing resin;
then applying reduced pressure or vacuum to the water-containing resin and regulating the temperature at below 200° C., and then removing the reduced pressure or vacuum, thereby obtaining an anhydrous and solvent-free catalyst resin having a water content of less than 2% by weight, without contacting the resin with an organic solvent after washing with the deionized water; and
conducting a reactive distillation or reactive rectification of a trichlorosilane-containing stream with the anhydrous and solvent-free catalyst resin, to obtain at least two silanes, thereby reducing a content of a compound comprising boron, iron, or both to less than 10 μg/kg,
wherein:
the at least two silanes are represented by formula (II):
H a SiCl b   (II);

a and b are integers;
a=0, 2, 3 or 4;
b=0, 1, 2 or 4;
a+b=4;
the catalyst resin, then contacted with the trichlorosilane, has a water content, if present, of less than 2% by weight and an organic solvent content, if present, of 2.5% by weight or less;
the content of the compound comprising boron, iron, or both is reduced by from 70 to 99% by weight; and
the reactive distillation or reactive rectification comprises reaction and distillative separation in one apparatus.

2. The process of claim 1 , wherein a silane of the at least two silanes comprises a monosilane which is distilled with the catalyst resin after the conducting and is decomposed thermally to ultrapure silicon.

3. The process of claim 1 , wherein contacting the trichlorosilane with the catalyst resin reduces a content of iron.

4. The process of claim 1 , wherein contacting the trichlorosilane with the catalyst resin reduces a content of boron.

5. The process of claim 1 , wherein the content of the compound comprising boron, iron, or both is reduced by from 95 to 99% by weight.

6. The process of claim 1 , wherein the catalyst resin, when contacted with the trichlorosilane, has an organic solvent content, if present, of 0.5% by weight or less.

7. The process of claim 1 , wherein the process does not comprise contacting either of the at least two silanes with activated carbon.

8. The process of claim 2 , wherein the process does not comprise any further purification step after the monosilane is distilled.

9. The process of claim 1 , wherein the catalyst resin has a water content of less than 0.8% by weight.

10. The process of claim 1 , wherein contacting trichlorosilane with the catalyst resin comprises supplying trichlorosilane is supplied batchwise to the catalyst resin.

11. The process of claim 1 , wherein the apparatus comprises a column.

12. The process of claim 11 , wherein the apparatus further comprises a side reactor assigned to the column.

Assignees

• Mueh Ekkehard
• Rauleder Hartwig
• Monkiewicz Jaroslaw
• Schork Reinhold
• Evonik Degussa Gmbh

Inventors

• Mueh Ekkehard
• Rauleder Hartwig
• Monkiewicz Jaroslaw
• Schork Reinhold

Classifications

• C01B33/10773

  Halogenated silanes obtained by disproportionation and molecular rearrangement of halogenated silanes · CPC title

• C01B33/10784

  by adsorption · CPC title

• C01P2006/80

  Compositional purity · CPC title

• C01B33/107 Primary

  Halogenated silanes · CPC title