# US 2013/0156675 A1 · Process for production of silane and hydrohalosilanes

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- Number: US 2013/0156675 A1
- Document ID: US20130156675A1
- Status: Published application
- Kind: A1
- Application number: 13/328,820
- Filed: 2011-12-16
- Published: 2013-06-20
- Earliest claimed: 2011-12-16
- Assignees: REC Silicon Inc
- Inventors: William C. Breneman
- Web page: https://patentgrep.com/patent/US20130156675A1

## CPC

- C01B 33/043: {Monosilane}
- C01B 33/1071: {Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof}
- C01B 33/10778: {Purification}
- Y02P 20/10: Process efficiency
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Embodiments of a system and process for the production of ultra-high purity silane and hydrohalosilanes of the general formula HySiX4-y (y=1, 2, or 3) by a reactive distillation method are disclosed.

## Claims

### Claim 1

A system for producing hydrosilanes, comprising:
(a) a first multi-zone fractional distillation column (2) comprising
a vessel defining a plurality of distillation zones,
a reactant stream inlet (1),
a first distillate stream outlet (5) positioned above the reactant stream inlet (1),
a first product flow inlet (8) positioned between the reactant stream inlet (1) and the first distillate stream outlet (5),
a bottom outlet (31), and
a vapor outlet (32) positioned above the first distillate stream outlet (5);
(b) a first catalytic redistribution reactor (7) comprising
a vessel defining a chamber,
an inlet (7a),
a product flow outlet (7b) spaced apart from the inlet (7a), and
a fixed-bed catalyst disposed within the chamber between the inlet (7a) and the product flow outlet (7b), wherein the product flow outlet (7b) is in communication with the first product flow inlet (8) of the first multi-zone fractional distillation column (2), and wherein the first catalytic redistribution reactor (7) does not include a pressure equilibrium outlet or a vapor return outlet;
(c) a first pump (6) operable to pump a first distillate stream (B) from the first distillate stream outlet (5) into the first catalytic redistribution reactor (7); and
(d) a condenser (28) in communication with the vapor outlet (32) of the first multi-zone fractional distillation column (2).

### Claim 2 (depends on 1)

The system of claim 1, further comprising a second condenser (29) in fluid communication with an outlet of the condenser (28).

### Claim 3 (depends on 1)

The system of claim 1, further comprising a reactant source operably coupled to the reactant stream inlet (1) and capable of providing a reactant stream (A) to the first multi-zone fractional distillation column (2).

### Claim 4 (depends on 1)

The system of claim 1, further comprising:
(d) a second catalytic redistribution reactor (12) comprising
a vessel defining a chamber,
an inlet (12a),
a product flow outlet (12b) spaced apart from the inlet (12a), and
a fixed-bed catalyst disposed within the chamber between the inlet (12a) and the product flow outlet (12b), wherein the second catalytic redistribution reactor (12) does not include a pressure equilibrium outlet or a vapor return outlet; and
(e) a second pump (11) operable to pump a condensate (F) from the condenser (28) into the second catalytic redistribution reactor (12).

### Claim 5 (depends on 4)

The system of claim 4, further comprising:
(f) a second multi-zone fractional distillation column (14) comprising
a vessel defining a plurality of distillation zones,
a second multi-zone fractional distillation column inlet (13) operably coupled to the product flow outlet (12b) of the second catalytic redistribution reactor (12),
a second outlet (19) positioned above the inlet (13),
a purge stream outlet (18) positioned above the second outlet (19). and
a bottom outlet (20).

### Claim 6

A method for producing hydrosilanes, comprising:
passing a reactant stream (A) comprising one or more hydrohalosilanes of formula HySiX4-y where X is a halogen and y is 1, 2, or 3 into a first multi-zone fractional distillation column (2) comprising a vessel defining a plurality of distillation zones including a first distillation zone (Z1) and a second distillation zone (Z2) located above the first distillation zone (Z1), wherein the reactant stream (A) is passed into the first multi-zone distillation column (2) through a reactant stream inlet (1) positioned at a height corresponding to the height of the first distillation zone (Z1);
maintaining the first distillation zone (Z1) at a temperature T1 that corresponds to a boiling point of the reactant stream at a pressure within the vessel;
maintaining the second distillation zone (Z2) at a temperature T2 at which liquid and/or vapor in the second distillation zone (Z2) has a halogen to silicon molar ratio between 2.8 and 3.2;
pumping a first distillate stream (B) from the first multi-zone fractional distillation column (2) via a first distillate stream outlet (5) positioned at a height corresponding to the height of the second distillation zone (Z2) through a first fixed-bed catalytic redistribution reactor (7) that does not include a pressure equilibrium outlet or a vapor return outlet to form a first product flow (C), and then back into the first multi-zone distillation column (2) via a first product flow inlet (8) positioned below the first distillate stream outlet (5) and above the reactant stream inlet (1); and
passing vapor (E) from an upper portion of the first multi-zone fractional distillation column (2) to a condenser (28) to produce a condensate (F) comprising HzSiX4-z where z=y+1.

### Claim 7 (depends on 6)

The method of claim 6, wherein the reactant stream (A) comprises trichlorosilane.

### Claim 8 (depends on 7)

The method of claim 7, wherein the first product flow (C) comprises at least 5% less trichlorosilane than the first distillate stream (B).

### Claim 9 (depends on 7)

The method of claim 7, wherein the condensate (F) comprises dichlorosilane.

### Claim 10 (depends on 6)

The method of claim 6, wherein the pressure within the vessel is from 450 kPa to 1750 kPa.

### Claim 11 (depends on 10)

The method of claim 10, wherein T2 is from 60° C. to 150° C.

### Claim 12 (depends on 10)

The method of claim 10, wherein the halogen to silicon molar ratio is 2.8-3.1.

### Claim 13 (depends on 6)

The method of claim 6, further comprising:
pumping the condensate (F) through a second fixed-bed catalytic redistribution reactor (12) that does not include a pressure equilibrium outlet or a vapor return outlet to produce a second product flow (G), which subsequently passes into a second multi-zone fractional distillation column (14) comprising a vessel defining a plurality of distillation zones and including a second multi-zone fractional distillation column inlet (13) positioned at a height corresponding to a distillation zone (Z3) located within the second multi-zone fractional distillation column (14) wherein the distillation zone (Z3) has a temperature corresponding to a boiling point of the second product flow (G) at a pressure within the region; and
withdrawing silane (H) from the second multi-zone distillation column through a second multi-zone fractional distillation column outlet (19) positioned above the second multi-zone fractional distillation column inlet (13).

### Claim 14 (depends on 13)

The method of claim 13, further comprising withdrawing a purge stream (I) comprising gaseous impurities from a top outlet (18) of the second multi-zone fractional distillation column (14).