IP Library Granted Patent US 9,352,971
Granted Patent B2
US 9,352,971 · App. 13/918,609 · Granted May 31, 2016

Method and apparatus for production of silane and hydrohalosilanes

Inventor: William C. Breneman (Moses Lake, WA)
Assignee: REC Silicon Inc
C01B33/043B01D3/009C01B33/107C01B33/1071
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Quick Facts
Patent No.
US 9,352,971
App. No.
13/918,609
Granted
May 31, 2016
Kind
B2
Abstract

Silane and hydrohalosilanes of the general formula H y SiX 4-y (y=1, 2, or 3) are produced by reactive distillation in a system that includes a fixed-bed catalytic redistribution reactor that can be back-flushed during operation.

Claims (36)

1. A system for producing silane and hydrohalosilanes, comprising:

(a) a multi-zone fractional distillation column ( 1 ) comprising

a vessel defining a plurality of distillation zones, having a reactant stream inlet ( 15 ) positioned in a lower portion of the column, a distillate stream outlet ( 14 ) positioned in an upper portion of the column, and a product stream inlet ( 3 ) positioned in a lower portion of the column;

(b) a first catalytic redistribution reactor ( 6 ) comprising

a vessel defining a chamber, the vessel having a first reactor lower port ( 8 ) positioned in a lower portion of the vessel and a first reactor upper port ( 9 ) positioned in an upper portion of the vessel,

a fixed-bed catalyst disposed within the chamber between the first reactor lower port ( 8 ) and the first reactor upper port ( 9 ), and

a plurality of valves ( 10 ), ( 11 ), ( 12 ), ( 13 ), wherein when valves ( 10 ) and ( 12 ) are open and valves ( 11 ) and ( 13 ) are closed, the first reactor lower port ( 8 ) is in fluid communication with the product stream inlet ( 3 ) and the first reactor upper port ( 9 ) is in fluid communication with the distillate stream outlet ( 14 ), and when valves ( 11 ) and ( 13 ) are open and valves ( 10 ) and ( 12 ) are closed, then the first reactor lower port ( 8 ) is in fluid communication with the distillate stream outlet ( 14 ) and the first reactor upper port ( 9 ) is in fluid communication with the product stream inlet ( 3 );

(c) a second catalytic redistribution reactor ( 6 a ) comprising

a vessel defining a chamber, the vessel having a second reactor lower port ( 8 a ) positioned in a lower portion of the vessel, and a second reactor upper port ( 9 a ) positioned in an upper portion of the vessel,

a fixed-bed catalyst disposed within the chamber between the second reactor lower port ( 8 a ) and the second reactor upper port ( 9 a ), and

a plurality of valves ( 10 a ), ( 11 a ), ( 12 a ), ( 13 a ), wherein when valves ( 10 a ) and ( 12 a ) are open and valves ( 11 a ) and ( 13 a ) are closed, the second reactor lower port ( 8 a ) is in fluid communication with the product stream inlet ( 3 ) and the second reactor upper port ( 9 a ) is in fluid communication with the distillate stream outlet ( 14 ), and when valves ( 11 a ) and ( 13 a ) are open and valves ( 10 a ) and ( 12 a ) are closed, then the second reactor lower port ( 8 a ) is in fluid communication with the distillate stream outlet ( 14 ) and the second reactor upper port ( 9 a ) is in fluid communication with the product stream inlet ( 3 ); and

(d) a pump ( 4 ) positioned downstream from the distillate stream outlet ( 14 ) and upstream from the first catalytic redistribution reactor ( 6 ) and the second catalytic redistribution reactor ( 6 a ).

2. The system of claim 1 , further comprising a cooling device ( 5 ) positioned downstream of the distillate stream outlet ( 14 ).

3. The system of claim 1 , wherein the valves ( 10 ), ( 12 ), ( 10 a ), and ( 12 a ) are configured to provide a greater flow rate of the distillate (B) than the valves ( 11 ), ( 13 ), ( 11 a ), and 13 ( a ).

4. The system of claim 3 , wherein the valves ( 10 ), ( 12 ), ( 10 a ), and ( 12 a ) are configured to provide a flow rate of the distillate (B) that is at least 9-fold greater than the flow rate through the valves ( 11 ), ( 13 ), ( 11 a ), and 13 ( a ).

5. The system of claim 1 , wherein the fixed-bed catalyst in the first catalytic redistribution reactor ( 6 ) and the second catalytic redistribution reactor ( 6 a ) is an ion-exchange resin.

6. The system of claim 5 , wherein the ion-exchange resin comprises a plurality of particles differing in size.

7. A method for producing silane and hydrohalosilanes, comprising:

passing a reactant stream (A) comprising one or more hydrohalosilanes of formula H y SiX 4-y where X is a halogen and y is 1, 2, or 3 into a multi-zone fractional distillation column ( 1 ) comprising a vessel defining a plurality of distillation zones, wherein the reactant stream (A) is passed into the multi-zone fractional distillation column ( 1 ) through a reactant stream inlet ( 15 ) positioned in a lower portion of the column ( 1 );

pumping a distillate (B) from the multi-zone fractional distillation column ( 1 ) via a distillate stream outlet ( 14 ) positioned in an upper portion of the column ( 1 ) through (i) a first catalytic redistribution reactor ( 6 ) comprising a vessel defining a chamber, a fixed-bed catalyst disposed within the chamber, a first reactor lower port ( 8 ) positioned in a lower portion of the first reactor, and a first reactor upper port ( 9 ) positioned in an upper portion of the first reactor ( 6 ), and (ii) a second catalytic redistribution reactor ( 6 a ) comprising a vessel defining a chamber, a fixed-bed catalyst disposed within the chamber, a second reactor lower port ( 8 a ) positioned in a lower portion of the second reactor ( 6 a ), and a second reactor upper port ( 9 a ) positioned in an upper portion of the second reactor ( 6 a ), thereby routing a first portion of the distillate (B) into the first catalytic redistribution reactor ( 6 ) via the first reactor upper port ( 9 ) and routing a first portion of a product stream (C) out of the first catalytic redistribution reactor ( 6 ) via the first reactor lower port ( 8 ), and further routing a second portion of the distillate (B) into the second catalytic redistribution reactor ( 6 a ) via the second reactor lower port ( 8 a ) and routing a second portion of the product stream (C) out of the second catalytic redistribution reactor ( 6 a ) via the second reactor upper port ( 9 a ), thereby back-flushing the second catalytic redistribution reactor ( 6 a ); and

flowing the product stream (C) into the multi-zone fractional distillation column ( 1 ) via a product stream inlet ( 3 ) positioned in a lower portion of the multi-zone fractional distillation column ( 1 ).

8. The method of claim 7 , wherein pumping the distillate comprises pumping the distillate to the first catalytic redistribution reactor ( 6 ) via the first reactor upper port ( 9 ) at a greater flow rate than a flow rate to the second catalytic redistribution reactor ( 6 a ) via the second reactor lower port ( 8 a ).

9. The method of claim 8 , wherein the flow rate to the first catalytic redistribution reactor ( 6 ) is at least 9-fold greater than the flow rate to the second catalytic redistribution reactor ( 6 a ).

10. The method of claim 7 , further comprising:

monitoring a pressure drop within the first catalytic redistribution reactor ( 6 );

determining whether the pressure drop exceeds a threshold value; and

reversing a direction of flow through the first catalytic redistribution reactor ( 6 ) and the second catalytic redistribution reactor ( 6 a ) when the pressure drop exceeds the threshold value.

11. The method of claim 10 , wherein reversing the direction of flow comprises:

routing a portion of the distillate (B) into the first catalytic redistribution reactor ( 6 ) via the first reactor lower port ( 8 ) and routing a portion of the product stream (C) out of the first catalytic redistribution reactor ( 6 ) via the first reactor upper port ( 9 ); and

routing a subsequent portion of the distillate (B) into the second catalytic redistribution reactor ( 6 a ) via the second reactor upper port ( 9 a ) and routing a subsequent portion of the product stream (C) out of the second catalytic redistribution reactor ( 6 a ) via the second reactor lower port ( 8 a ), thereby reversing the direction of flow through the first catalytic redistribution reactor ( 6 ) and the second catalytic redistribution reactor ( 6 a ).

12. The method of claim 11 , wherein reversing the direction of flow further comprises pumping the distillate to the second catalytic redistribution reactor ( 6 a ) via the second reactor upper port ( 9 a ) at a greater flow rate than a flow rate to the first catalytic redistribution reactor ( 6 ) via the first reactor lower port ( 8 ).

13. The method of claim 10 , further comprising:

monitoring a subsequent pressure drop within the second catalytic redistribution reactor ( 6 a );

determining whether the subsequent pressure drop exceeds the threshold value; and

reversing the direction of flow through the first catalytic redistribution reactor ( 6 ) and the second catalytic redistribution reactor ( 6 a ) when the subsequent pressure drop exceeds the threshold value.

14. The method of claim 7 , further comprising cooling the distillate (B) before pumping the distillate (B) through the first catalytic redistribution reactor ( 6 ) and the second catalytic redistribution reactor ( 6 a ).

Assignments (2)
SECURITY INTEREST Recorded Jan 24, 2025
From: REC SILICON INC; REC ADVANCED SILICON MATERIALS LLC
To: HANWHA INTERNATIONAL LLC, AS LENDER
Reel/Frame 070002/0600 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 1, 2013
From: BRENEMAN, WILLIAM C.
To: REC SILICON INC
Reel/Frame 031323/0012 →
Continuity (1)
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