Hydrogen gas recovery system and hydrogen gas separation and recovery method

Patent metadata

Field	Value
Publication number	US-10611635-B2
Application number	US-201615751359-A
Country	US
Kind code	B2
Filing date	Aug 2, 2016
Priority date	Aug 28, 2015
Publication date	Apr 7, 2020
Grant date	Apr 7, 2020

Abstract

A hydrogen gas recovery system according to the present ingestion is configured by a condensation and separation apparatus (A) that condenses and separates chlorosilanes from a hydrogen-containing reaction exhaust gas exhausted from a polycrystalline silicon production step, a compression apparatus (B) that compresses the hydrogen-containing reaction exhaust gas, an absorption apparatus (C) that absorbs and separates hydrogen chloride by contacting the hydrogen-containing reaction exhaust gas with an absorption liquid, a first adsorption apparatus (D) comprising an adsorption column filled with activated carbon for adsorbing and removing methane, hydrogen chloride, and part of the chlorosilanes each contained in the hydrogen-containing reaction exhaust gas, a second adsorption apparatus (E) comprising an adsorption column filled with synthetic zeolite that adsorbs and removes methane contained in the hydrogen-containing reaction exhaust gas, and a gas line (F) that recovers a purified hydrogen gas having a reduced concentration of methane.

First claim

The invention claimed is:

1. A hydrogen gas recovery system for separating and recovering a hydrogen gas from a reaction exhaust gas exhausted from an apparatus for producing polycrystalline silicon using trichlorosilane as a raw material, the system comprising:
A: a condensation and separation apparatus configured to condense and separate chlorosilanes from a hydrogen-containing reaction exhaust gas exhausted from a polycrystalline silicon production;
B: a compression apparatus configured to compress the hydrogen-containing reaction exhaust gas that has passed through the condensation and separation apparatus;
C: an absorption apparatus configured to absorb and separate hydrogen chloride by contacting the hydrogen-containing reaction exhaust gas that has passed through the compression apparatus with an absorption liquid;
D: a first adsorption apparatus comprising at least one first adsorption column filled with activated carbon that adsorbs and removes methane, hydrogen chloride, and part of the chlorosilanes from the hydrogen-containing reaction exhaust gas that has passed through the absorption apparatus;
E: a second adsorption apparatus comprising at least one second adsorption column filled with synthetic zeolite that adsorbs and removes methane contained in the hydrogen-containing reaction exhaust gas that has passed through the first adsorption apparatus, the synthetic zeolite being a ferrierite having a molecular ratio of silica (SiO 2 ) to alumina (Al 2 O 3 ) (SiO 2 /Al 2 O 3 ) of from 15 to 20 and comprising at least one positive ion selected from the group consisting of potassium, magnesium, and barium; and
F: a first gas line configured to recover a purified hydrogen gas having a reduced concentration of methane, the purified hydrogen gas having been exhausted from the second adsorption apparatus,
wherein the purified hydrogen gas has a concentration of methane of 1 ppm or less.

2. The hydrogen gas recovery system according to claim 1 ,
wherein each of the silica (SiO 2 ) and alumina (Al 2 O 3 ) is a main component of the synthetic zeolite.

3. The hydrogen gas recovery system according to claim 1 , wherein the first adsorption apparatus comprises a plurality of the first adsorption columns filled with the activated carbon.

4. The hydrogen gas recovery system according to claim 1 , wherein the second adsorption apparatus comprises a plurality of the second adsorption columns filled with the synthetic zeolite.

5. The hydrogen gas recovery system according to claim 1 , further comprising a second gas line configured to utilize the purified hydrogen gas as a carrier gas to be used for regenerating at least one of the activated carbon in the first adsorption column and the synthetic zeolite in the second adsorption column.

6. The hydrogen gas recovery system according to claim 1 , further comprising: a third gas line configured to utilize the purified hydrogen gas as a carrier gas to be used for regenerating the synthetic zeolite in the second adsorption column; and a fourth gas line configured to utilize an exhaust gas exhausted during the regeneration of the synthetic zeolite in the second adsorption column as a carrier gas to be used for regenerating the activated carbon in the first adsorption column.

7. A hydrogen gas separation and recovery method for separating and recovering a hydrogen gas from a reaction exhaust gas exhausted from an apparatus for producing polycrystalline silicon using trichlorosilane as a raw material,
the method using the hydrogen gas recovery system according to claim 1 , and the method comprising:
purifying the hydrogen gas to a concentration of methane in the hydrogen gas of 1 ppm or less with the second adsorption apparatus, and then
recovering the purified hydrogen gas.

8. The hydrogen gas separation and recovery method according to claim 7 , comprising purifying the hydrogen gas to a concentration of hydrogen chloride in the hydrogen gas of 100 ppmv or less and a concentration of chlorosilanes in the hydrogen gas of 100 ppmv or less with the first adsorption apparatus.

9. The hydrogen gas separation and recovery method according to claim 7 , comprising regenerating the synthetic zeolite in the second adsorption column under a condition where a pressure in the second adsorption column is 0.3 MPa or less.

Assignees

• Shinetsu Chemical Co

Inventors

• Ishida Masahiko
• Netsu Shigeyoshi
• Saito Hiroshi
• Tanaka Shuji

Classifications

• B01D2257/102

  Nitrogen · CPC title

• C01B7/03

  Preparation from chlorides · CPC title

• C01B33/035

  by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process · CPC title

• B01J20/3416

  of sorbents or filter aids comprising free carbon, e.g. activated carbon · CPC title

• B01D53/75

  Multi-step processes · CPC title