Compositional analysis of a gas or gas stream in a chemical reactor and method for preparing chlorosilanes in a fluidized bed reactor

Patent metadata

Field	Value
Publication number	US-10031082-B2
Application number	US-201414899147-A
Country	US
Kind code	B2
Filing date	Jun 17, 2014
Priority date	Jul 2, 2013
Publication date	Jul 24, 2018
Grant date	Jul 24, 2018

Abstract

The composition of a gas or gas stream containing AlCl3 in a chemical reactor is measured by removing AlCl3 from the gas and analyzing the gas by gas chromatography or spectroscopy. Chlorosilanes may be prepared in a fluidized bed reactor having a reactor height H0, in which supplied HCl reacts with silicon, wherein a temperature profile in the fluidized bed reactor is greater than S1(H/H0)=(a1−b1)*(1/(1+exp(−c1((H/H0)−d1))))+b1 and less than S2(H/H0)=(a2−b2)*(1/(1+exp(−c2((H/H0)−d2))))+b2, where a1=100° C., a2=300° C., b1=300° C., b2=400° C., c1=50, c2=20, d1=0.2, and d2=0.8.

First claim

The invention claimed is:

1. A method for analyzing the composition of a gas or gas stream comprising AlCl 3 exiting a fluidized bed chemical reactor having a reactor height H0 in which HCI reacts with Si forming chlorosilanes, comprising removing AlCl 3 from the gas or gas stream, subsequently analyzing the gas or gas stream by means of on-line gas chromatography or spectroscopy, and employing the results of analyzing the gas or gas stream to establish or modify a temperature profile in the reactor as a function of reactor height by changing at least one reactor operating parameter, wherein the temperature profile in the fluidized bed chemical reactor having a reactor height H0, is above S1(H/H0)=(a1−b1)*(1/(1+exp(−c1((H/H0)−d1))))+b1 and below S2(H/H0)=(a2−b2)*(1/(1+exp(−c2((H/H0)−d2))))+b2, where a1=100° C., a2=300° C., b1=300° C., b2=400° C., c1=50, c2=20, d1=0.2, and d2=0.8.

2. The method of claim 1 , wherein the silicon comprises metallurgical grade silicon.

3. The method of claim 1 , wherein removing AlCl 3 , from the gas or gas stream is accomplished by absorption on solid sodium chloride.

4. The method of claim 1 , further comprising removing particulate solids as well as AlCl 3 from the gas or gas stream.

5. The method of claim 1 , wherein the gas or gas stream is analyzed by Raman spectroscopy, gas chromatography or IR spectroscopy.

6. The method of claim 1 , wherein the analysis of the gas or gas stream determines at least one of the concentrations of HCl, N 2 , H 2 , or one or more chlorosilanes in the gas or gas stream.

7. The method of claim 1 , wherein the data obtained from analysis of the gas controls the fluidized bed temperature profile of the chemical reactor.

8. The method of claim 7 , wherein the reactor is a fluidized bed reactor in which trichlorosilane is prepared by reaction of metallurgical grade silicon with HCl.

9. The method of claim 8 , wherein analysis of the gas is used to change one or more operating parameters so as to optimize one or more variables selected from the group consisting of chlorosilane yield, trichlorosilane selectivity, HCl conversion rate, and space-time yield.

10. The method of claim 1 , wherein the analysis of the gas or gas stream is used to modify temperatures in the reactor and temperature profile as a function of a reactor height.

11. The method of claim 1 , wherein analysis of the gas determines a time for discharge of catalyst material.

12. A method for preparing chlorosilanes in a fluidized bed reactor having a reactor height H0, in which HCl reacts with silicon, comprising establishing a temperature profile in the fluidized bed reactor which is above S1(H/H0)=(a1−b1)*(1/(1+exp(−c1((H/H0)−d1))))+b1 and below S2(H/H0)=(a2−b2)*(1/(1+exp(−c2((H/H0)−d2))))+b2, where a1=100° C., a2=300° C., b1=300° C., b2=400° C., c1=50, c2=20, d1=0.2, and d2=0.8.

13. The method of claim 12 , further comprising removing AlCl 3 from a product gas stream and analyzing the product gas stream by on-line gas chromatography or spectroscopy to obtain data on the composition of the product gas stream, and adjusting the temperature profile of the reactor from the data to optimize production of a desired chlorosilane product.

14. The method of claim 13 , wherein AlCl 3 is removed from the gas stream by contacting solid sodium chloride forming a liquid adduct of sodium chloride and aluminum chloride, and collecting the liquid adduct in a collecting vessel below a container in which the solid sodium chloride is contained.

Assignees

• Wacker Chemie Ag

Inventors

• Goebel Thorsten
• Haeckl Walter
• Muenzer Wolfgang
• Paetzold Uwe
• Sofina Natalia

Classifications

• G01N21/3504

  for analysing gases, e.g. multi-gas analysis · CPC title

• B01D2257/204

  Inorganic halogen compounds · CPC title

• G01N2201/08

  Optical fibres; light guides · CPC title

• G01N2201/06113

  Coherent sources; lasers · CPC title

• B01D53/685

  by treating the gases with solids · CPC title