Generation of sulfur trioxide and sulfuric acid

• US 8,679,435 B2
• Filed: 10/03/2011
• Issued: 03/25/2014
• Est. Priority Date: 05/11/2009
• Status: Active Grant

• Current Assignee: Thermo Fisher Scientific Incorporated
• Original Assignee: Thermo Fisher Scientific Incorporated
• Inventors: Kita, Dieter, Li, Yongquan, Socha, Jeffrey, Marcotte, Bryan A.
• Primary Examiner(s): Mayes, Melvin C
• Assistant Examiner(s): DAVIS, SHENG HAN
• Application Number:
  US13/251,754
• Publication Number:
  US 20120087856A1
• Time in Patent Office: 904 Days
• Field of Search: None
• US Class Current: 423/222
• CPC Class Codes: C01B 17/76 by contact processes
• CPC Class Codes: C01B 17/80 Apparatus
• CPC Class Codes: G01N 2001/2893 Preparing calibration standards
• CPC Class Codes: G01N 33/0006 Calibrating gas analysers
• CPC Class Codes: G01N 33/0042 for SO2, SO3
• CPC Class Codes: Y10T 436/10 Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing

Abstract

Configurations herein include a novel process and apparatus for generating and maintaining sulfur trioxide gas. The generation system and process operate to provide sulfur trioxide calibration gas for calibrating sulfur trioxide detection devices. The system and process provides a known, concentration of sulfur trioxide gas via a heated catalyst, which enables accurate calibration of measurement equipment. The system functions in part by controlling temperature, amount of moisture, residence time, catalyst selection, diluting generated sulfur trioxide and by locating the sulfur trioxide generator at a point of injection of a sulfur trioxide detection system.

Claims

1. A method comprising:

receiving a known concentration of sulfur dioxide gas;

receiving an oxidizing agent gas;

controlling the known concentration of sulfur dioxide gas and the oxidizing agent gas to be substantially free of water;

conveying the known concentration of sulfur dioxide gas and the oxidizing agent gas, which are substantially free of water, to a reaction chamber;

exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to a catalyst in the reaction chamber, the catalyst being heated, to react the known concentration of sulfur dioxide gas and the oxidizing agent gas into a known concentration of sulfur trioxide gas; and

maintaining the known concentration of sulfur trioxide gas in a gaseous state.

2. The method of claim 1, wherein maintaining the known concentration of sulfur trioxide gas in the gaseous state includes:

diluting the sulfur trioxide gas with a dilution gas, the dilution gas being substantially free of water; and

maintaining the diluted sulfur trioxide gas above a conversion point temperature of sulfuric acid.

3. The method of claim 2, further comprising:

passing a portion of the diluted sulfur trioxide gas, having a known concentration of sulfur trioxide gas, through a sulfur trioxide detection device.

4. The method of claim 3, wherein passing the portion of the diluted sulfur trioxide gas, having a known concentration of sulfur trioxide gas, through the sulfur trioxide detection device includes:

passing the diluted sulfur trioxide gas through a multi-pass optical cell that measures a concentration of sulfur trioxide.

5. The method of claim 3, further comprising:

calibrating the sulfur trioxide detection device by measuring the known concentration of sulfur trioxide gas passing through the sulfur trioxide detection device; and

adjusting measurements of the sulfur trioxide detection device based on calibration using the known concentration of sulfur trioxide gas.

6. The method as in claim 5 further comprising:

exposing the known concentration of sulfur trioxide gas to water to convert the sulfur trioxide gas into sulfuric acid; and

utilizing the sulfuric acid for calibration.

7. The method of claim 1, wherein receiving the known concentration of sulfur dioxide gas includes pre-heating the sulfur dioxide gas before exposing the sulfur dioxide gas to the catalyst.

8. The method of claim 1, further comprising:

heating the catalyst to above about 550 degrees Celsius to restore a degraded condition of the catalyst, the degraded condition causing reduced efficiency of converting the sulfur dioxide into the sulfur trioxide.

9. The method of claim 1, wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to a catalyst includes heating the catalyst to a temperature between 225 degrees Celsius and 600 degrees Celsius.

10. The method of claim 1, wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to a catalyst includes:

exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to a catalyst at different flow rates at different time periods; and

adjusting the temperature of the catalyst according to the different flow rates at the different time periods to yield a conversion of the sulfur dioxide gas to the sulfur trioxide gas at an efficiency level above about 99%.

11. The method of claim 1, further comprising:

converting the sulfur trioxide gas to sulfuric acid by adding dihydrogen monoxide; and

heating the sulfuric acid to a temperature sufficient to convert the sulfuric acid to sulfur trioxide gas.

12. The method of claim 1, wherein a generator that performs the method of converting the sulfur dioxide gas to sulfur trioxide gas is disposed less than about 6 feet from a sulfur trioxide detection device.

13. The method as in claim 1 further comprising:

preventing exposure of the sulfur trioxide gas produced in the reaction chamber to water.

14. The method of claim 13, further comprising:

adjusting dilution of the sulfur trioxide with the dilution gas to produce different concentrations of sulfur trioxide gas; and

performing a multi-point calibration of a sulfur trioxide detection device by measuring the different concentrations of sulfur trioxide gas passing through the sulfur trioxide detection device.

15. The method of claim 14, wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to a catalyst includes heating the catalyst to a temperature between 225 degrees Celsius and 600 degrees Celsius.

16. The method of claim 15, wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to the catalyst includes:

exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to the catalyst at different flow rates at different time periods; and

adjusting the temperature of the catalyst according to the different flow rates at the different time periods to yield a conversion of sulfur dioxide gas to sulfur trioxide gas at an efficiency level above about 99%.

17. The method of claim 16, further comprising:

heating the catalyst to above about 550 degrees Celsius to restore a degraded condition of the catalyst, the degraded condition causing reduced efficiency of converting the sulfur dioxide into the sulfur trioxide.

18. The method of claim 13 further comprising:

to maintain a desired conversion efficiency of converting the sulfur dioxide gas into the sulfur trioxide gas, adjusting a temperature of heating the catalyst depending on a flow rate of inputting the known concentration of sulfur dioxide through the catalyst.

19. The method of claim 13 further comprising:

controlling flow rates of the sulfur dioxide gas and oxidizing agent gas and controlling the temperature of the catalyst to control a conversion efficiency of converting the known concentration of sulfur dioxide gas into the known concentration of the sulfur trioxide gas, the conversion efficiency controlled to an accuracy of less than a percentage point, the reaction chamber converting above about 99% of the sulfur dioxide gas into sulfur trioxide gas.

20. The method of claim 19 further comprising:

heating the catalyst to above about 550 degrees Celsius to restore a degraded condition of the catalyst, the degraded condition causing reduced efficiency of converting the sulfur dioxide into the sulfur trioxide;

wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to the catalyst includes heating the catalyst to a temperature between 225 degrees Celsius and 600 degrees Celsius;

wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to the catalyst includes;

exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to the catalyst at different flow rates at different time periods; and

adjusting the temperature of the catalyst according to the different flow rates at the different time periods to yield a conversion of sulfur dioxide gas to sulfur trioxide gas at an efficiency level above about 99%.

21. The method of claim 1, further comprising:

wherein maintaining the known concentration of sulfur trioxide gas in the gaseous state includes maintaining the sulfur trioxide gas above a conversion point temperature of sulfuric acid;

passing a portion of the sulfur trioxide gas through a sulfur trioxide detection device, the sulfur trioxide detection device being a device that measures a concentration of sulfur trioxide;

wherein receiving the known concentration of sulfur dioxide gas includes pre-heating the sulfur dioxide gas before exposing the sulfur dioxide gas to the catalyst;

wherein exposing the known concentration of sulfur dioxide gas and the oxidizing agent gas to the catalyst includes heating the catalyst to a temperature between 225 degrees Celsius and 600 degrees Celsius; and

heating the catalyst to above about 550 degrees Celsius to restore a degraded condition of the catalyst, the degraded condition causing reduced efficiency of converting the sulfur dioxide into the sulfur trioxide.

22. The method of claim 1, wherein maintaining the known concentration of sulfur trioxide gas in the gaseous state includes:

outputting sulfur trioxide gas from the reaction chamber;

diluting the outputted sulfur trioxide gas with a dilution gas, the dilution gas being substantially free of water;

hydrating the diluted sulfur trioxide gas; and

heating a conduit through which the hydrated diluted sulfur trioxide gas is conveyed to an analyzer, the conduit heated to a sufficiently high temperature to prevent conversion of the hydrated diluted sulfur trioxide gas into sulfuric acid.

23. The method as in claim 22 further comprising:

preventing exposure of the sulfur trioxide gas produced in the reaction chamber to water.