IP Library Granted Patent US 7,167,240
Granted Patent B2
US 7,167,240 · App. 10/622,318 · Granted Jan 23, 2007

Carbon black sampling for particle surface area measurement using laser-induced incandescence and reactor process control based thereon

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Quick Facts
Patent No.
US 7,167,240
App. No.
10/622,318
Granted
Jan 23, 2007
Kind
B2
Abstract

Disclosed is a method for in-situ sampling and measuring particulate fineness in a process stream, comprising (a) sampling particles in-situ from a process stream, (b) adjusting the sample to conditions suitable for LII, (c) measuring the fineness using LII, and (d) correlating the LII fineness measurement with actual particle fineness. Also disclosed is a method for sampling and controlling a process based on the real-time, on-line, in-situ methods for sampling and measuring particles. Sampling can comprise drawing a sidestream from a source of the particles. Adjusting the sample to conditions suitable for LII can comprise diluting the sample or bringing the temperature of the sample to ambient conditions. Correlating may comprise using a correlation function determined by comparing LII measurements and laboratory fineness measurements for particle samples drawn at the same time.

Claims (50)

1. An in-situ method for sampling a particle-containing stream and measuring particle fineness using laser-induced incandescence (LII) comprising

a) sampling particles in-situ by drawing a sidestream from a source of the particles using an in-situ eductor with a sample inlet and an in-situ critical orifice on the sample inlet wherein the sample enters a sampling system through the critical orifice,

b) adjusting the sample to conditions suitable for LII,

c) measuring the adjusted sample using LII, and

d) correlating the LII measurements with actual particle fineness.

2. The method of claim 1 wherein the adjusting comprises adding secondary dilution air to the sample.

3. The method of claim 1 wherein adjusting the sample to conditions suitable for LII comprises diluting the sample.

4. The method of claim 3 wherein diluting the sample is to a level of about less than or equal to 90, 80, 75, 70, 60, 50, 40, 30, 25, 20, 15, 10, 5, 3, 2, 1, 0.7, 0.5, 0.4, 0.3, 0.2, or 0.1 ppm.

5. The method of claim 3 wherein diluting the sample is to a level of about less than or equal to 1 ppm.

6. The method of claim 1 wherein adjusting the sample to conditions suitable for LII comprises bringing the temperature of the sample to ambient conditions.

7. The method of claim 1 further comprising determining a correlation function by comparing LII measurements and laboratory fineness measurements for particle samples drawn at the same time.

8. The method of claim 7 wherein the LII measurement is the decay rate of the LII intensity signal.

9. The method of claim 7 wherein the LII measurement is the decay rate of the temperature of the particles.

10. The method of claim 7 wherein the LII measurement is normalized specific surface area.

11. The method of claim 1 wherein the sampling and measurement of particle fineness is done in real-time.

12. The method of claim 1 wherein the sampling and measurement of particle fineness is done on-line.

13. The method of claim 1 wherein the particles are carbon black.

14. The method of claim 1 wherein the particle-containing stream is in a carbon black reactor or reactor breeching section.

15. The method of claim 1 , wherein the in-situ sampling of a) is performed at a temperature above ambient conditions.

16. An in-situ method for sampling and measuring carbon black fineness in a process stream comprising

a) sampling carbon black particles in-situ from a process stream by drawing a sidestream from the process stream using an in-situ eductor with a sample inlet and an in-situ critical orifice on the sample inlet wherein the sample enters a sampling system through the critical orifice,

b) adjusting the sample to conditions suitable for LII,

c) measuring the carbon black fineness using LII, and

d) correlating the LII fineness measurement with actual carbon black particle size.

17. The method of claim 16 wherein the process stream is in a carbon black reactor.

18. An in-situ method for sampling a particle-containing stream for LII-based particle fineness measurement comprising

a) sampling in-situ a particle-containing stream by drawing a sidestream from the particle-containing stream using an in-situ eductor with a sample inlet and an in-situ critical orifice on the sample inlet wherein the sample enters a sampling system through the critical orifice, and

b) adjusting the sample to conditions suitable for LII, wherein the sampling is done with a sidestream.

19. The method of claim 18 wherein the stream is in a carbon black reactor.

20. The method of claim 18 wherein adjusting the sample to conditions suitable for LII comprises diluting the sample.

21. A method for sampling a carbon black stream for LII-based measurement of particle surface area comprising

a) drawing a sample of carbon black from the stream by drawing a sidestream using an in-situ eductor with a sample inlet and an in-situ critical orifice on the sample inlet wherein the sample enters a sampling system through the critical orifice,

b) adjusting the sample to conditions suitable for LII, and

c) providing the adjusted sample to an LII system for particle surface area measurement.

22. A method for controlling particle fineness during production of flame generated particulates comprising

a) sampling the flame generated particulate in-situ in the production process,

b) adjusting the flame generated particulate sample to conditions suitable for LII,

c) measuring particle fineness of the adjusted particulate sample using LII,

d) sending a signal related to Lu-measured particle fineness to a controller,

e) comparing the particle fineness signal to a set point, and

f) sending a signal from the controller to adjust operation of the flame generated particulate production process.

23. The method of claim 22 further comprising correlating the LII-measured particle fineness to actual particle fineness.

24. The method of claim 22 wherein the flame generated particulate is carbon black.

25. The method of claim 24 wherein the adjustment of operation of the carbon black production process is via control of the air/feedstock ratio.

26. The method of claim 22 wherein the flame generated particulate is titania or silica.

27. An in-situ method for sampling a particle-containing stream and measuring particle fineness and aggregate size using laser-induced incandescence (LII) comprising

a) sampling particles in-situ,

b) adjusting the sample to conditions suitable for LII,

c) measuring incandescence signals and scattering data for the adjusted sample using LII, and

d) correlating the LII incandescence signals and scattering data measurements with actual particle fineness and aggregate size.

Assignments (12)
CHANGE OF NAME Recorded Jul 19, 2019
From: COLUMBIAN CHEMICALS COMPANY
To: BIRLA CARBON U.S.A., INC.
Reel/Frame 049805/0885 →
RELEASE OF SECURITY INTEREST Recorded May 3, 2018
From: BANK OF AMERICA, N.A.
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 045699/0531 →
CORRECTIVE ASSIGNMENT TO CORRECT THE CONVEYING PARTY NAME PREVIOUSLY RECORDED ON REEL 037436 FRAME 0083. ASSIGNOR(S) HEREBY CONFIRMS THE SECURITY INTEREST. Recorded Jan 21, 2016
From: COLUMBIAN CHEMICALS COMPANY
To: BANK OF AMERICA, N.A., AS SECURITY AGENT
Reel/Frame 037567/0710 →
SECURITY INTEREST Recorded Jan 8, 2016
From: COLUMBIA CHEMICALS COMPANY
To: BANK OF AMERICA, N.A., AS SECURITY AGENT
Reel/Frame 037436/0083 →
RELEASE (REEL 026480 / FRAME 0804) Recorded Dec 21, 2015
From: BANK OF AMERICA, N.A.
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 037354/0847 →
PATENT SECURITY AGREEMENT Recorded Jun 23, 2011
From: COLUMBIAN CHEMICALS COMPANY, A DELAWARE CORPORATION
To: BANK OF AMERICA, N.A., AS SECURITY AGENT
Reel/Frame 026480/0804 →
RELEASE OF PATENT SECURITY AGREEMENT Recorded Jun 22, 2011
From: UBS, AG, STAMFORD BRANCH, AS SECURITY AGENT
To: COLUMBIAN CHEMICALS COMPANY, A DELAWARE CORPORATION
Reel/Frame 026479/0126 →
SECURITY AGREEMENT Recorded Nov 22, 2010
From: COLUMBIAN CHEMICALS COMPANY
To: UBS AG, STAMFORD BRANCH
Reel/Frame 025412/0104 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENT RIGHTS Recorded Nov 19, 2010
From: HSBC BANK, USA, NATIONAL ASSOCIATION
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 025408/0645 →
RELEASE OF SECURITY INTEREST Recorded May 25, 2007
From: JPMORGAN CHASE BANK SEOUL BRANCH
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 019341/0120 →
SECURITY AGREEMENT Recorded Mar 22, 2006
From: COLUMBIAN CHEMICALS COMPANY
To: JPMORGAN CHASE BANK SEOUL BRANCH
Reel/Frame 017344/0361 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 10, 2003
From: STAGG, BARRY JAMES
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 014685/0156 →