Optics: measuring and testing – By dispersed light spectroscopy – With raman type light scattering
Reexamination Certificate
2006-09-12
2006-09-12
Evans, F. L. (Department: 2877)
Optics: measuring and testing
By dispersed light spectroscopy
With raman type light scattering
Reexamination Certificate
active
07106437
ABSTRACT:
Methods are provided for determining and controlling polymer product properties on-line in a slurry reactor system, such as a stirred slurry or slurry loop reactor. The methods include obtaining a regression model for determining a polymer product property, the regression model including principal component loadings and principal component scores, acquiring a Raman spectrum of polymer product in the slurry reactor system, calculating a new principal component score from at least a portion of the Raman spectrum and the principal component loadings, and calculating the polymer product property by applying the new principal component score to the regression model. The property can be controlled by adjusting at least one polymerization parameter based on the calculated polymer product property.
REFERENCES:
patent: 3725378 (1973-04-01), Chamberlin
patent: 3779712 (1973-12-01), Calvert et al.
patent: 4175169 (1979-11-01), Beals et al.
patent: 4182810 (1980-01-01), Willcox
patent: 4243619 (1981-01-01), Fraser et al.
patent: 4469853 (1984-09-01), Mori
patent: 4540753 (1985-09-01), Cozewith et al.
patent: 4543399 (1985-09-01), Jenkins, III et al.
patent: 4588790 (1986-05-01), Jenkins, III et al.
patent: 4620049 (1986-10-01), Schmidt et al.
patent: 4621952 (1986-11-01), Aronson
patent: 4888704 (1989-12-01), Topliss et al.
patent: 5096634 (1992-03-01), Tsadares et al.
patent: 5121337 (1992-06-01), Brown
patent: 5151474 (1992-09-01), Lange et al.
patent: 5202395 (1993-04-01), Chambon
patent: 5270274 (1993-12-01), Hashiguchi et al.
patent: 5274056 (1993-12-01), McDaniel et al.
patent: 5352749 (1994-10-01), DeChellis et al.
patent: 5405922 (1995-04-01), DeChellis et al.
patent: 5436304 (1995-07-01), Griffin et al.
patent: 5462999 (1995-10-01), Griffin et al.
patent: 5589555 (1996-12-01), Zboril et al.
patent: 5638172 (1997-06-01), Alsmeyer et al.
patent: 5675253 (1997-10-01), Smith et al.
patent: 5678751 (1997-10-01), Buchanan et al.
patent: 5682309 (1997-10-01), Bartusiak et al.
patent: 5696213 (1997-12-01), Schiffino et al.
patent: 5864403 (1999-01-01), Ajji et al.
patent: 5892228 (1999-04-01), Cooper et al.
patent: 5999255 (1999-12-01), Dupee et al.
patent: 6072576 (2000-06-01), McDonald et al.
patent: 6144897 (2000-11-01), Selliers
patent: 6204344 (2001-03-01), Kendrick et al.
patent: 6204664 (2001-03-01), Sardashti et al.
patent: 6218484 (2001-04-01), Brown et al.
patent: 6228793 (2001-05-01), Hosaka et al.
patent: 6239235 (2001-05-01), Hottovy et al.
patent: 6281300 (2001-08-01), Kendrick
patent: 6380325 (2002-04-01), Kendrick
patent: 6405579 (2002-06-01), Tjahjadi et al.
patent: 6479597 (2002-11-01), Long et al.
patent: 6673878 (2004-01-01), Donck
patent: 2002/0156205 (2002-10-01), Long et al.
patent: 2004/0198927 (2004-10-01), Battiste
patent: 2004/0233425 (2004-11-01), Long et al.
patent: 2004/0266959 (2004-12-01), Heslop et al.
patent: 2005/0154155 (2005-07-01), Battiste
patent: 238 796 (1987-09-01), None
patent: 257 316 (1988-03-01), None
patent: 257 316 (1988-03-01), None
patent: 328 826 (1989-08-01), None
patent: 561 078 (1993-09-01), None
patent: 406 805 (1995-12-01), None
patent: 0561078 (1997-04-01), None
patent: 02038841 (1990-08-01), None
patent: WO 94/21962 (1994-09-01), None
patent: WO 96/41822 (1996-12-01), None
patent: WO 98/08066 (1998-02-01), None
patent: WO 99/01750 (1999-01-01), None
patent: WO 01/09201 (2001-02-01), None
patent: WO 01/09203 (2001-02-01), None
patent: WO 2004/063234 (2004-07-01), None
patent: WO 2005/049663 (2005-06-01), None
K.R. Beebe et al., “An Introduction to Multivariate Calibration and Analysis,” Analytical Chemistry, vol. 59, No. 17, pp. 1007A-1017A, Sep. 1, 1987.
J. M. Tedesco et al., “Calibration of dispersive Raman Process Analyzers,” The Society Of Photo-Optical Instrumentation Engineers, vol. 3537, pp. 200-212, 1999.
G.A. Bakken et al., “Examination of Criteria for Local Model Principal Component Regression,” Society for Applied Spectroscopy, vol. 51, No. 12, pp. 1814-1822, 1997.
P. Erlich et al., “Fundamentals of the Free-Radical Polymerization of Ethylene,” Advanced Polymer Science, vol. 7, pp. 386-448, 1970.
M.L. Myrick et al., “In Situ Fiber-Optic Raman Spectroscopy of Organic Chemistry in a Supercritical Water Reactor,” Journal of Raman Spectroscopy, vol. 25, pp. 59-65, 1994.
T. Naes et al., “Locally Weighted Regression and Scatter Correction for Near-Infrared Reflectance Data,” Analytical Chemistry, vol. 62, pp. 664-673, 1990.
J.J. Zacca et al., “Modelling of the Liquid Phase Polymerization of Olefins in Loop reactors,” Chemical Engineering Science, vol. 48, No. 22, pp. 3743-3765, 1993.
L.P. Russo et al., “Moving-Horizon State Estimation Applied to an Industrial Polymereization Process,” American Control Conf. Proc., San Diego, CA, 1999.
H. Martens et al., “Multivariate Calibration,” Wiley & Sons Ltd., pp. vii-ix, 1989.
Multivariate Data Analysis for Windows—Version 3.0, excerpted from Pirouette Software Manual, Exploratory Analysis: Principal Component Analysis, pp. 5-13 through 5-40, 1985-2000.
E.P.C. Lai et al., “Noninvasive Spectroscopic Detection of Bulk Polymerization by Stimulated Raman Scattering,” Applied Spectroscopy, vol. 48, No. 8, 1994.
S. Sekulic et al., “Nonlinear Multivariate Calibration Methods in Analytical Chemistry,” Analytical Chemistry, vol. 65, No. 19, pp. 835A-845A, Oct. 1, 1993.
E.D. Lipp et al., “On-Line Monitoring Of Chlorosilane Streams By Raman Spectroscopy,” Reprinted from Applied Spectroscopy, vol. 52, No. 1, Jan., 1998.
D.R. Battiste et al., “On-Line Raman Analysis of Ethylene and Hexene in the Phillips I-Hexene and Polyethylene Processes,” Gulf Coast Conference presentation (Abstract).
M.J. Pelletier et al.; “Optical fibers enable Raman instruments to analyze industrial process problems quickly and accurately,” Raman Spectroscopy—Keeps Industry Under Control, Reprint: Photonics Spectra, 4 pgs., Oct., 1997.
V. Centner et al., “Optimization in Locally Weighted Regression,” Analytical Chemistry, vol. 70, No. 19, pp. 4206-4211, Oct. 1, 1998.
“Principal Components Analysis,” excerpted from PLS—Toolbox, Version 2.0 Data Analysis Manual, Eigenvector Research, Inc., pp. 32-34, 1998.
L. Markwort et al., “Raman Imaging of Heterogeneous Polymers: A Comparison of Global versus Point Illumination,” Applied Spectroscopy, vol. 49, No. 10, pp. 1411-1430, 1995.
I. Modric et al., “Raman- und Infrarotspektren isotaktischer Polyalkylathylene*,” Colloid & Polymer Sci., vol. 254, pp. 342-347, 1976.
M.G. Hansen et al., “Real-Time Monitoring of Industrial Polymers,” Raman Review; pp. 1-4, Mar. 1998.
S.E. Nave “Rugged Fiber Optic Probes and Sampling Systems for Remote Chemical analysis Via the Raman Technique,” ISA, Paper #96-042, pp. 453-467, 1996.
M.J. Pelletier et al., “Shining a Light on Wet Process Control,” Semiconductor International, 4 pages, Mar. 1996.
K.P.J. Williams et al., “Use of Micro Raman Spectroscopy for the Quantitative Determination of Polyethylene Density Using Partial Least-Squares Calibration,” Journal of Raman Spectroscopy, vol. 26, pp. 427-433, 1995.
Ardell, George G., et al., Model Prediction for Reaction Control,Chemical Engineering Progress, American Institute of Chemical Engineers, vol. 79, No. 6, pp. 77-83 (Jun. 1, 1983).
J.M. Tedesco et al., “Calibration of dispersive Raman process analyzers,” Part of the SPIE Conference on Online Chemical Process Monitoring w/Advanced Techniques, SPIE, vol. 3537, pp. 200-212, Nov. 1998.
A.C. Ouano et al., “Gel Permeation Chromatography,” Polymer Molecular Weights Part II, Chapter 6, pp. 287-378, 1975.
Verstrate et al., “Near Monodisperse Ethylene-Propylene Copolymers by Direct Ziegler-Natta Polymerization. Preparation, Characterization, Properties,” Macromolecules, vol. 21, pp. 3360-
Cochran Andrew M.
Marrow David Geoffrey
Roger Scott Thomas
Evans F. L.
ExxonMobil Chemical Patents Inc.
Griffis Andrew B.
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