Detection of polymer concentration in polymerization process using refractive index measurement

Patent metadata

Field	Value
Publication number	US-11384174-B2
Application number	US-202016847744-A
Country	US
Kind code	B2
Filing date	Apr 14, 2020
Priority date	May 15, 2019
Publication date	Jul 12, 2022
Grant date	Jul 12, 2022

Abstract

A method for determining polymer concentration can include synthesizing a polymer in a reactor under a set of parameters, wherein the reactor comprises a solution mixture having a refractive index, and wherein the solution mixture comprises a solvent, a polymer, and optionally a monomer, wherein the solution mixture has a polymer concentration; measuring the refractive index of the solution mixture; comparing the refractive index of the solution mixture with a calibration curve; and identifying the polymer concentration in the solution mixture. A system for determining polymer concentration can include a reactor containing a solution mixture comprising a solvent, a polymer, and optionally a monomer; a flash vessel fluidly coupled to the reactor to receive the solution mixture from the reactor; and a first refractometer fluidly coupled to the reactor, placed between the reactor and the flash vessel, and configured to measure a refractive index of the solution mixture.

First claim

The invention claimed is:

1. A method, comprising:
synthesizing a polymer in a reactor under a set of parameters, wherein the reactor comprises a solution mixture having a refractive index, wherein the solution mixture comprises a solvent, a polymer, and optionally a monomer, and wherein the solution mixture has a polymer concentration;
measuring the refractive index of the solution mixture;
comparing the refractive index of the solution mixture with a calibration curve; and
identifying the polymer concentration in the solution mixture.

2. The method of claim 1 , further comprising modifying the set of parameters based on the polymer concentration of the solution mixture.

3. The method of claim 1 , wherein the reactor is a loop reactor.

4. The method of claim 1 , wherein the reactor is a stirred tank reactor.

5. The method of claim 1 , further comprising a devolatilization step.

6. The method of claim 5 , wherein the refractive index is measured before the devolatilization step.

7. The method of claim 1 , further comprising a finishing step.

8. The method of claim 7 , wherein the refractive index is measured before the finishing step.

9. The method of claim 1 , wherein the polymer comprises a polyolefin.

10. The method of claim 1 , wherein the monomer is selected from the group consisting of: ethylene, propylene, butene, pentene, hexene, heptene, octene, nonene, decene, dodecene, 4-methylpentene-1,3-methylpentene-1,3,5,5-trimethylhexene-1, 5-ethylnonene-1, styrene, alpha-methyl styrene, para-alkylstyrenes, vinyltoluenes, vinylnaphthalene, indene, paramethylstyrene, 4-phenyl-butene-1, allylbenzene, vinylcyclohexane, vinylcyclohexene, vinylnorbornene, ethylidene norbornene, cyclopentadiene, cyclopentene, cyclohexene, cyclobutene, butadiene, pentadiene, hexadiene, heptadiene, octadiene, nonadiene, decadiene, undecadiene, dodecadiene, tridecadiene, tetradecadiene, pentadecadiene, hexadecadiene, heptadecadiene, octadecadiene, nonadecadiene, icosadiene, heneicosadiene, docosadiene, tricosadiene, tetracosadiene, pentacosadiene, hexacosadiene, heptacosadiene, octacosadiene, nonacosadiene, and triacontadiene.

11. The method of claim 1 , wherein the polymer concentration is in a range from about 1 wt % to about 75 wt %.

12. A system comprising:
a reactor containing a solution mixture comprising a solvent, a polymer, and optionally a monomer;
a flash vessel fluidly coupled to the reactor to receive the solution mixture from the reactor; and
a first refractometer fluidly coupled to the reactor, placed between the reactor and the flash vessel, and configured to measure a refractive index of the solution mixture.

13. The system of claim 12 , wherein the reactor is a loop reactor.

14. The system of claim 12 , wherein the reactor is a stirred tank reactor.

15. The system of claim 12 , further comprising a devolatilization unit.

16. The system of claim 15 , further comprising a finishing unit.

17. The system of claim 16 , further comprising a second refractometer placed between the flash vessel and the devolatilization unit and/or between the flash vessel and the finishing unit.

18. The system of claim 12 , wherein the polymer comprises a polyolefin.

19. The system of claim 12 , wherein the monomer is selected from the group consisting of: ethylene, propylene, butene, pentene, hexene, heptene, octene, nonene, decene, dodecene, 4-methylpentene-1,3-methylpentene-1,3,5,5-trimethylhexene-1, 5-ethylnonene-1, styrene, alpha-methylstyrene, para-alkylstyrenes, vinyltoluenes, vinylnaphthalene, indene, paramethylstyrene, 4-phenyl-butene-1, allylbenzene, vinylcyclohexane, vinylcyclohexene, vinylnorbornene, ethylidene norbornene, cyclopentadiene, cyclopentene, cyclohexene, cyclobutene, butadiene, pentadiene, hexadiene, heptadiene, octadiene, nonadiene, decadiene, undecadiene, dodecadiene, tridecadiene, tetradecadiene, pentadecadiene, hexadecadiene, heptadecadiene, octadecadiene, nonadecadiene, icosadiene, heneicosadiene, docosadiene, tricosadiene, tetracosadiene, pentacosadiene, hexacosadiene, heptacosadiene, octacosadiene, nonacosadiene, and triacontadiene.

20. The system of claim 12 , wherein the polymer concentration is in a range from about 1 wt % to about 75 wt %.

Assignees

• Exxonmobil Chemical Patents Inc

Inventors

• Reimers Jay L
• Hong Yifeng

Classifications

• B01J19/2435

  Loop-type reactors · CPC title

• C08F2/06

  Organic solvent · CPC title

• B01J19/1837 Primary

  Loop-type reactors · CPC title

• B01J2219/00128

  by evaporation of reactants · CPC title

• B01J2219/00961

  Temperature · CPC title