# US 9,040,605 B2 · Polymerization process and raman analysis for olefin-based polymers

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- Number: US 9,040,605 B2
- Document ID: US9040605B2
- Status: Granted
- Kind: B2
- Application number: 13/991,832
- Filed: 2011-12-21
- Published: 2013-10-03
- Granted: 2015-05-26
- Earliest claimed: 2010-12-21
- Assignees: Dow Global Technologies LLC
- Applicants: Kishori Deshpande; Serena K. Stephenson; Ravindra S. Dixit
- Inventors: Kishori Deshpande; Serena K. Stephenson; Ravindra S. Dixit
- Web page: https://patentgrep.com/patent/US9040605B2

## CPC

- C08F 210/14: Monomers containing five or more carbon atoms
- C08F 10/02: Ethene
- G01N 21/65: Raman scattering
- C08F 210/16: Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
- C08F 2400/02: Control or adjustment of polymerization parameters
- G01N 2021/8416: {and process controlling, not otherwise provided for}
- G01N 2201/129: Using chemometrical methods
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

The invention provides a process for monitoring and/or adjusting a dispersion polymerization of an olefin-based polymer, the process comprising monitoring the concentration of the carbon-carbon unsaturations in the dispersion using Raman Spectroscopy. The invention also provides a process for polymerizing an olefin-based polymer, the process comprising polymerizing one or more monomer types, in the presence of at least one catalyst and at least one solvent, to form the polymer as a dispersed phase in the solvent; and monitoring the concentration of the carbon-carbon unsaturations in the dispersion using Raman Spectroscopy.

## Claims

### Claim 1

A process for monitoring and/or adjusting a dispersion polymerization of an olefin-based polymer, the process comprising monitoring the concentration of the carbon-carbon unsaturations in the dispersion using Raman Spectroscopy; and
wherein, in the dispersion polymerization, one or more monomer types are polymerized, in the presence of at least one catalyst and at least one solvent, to form a polymer, and wherein the polymer forms a dispersed phase in the solvent; and
wherein the at least one catalyst is soluble in the at least one solvent.

### Claim 2 (depends on 1)

The process of claim 1, wherein the temperature of the polymerization is from 60° C. to 200° C.

### Claim 3 (depends on 1)

The process of claim 1, wherein the pressure of the polymerization is from 1 to 10 MPa.

### Claim 4 (depends on 1)

The process of claim 1, wherein the at least one solvent is a hydrocarbon.

### Claim 5 (depends on 1)

The process of claim 1, wherein the process further comprises monitoring the vibrational spectra of the olefin-based polymer.

### Claim 6 (depends on 1)

The process of claim 1, wherein the dispersion is in contact with a Raman probe.

### Claim 7 (depends on 1)

The process of claim 1, wherein, during the Raman spectroscopy, a Raman spectrum is generated by a control computer.

### Claim 8 (depends on 7)

The process of claim 7, wherein the Raman spectrum is processed using a chemometric model to determine the concentration of the carbon-carbon unsaturations in the dispersion, and/or and the amount of incorporation of one or more monomer types in the olefin-based polymer.

### Claim 9 (depends on 8)

The process of claim 8, wherein the concentration of the carbon-carbon unsaturations and/or the amount of monomer(s) incorporation is fed back to a process control system.

### Claim 10 (depends on 9)

The process of claim 9, wherein the process control system, based on the carbon-carbon unsaturations and/or the amount of monomer(s) incorporation, monitors and/or adjusts monomer flow rate, catalyst flow rate, polymerization temperature, polymerization pressure, and/or polymer properties.

### Claim 11

A process for polymerizing an olefin-based polymer, the process comprising polymerizing one or more monomer types, in the presence of at least one catalyst and at least one solvent, to form the polymer as a dispersed phase in the solvent; and monitoring the concentration of the carbon-carbon unsaturations in the dispersion using Raman Spectroscopy; and
wherein the at least one catalyst is soluble in the at least one solvent.

### Claim 12 (depends on 11)

The process of claim 11, wherein the at least one solvent is a hydrocarbon.