# US 5,710,227 A · High temperature polymerization process for making terminally unsaturated oligomers

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- Number: US 5,710,227 A
- Document ID: US5710227A
- Status: Granted
- Kind: A
- Application number: 08/587,707
- Filed: 1996-01-19
- Granted: 1998-01-20
- Earliest claimed: 1994-06-13
- Assignees: Rohm and Haas Company
- Inventors: Michael Bennett Freeman; Gary Robert Larson; Richard Foster Merritt; Yi Hyon Paik; Jan Edward Shulman; Graham Swift; Robert Wilczynski
- Web page: https://patentgrep.com/patent/US5710227A

## CPC

- C11D 3/3788: {Graft polymers}
- C08F 2/18: Suspension polymerisation
- C08F 20/04: Acids, Metal salts or ammonium salts thereof
- C08F 220/06: Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
- C08F 290/046: {Polymers of unsaturated carboxylic acids or derivatives thereof}
- C11D 3/3757: {(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions}
- C11D: DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS

## Abstract

High temperature polymerization process and products obtained therefrom are provided. The polymerization is conducted at above 225.degree. C. to produce polymers having a degree of polymerization below 50. The products are useful as detergent additives and for subsequent polymerization.

## Claims

### Claim 1

A continuous process for preparing terminally unsaturated oligomers comprising:
(a) forming a reaction mixture comprising
(i) from 0.5 to 99.95 percent by weight of the reaction mixture of at least one monomer selected from the group consisting of acrylic acid and salts thereof, and acrylic acid and salts thereof in combination with at least one monoethylenically unsaturated monomer;
(ii) from 0.05 to 25 percent by weight based on the weight of the at least one monomer of at least one free-tactical initiator; and
(iii) no solvent or in the presence of up to 99.5 percent by weight of the reaction mixture of at least one solvent selected from the group consisting of water, acetone, methanol, isopropanol, propionic acid, acetic acid, methylethyl ketone, dimethylformamide, dimethylsulfoxide and combinations thereof, and
(b) continuously passing the reaction mixture through a heated zone wherein the reaction mixture is maintained at a temperature of at least 275.degree. C. for from 0. 1 seconds to 2 minutes to form terminally unsaturated oligomers.

### Claim 2 (depends on 1)

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

### Claim 3 (depends on 1)

The process of claim 1, wherein the reaction mixture is heated to a temperature in the range of from 175.degree. C. to 500.degree. C.

### Claim 4 (depends on 1)

The process of claim 1, wherein the reaction mixture is heated to a temperature in the range of from 275.degree. C. to 450.degree. C.

### Claim 5

A continuous process for preparing terminally unsaturated oligomers comprising:
(a) continuously forming, at a temperature of at least 275.degree. C., a reaction mixture comprising
(i) from 0.5 to 99.95 percent by weight of the reaction mixture of at least one monomer selected from the group consisting of acrylic acid and salts thereof, and acrylic acid and salts thereof in combination with at least one monoethylenically unsaturated monomer;
(ii) from 0.05 to 25 percent by weight based on the weight of the at least one monomer of at least one frec-radical initiator; and
(iii) no solvent or in the presence of up to 99.5 percent by weight of the reaction mixture of at least one solvent selected from the group consisting of water, acetone, methanol, isopropanol, propionic acid, acetic acid, methylethyl ketone, dimethylformamide, dimethylsulfoxide and combinations thereof; and
(b) maintaining the reaction mixture at a temperature of at least 275.degree. C. for from 0-1 seconds to 300 seconds to form terminally unsaturated oligomers.