IP Library Granted Patent US 9,975,980
Granted Patent B2
US 9,975,980 · App. 13/876,887 · Granted May 22, 2018

Preparation of hydrophilic polymers of high mass by controlled radical polymerization

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Quick Facts
Patent No.
US 9,975,980
App. No.
13/876,887
Granted
May 22, 2018
Kind
B2
Abstract

The present invention concerns a process for preparing a polymer comprising at least one gel polymerization step (E) in which the following are contacted: ethylenically unsaturated water-soluble monomers, the same or different; a source of free radicals adapted to the polymerization of the said monomers, typically a redox system; and a radical polymerization control agent, preferably comprising a thiocarbonylthio —S(C═S)— group; with a concentration of monomers in the reaction medium of step (E) sufficiently high to cause gelling of the medium if polymerization was conducted without the control agent.

Claims (15)

1. A process for preparing a polymer comprising at least one polymerization in a reaction medium wherein the polymerization comprises contacting:

ethylenically unsaturated water-soluble monomers, the same or different;

a source of free radicals adapted to the polymerization of said monomers; and

a radical polymerization control agent, wherein said control agent is a reversible transfer agent;

wherein the polymerization is performed without any cross-linking agent and the concentration of monomers in the reaction medium of the polymerization is sufficiently high to cause gelling of the medium and lead to a non-covalent gel if polymerization was conducted without the control agent,

wherein in the polymerization, the initial concentration of control agent in the medium is chosen so that the number-average molecular weight M n of the synthesized polymer is higher than 100,000 g/mol;

wherein the control agent is a compound carrying an —S(C═S)O— xanthate function; and

wherein number-average molecular weight M n of the synthesized polymer is of 500 000 g/mol or higher.

2. The process according to claim 1 wherein the monomers, the source of free radicals and the control agent are contacted in an aqueous medium.

3. The process according to claim 1 wherein the monomers comprise acrylamido monomers.

4. The process according to claim 1 wherein the initial concentration of monomers in the reaction medium is between 10 and 40% by weight relative to the total weight of the reaction medium.

5. The process according to claim 1 wherein the source of free radicals used is a redox initiator.

6. The process according to claim 5 wherein the source of free radicals is a redox system which is an association of ammonium persulfate and sodium formaldehyde sulfoxylate.

7. The process according to claim 1 wherein the reaction medium is free of copper.

8. The process according to claim 1 , wherein the control agent is a compound carrying an O-ethyl xanthate function of formula —S(C═S)OCH 2 CH 3 .

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 26, 2024
From: RHODIA OPERATIONS
To: SPECIALTY OPERATIONS FRANCE
Reel/Frame 066374/0642 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 7, 2023
From: RHODIA OPERATIONS
To: SPECIALTY OPERATIONS FRANCE
Reel/Frame 065488/0365 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2013
From: DESTARAC, MATHIAS; GUINAUDEAU, AYMERIC; MAZIERES, STEPHANE; WILSON, JAMES
To: RHODIA OPERATIONS; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (C.N.R.S.)
Reel/Frame 030682/0900 →