Decolorization of hydroxy-containing methacrylate homopolymers and copolymers

• US 5,750,772 A
• Filed: 01/30/1997
• Issued: 05/12/1998
• Est. Priority Date: 01/30/1997
• Status: Expired due to Fees

• Current Assignee: E. I. du Pont de Nemours and Company (Corteva, Inc.)
• Original Assignee: E. I. du Pont de Nemours and Company (Corteva, Inc.)
• Inventors: Gridnev, Alexei Alexeyevich
• Primary Examiner(s): Killos, Paul J.
• Application Number:
  US08/791,373
• Time in Patent Office: 467 Days
• Field of Search: 560/218
• US Class Current: 560/218
• CPC Class Codes: C08F 6/003 from polymer solutions, suspensions, dispersions or emulsions without recovery of the polymer therefrom
• CPC Class Codes: C08F 6/02 Neutralisation of the polymerisation mass, e.g. killing the catalyst short-stopping C08F2/42 also removal of catalyst residues
• CPC Class Codes: C08L 33/04 Homopolymers or copolymers of esters C08L43/04 takes precedence

Abstract

This invention relates to a process whereby hydroxy-containing methacrylate homo- and copolymers are decolorized by the addition of a strong acid and a chelating bidentate nitrogen ligand, with subsequent filtering through a polar adsorption medium.

Claims

1. A process for decolorizing homo- and co-polymers of hydroxy-containing methacrylates of the formula ##STR2## wherein n>

2,m>

4 and b>

1;

wherein said homo- and co-polymers are prepared in the presence of a chain transfer catalyst;

comprising the steps of exposing the polymers to;

(a) an acid having a pKa less than about 2;

(b) a chelating bidentate nitrogen ligand containing a fragment of the formula alkylidene(NR₂)_x (imidazolyl)_y

wherein y>

1 and (y+x)>

2;

said alkylidene is C₂ to C₁₀ ;

each R is independently H or C₁ to C₁₀ alkyl;

and

(c) a polar absorbent medium.

2. The process as recited in claim 1, wherein said acid is a strong mineral acid.

3. The process of claim 2 wherein said acid is selected from the group consisting of hydrochloric acid, hydrobromic acid, hydroiodic acid, nitric acid, sulfuric acid and perchloric acid.

4. The process as recited in claim 1, wherein said ligand is 1-(3-aminopropyl)-imidazole.

5. The process as recited in claim 1, wherein said absorbent medium is silica gel.

6. The process as recited in claim 2, wherein said catalyst is Bis- (1,2-diR*-ethanedioximato)(2-)O:

O'"'"'-tetrafluorodiborato(2-)-N'"'"'N"N'"'"'"N""!(A)(B) cobalt(III), where R* is alkyl, aryl or substituted aryl, A is an acido ligand, and B is a Lewis base.

7. The process as recited in claim 4, wherein said catalyst is Bis- (1,2-diR*-ethanedioximato)(2-)O:

O'"'"'-tetrafluorodiborato(2-)-N'"'"'N"N'"'"'"N""!(A)(B) cobalt(III), where R* is alky, aryl or substituted aryl, A is an acido ligand, and B is a Lewis base.

8. The process as recited in claim 5, wherein said catalyst is Bis- (1,2-diR*-ethanedioximato)(2-)O:

O'"'"'-tetrafluorodibrato(2-)-N'"'"'N"N'"'"'"N""!(A)(B) cobalt(III), where R* is alkyl, aryl or substituted aryl, A is an acido ligand, and B is a Lewis base.

9. The process as recited in claim 6, 7, or 8, wherein R* is methyl, A is isopropyl and B is water.

10. The process as recited in claim 2, wherein said acid is added first to the reaction mixture followed by the addition of 1-(3-aminopropyl)-imidazole and then the mixture is filtered through a bed of silica gel.

11. The process as recited in claim 1, wherein said alkylidene is C₂ to C₄.

12. The process as recited in claim 2, wherein said catalyst is described as indicated Bis- (1,2-diR*-ethanedioximato)(2-)O:

O'"'"'-tetrafluorodiborato(2-)-N'"'"'N"N'"'"'"N""!cobalt(II), where R* is alkyl, aryl or substituted aryl.

13. The process as recited in claim 4, wherein said catalyst is Bis- (1,2-diR*-ethanedioximato)(2-)O:

O'"'"'-tetrafluorodiborato(2-)-N'"'"'N"N'"'"'"N""!cobalt(II), where R* is alkyl, aryl or substituted aryl.

14. The process as recited in claim 5, wherein said catalyst is Bis- (1,2-diR*-ethanedioximato)(2-)O:

O'"'"'-tetrafluorodiborato(2-)-N'"'"'N"N'"'"'"N""!(A)(B) cobalt(III), where R* is alkyl, aryl or substituted aryl, A is an acido ligand, and B is a Lewis base.

15. The process as recited in claim 12, 13, or 14 wherein R* is phenyl.