Polymerisation process

• US 20040077744A1
• Filed: 08/15/2003
• Published: 04/22/2004
• Est. Priority Date: 02/20/2001
• Status: Abandoned Application

• Current Assignee: CIBA Specialty Chemicals Water Treatments Limited (BASF SE)
• Original Assignee: CIBA Specialty Chemicals Water Treatments Limited (BASF SE)
• Inventors: Green, David, Raistrick, Lee, James, Philippa Jane, Whitley, Martin William, Naylor, Gareth Ian
• Application Number:
  US10/468,191
• Publication Number:
  US 20040077744A1
• Time in Patent Office: Days
• US Class Current: 522/150
• CPC Class Codes: C08F 2/10 Aqueous solvent
• CPC Class Codes: C08F 2/48 by ultraviolet or visible light
• CPC Class Codes: C08F 220/34 Esters containing nitrogen , e.g. N,N-dimethylaminoethyl (meth)acrylate
• CPC Class Codes: C08F 220/56 Acrylamide; Methacrylamide
• CPC Class Codes: C08F 6/006 Removal of residual monomers by chemical reaction, e.g. scavenging

Abstract

A process of preparing water soluble or water swellable polymer comprising the steps: a) forming an aqueous mixture comprising, i) a water soluble ethylenically unsaturated monomer or blend of monomers and, ii) at least one first ultra-violet initiator, iii) at least one second ultra-violet initiator; b) effecting polymerisation by subjecting the aqueous mixture formed in step (a) to irradiation by ultraviolet light at an intensity of up to 1,000 μWcm⁻²; subjecting the product of step (b) to irradiation by ultraviolet light of greater than 1,000 μWcm⁻², characterised in that a significant amount of the first initiator(s) is/are activated in step (b) and a significant amount of the second initiator(s) is/are activated in step (c). The process is particularly suitable for making highly effective water soluble and water swellable polymers useful as flocculants, coagulants, rheology modifiers, dispersants, superabsorbents and binders etc.

Claims

1. A process of preparing water soluble or water swellable polymer comprising the steps,

(a) forming an aqueous mixture comprising,

(i) a water soluble ethylenically unsaturated monomer or blend of monomers and,

(ii) at least one first ultra-violet initiator,

(iii) at least one second ultra-violet initiator,

(b) effecting polymerisation by subjecting the aqueous mixture formed in step (a) to irradiation by ultraviolet light at an intensity of up to 1,000 μ

Wcm<sup>−

2</sup>,

(c) subjecting the product of step (b) to irradiation by ultraviolet light of greater than 1,000 μ

Wcm<sup>−

2</sup>,

characterised in that a significant amount of the first initiator(s) is/are activated in step (b) and a significant amount of the second initiator(s) is/are activated in step (c).

2. A process according to claim 1 in which the first initiator(s) is/are activated in step (b) and the second initiator(s) is/are predominantly activated in step (c).

3. A process according to claim 1 or claim 2 in which the ultraviolet light intensity in step (b) is between 100 μ

Wcm<sup>−

2</sup> and 500 μ

Wcm<sup>−

2</sup>.

4. A process according to any of claims 1 to 3 in which the ultraviolet light in step (b) is a constant or intermittent dose and wherein the ultraviolet radiation is substantially the same time average intensity.

5. A process according to any of claims 1 to 3 in which the ultraviolet light in step (b) is increased from a lower intensity to a higher intensity up to 1 000 μ

Wcm<sup>−

2</sup>.

6. A process according to any one of claims 1 to 5 in which the ultra violet light intensity in step (c) is between 1 mWcm⁻

2 and 1,000 mWcm<sup>−

2</sup>, and the duration of step (c) is no more than 10 minutes.

7. A process according to any one of claims 1 to 6 in which the ultraviolet light in step (c) is a constant or intermittent dose and wherein the ultraviolet radiation is substantially the same time average intensity.

8. A process according to any of claims 1 to 6 in which the ultraviolet light in step (c) is increased from a lower intensity which is greater than 1000 μ

Wcm<sup>−

2</sup> to a higher intensity.

9. A process according to any one of claims 1 to 8 in which substantially all of the first ultraviolet initiator(s) is/are activated in step (b).

10. A process according to any of claims 1 to 9 in which the ultra violet initiator is a compound of formula:

11. A process according to any one of claims 1 to 10 in which at least 50% by weight of the second ultraviolet initiator remains unactivated in step (b).

12. A process according to any one of claims 1 to 11 in which the ultra violet initiator is a compound of formula:

13. A process according to any one of claims 1 to 12 in which the aqueous mixture formed in step (a) comprises acrylamide.

14. A process according to any of claims 1 to 13 in which the polymer is a water soluble polymer which has an intrinsic viscosity of at least 4 dl/g.

15. A process according to any of claims 1 to 14 in which the aqueous mixture formed in step (a) is subjected to step (b) and then step (c) while said aqueous mixture is on a moving surface.

16. A process according to any one of claim 15 in which polymer is produced continuously and said moving surface is a moving belt, which carries the aqueous mixture to step (b) where one or more ultraviolet lamps irradiates the mixture to form a polymer product and then carries the product of step (b) to step (c) where one or more ultraviolet lamps irradiates the mixture.

17. A process according to any one of claims 1 to 16 in which the ultra-violet radiation in step (b) has a substantially uniform distribution of intensity.

18. A process according to any one of claims 1 to 17 in which the ultraviolet radiation in step (b) is substantially all in the range 100 to 200 μ

Wcm<sup>−

2</sup>.

19. A process according to any one of claims 1 to 18 in which the ultraviolet radiation in step (b) and/or step (c) is provided by a multiplicity of individual ultra violet light sources, wherein each individual light source produces a light distribution pattern ranging from high intensity light in the centre to low intensity light at the out edges of the pattern, and arranging the light sources such that the light distribution patterns overlap in such a way that provides a substantially uniform distribution of light.

20. A process according to any one of claims 1 to 19 in which the ultraviolet light of step (b) and/or step (c) is filtered to remove at least some extraneous infra red radiation.

21. A water soluble or water swellable polymer obtainable by a process defined by any one of claims 1 to 20 in which the amount of residual monomer is below 100 ppm.