Hydrophilic hydrogels with a high swelling capacity and method for producing and using them

• US 6,602,950 B1
• Filed: 04/06/2001
• Issued: 08/05/2003
• Est. Priority Date: 10/08/1998
• Status: Expired due to Fees

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Engelhardt, Friedrich, Herfert, Norbert, Funk, Rüdiger, Wanior, Mariola, Dentler, Joachim
• Primary Examiner(s): Lovering, Richard D.
• Application Number:
  US09/806,944
• Time in Patent Office: 851 Days
• Field of Search: 516/108, 516/105, 524/832, 524/835, 524/916, 264/177.17, 252/194, 604/368, 604/372, 604/904, 525/54.23, 525/54.26, 526/932
• US Class Current: 524/832
• CPC Class Codes: A61L 15/60 Liquid-swellable gel-forming materials, e.g. super-absorbents
• CPC Class Codes: C08F 251/00 Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
• CPC Class Codes: C08F 283/00 Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
• CPC Class Codes: C08F 283/02 on to polycarbonates or saturated polyesters C08F283/004 takes precedence
• CPC Class Codes: C08F 283/06 on to polyethers, polyoxymethylenes or polyacetals C08F283/004 takes precedence
• CPC Class Codes: C08F 8/00 Chemical modification by after-treatment graft polymers, block polymers, crosslinking with unsaturated monomers or with polymers C08F251/00 - C08F299/00; of conjugated diene rubbers C08C
• CPC Class Codes: Y10S 524/916 Hydrogel compositions
• CPC Class Codes: Y10S 526/932 Thickener or dispersant for aqueous system
• CPC Class Codes: Y10S 604/904 Tampons

Abstract

A hydrophilic, highly swellable hydrogel based on (co)polymerized monomers or based on graft (co)polymers and prepared by

a) free-radically (co)polymerizing one-or more hydrophilic monomers or graft (co)polymerizing one or more hydrophilic monomers onto a grafting base, the average degree of neutralization of the acid-functional monomers being from 0 to 40 mol %,

b) comminuting the acidic hydrogel,

c) neutralizing the acidic hydrogel to an ultimate degree of neutralization of 50-85 mol % by adding a neutralizing agent,

d) drying, grinding and sieving the hydrogel particles characterized by

a centrifuge retention and a vertical absorption swell height, each having a specified minimum.value, coupled with an extractables content having a specified maximum value or

a centrifuge retention and a vertical absorption swell height, each having a specified minimum value and

an extractables content having a specified maximum value.

Claims

1. A hydrophilic, highly swellable hydrogel based on (co)polymerized monomers or based on graft (co)polymers and prepared by

a) free-radically (co)polymerizing one or more hydrophilic monomers

 

where

R¹ is hydrogen, methyl or ethyl,

R² is —

COOR⁴, hydroxysulfonyl, phosphonyl, a (C₁-C₄)-alkanol-esterified phosphonyl group or a group of the general formula (II)

R³ is hydrogen, methyl, ethyl or carboxyl,

R⁴ is hydrogen, amino-(C₁-C₄)-alkyl or hydroxy-(C₁-C₄)-alkyl, and

R⁵ is hydroxysulfonyl, phosphonyl or carboxyl;

or

 

graft (co)polymerizing one or more hydrophilic monomers of the formula (I) onto a grafting base, the average degree of neutralization of the acid-functional monomers being from 0 to 40 mol %;

b) comminuting the acidic hydrogel;

c) neutralizing the acidic hydrogel to an ultimate degree of neutralization of 50-85 mol % by adding a neutralizing agent; and

d) drying, grinding and sieving the hydrogel particles characterized by

a centrifuge retention of at least 29 g/g for a 0.9% aqueous NaCl solution, and

a vertical absorption (1 g) swell height of at least 3.5 cm coupled with an extractables content (16 h value) of less than 5%;

or

a centrifuge retention of at least 23 g/g for a 0.9% aqueous NaCl solution, and

a vertical absorption (3 g) swell height of at least 5 cm

an extractables content (16 h value) of less than 4%.

2. The hydrophilic, highly swellable hydrogel of claim 1, wherein the polymerization is carried out quiescently.

3. The hydrogel of claim 1, wherein suitable grafting bases are selected from the group consisting of starch, starch derivatives, cellulose, cellulose derivatives, polyvinyl alcohol, polyalkylene oxide, polyethylene oxide, polypropylene oxide and hydrophilic polyesters.

4. The hydrogel of claim 1, wherein the (co)polymerizing of the hydrophilic monomers is effected in the presence of crosslinkers.

5. The hydrogel of claim 1, wherein the acidic hydrogel is neutralized to an ultimate degree of neutralization of 50-85 mol % by mixing with a neutralizing agent in a mincer comprising a system of screw, rotating blade, restricted flow zone and breaker plate, wherein

a) the mincer has a power output of from 1000 to 6000 Wh/m³.

b) the hydrogel is passed through a zone having an energy dissipation intensity of from 400 to 800 W/l of mixing volume,

c) the average hydrogel residence time in the mincer is from 5 to 30 seconds,

d) the open area of the breaker plate is from 20 to 40% and the postneutralized hydrogel particles are subjected to the drying step without further shearing.

6. The hydrogel of claim 1, wherein, as well as the neutralizing agent, one or more other reactive materials capable of reacting with free acrylic acid and/or with the carboxyl groups of the hydrogel and/or water-swellable hydrophilic polymer fines are added during the neutralization of the gel.

7. The hydrogel of claim 1, wherein the postneutralization is carried out in two steps, the first neutralization step taking place in the mincer and the second neutralization step being effected by applying the neutralizing agent to the hydrogel particles without mechanical shearing stress.

8. The hydrogel of claim 1, wherein the dried and ground hydrogel particles are covalently surface postcrosslinked.

9. The hydrogel of claim 1, wherein the surface of the dried and ground hydrogel particles is modified by the formation of metal complexes.

10. A method of absorbing water or aqueous fluid, comprising contacting the hydrogel according to claim 1 with water or aqueous fluid.

11. A method of absorbing bodily fluid, comprising contacting the hydrogel according to claim 1 with bodily fluid.

12. An absorbent, comprising the hydrogel according to claim 1.

13. A method of absorbing water or aqueous fluid, comprising contacting the absorbent according to claim 12 with water or aqueous fluid.

14. A method of absorbing bodily fluid, comprising contacting the absorbent according to claim 12 with bodily fluid.

15. A diaper, comprising the hydrogel according to claim 1.

16. A method of absorbing water or aqueous fluid, comprising contacting the diaper according to claim 15 with water or aqueous fluid.

17. A method of absorbing bodily fluid, comprising contacting the diaper according to claim 15 with bodily fluid.

18. A tampon, comprising the hydrogel according to claim 1.

19. A method of absorbing water or aqueous fluid, comprising contacting the tampon according to claim 18 with water or aqueous fluid.

20. A method of absorbing bodily fluid, comprising contacting the tampon according to claim 18 with bodily fluid.

21. A sanitary napkin, comprising the hydrogel according to claim 1.

22. A method of absorbing water or aqueous fluid, comprising contacting the sanitary napkin according to claim 21 with water or aqueous fluid.

23. A method of absorbing bodily fluid, comprising contacting the sanitary napkin according to claim 21 with bodily fluid.