ZA200504380B - Ultra-thin materials made from fibre and superabsorbent - Google Patents
Ultra-thin materials made from fibre and superabsorbent Download PDFInfo
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- ZA200504380B ZA200504380B ZA200504830A ZA200504830A ZA200504380B ZA 200504380 B ZA200504380 B ZA 200504380B ZA 200504830 A ZA200504830 A ZA 200504830A ZA 200504830 A ZA200504830 A ZA 200504830A ZA 200504380 B ZA200504380 B ZA 200504380B
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- sap
- ccm
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- 239000000463 material Substances 0.000 title claims abstract description 130
- 239000000835 fiber Substances 0.000 title claims abstract description 21
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 230000006835 compression Effects 0.000 claims description 16
- 238000007906 compression Methods 0.000 claims description 16
- 230000014759 maintenance of location Effects 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 7
- 210000001124 body fluid Anatomy 0.000 claims description 2
- 239000010839 body fluid Substances 0.000 claims description 2
- 239000002648 laminated material Substances 0.000 claims 5
- 229920000247 superabsorbent polymer Polymers 0.000 abstract description 37
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000012153 distilled water Substances 0.000 description 13
- 239000007858 starting material Substances 0.000 description 9
- 239000000654 additive Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000002745 absorbent Effects 0.000 description 4
- 239000002250 absorbent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008961 swelling Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- CYJRNFFLTBEQSQ-UHFFFAOYSA-N 8-(3-methyl-1-benzothiophen-5-yl)-N-(4-methylsulfonylpyridin-3-yl)quinoxalin-6-amine Chemical compound CS(=O)(=O)C1=C(C=NC=C1)NC=1C=C2N=CC=NC2=C(C=1)C=1C=CC2=C(C(=CS2)C)C=1 CYJRNFFLTBEQSQ-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 206010021639 Incontinence Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
- B01J2220/68—Superabsorbents
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249924—Noninterengaged fiber-containing paper-free web or sheet which is not of specified porosity
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Epidemiology (AREA)
- Hematology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Dispersion Chemistry (AREA)
- Absorbent Articles And Supports Therefor (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polymerisation Methods In General (AREA)
- Nonwoven Fabrics (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to materials formed from superabsorbent polymer (SAP) and fibers that are obtainable by pressing at not less than 60° C. and not less than 3 bar. More particularly, the present invention relates to materials which are obtained by in situ polymerization of SAP precursor mixtures on the fiber. The present invention also relates to processes for producing such materials and to their use.
Description
“- . PF54033
Ultra-thin materials made from fibre and superabsorbent :
The present invention relates to materials formed from superabsorbent polymer (SAP) and fibers that are obtainable by pressing at not less than 60°C and not less than 3 bar. More particularly, the present invention relates to materials which are obtained by in situ polymerization of SAP precursor mixtures on the fiber. The present invention also relates to processes for producing such materials and to their use.
In situ materials have been known since the early 1980s. They are notable for a sheetlike fibrous structure, especially a nonwoven, being treated with liquid medium which, after polymerization on the fibrous structure (in situ), forms an absorbent polymer. Polymerization may be initiated in any known way, as by radiation (UV, electron beam, heat), additives (eg redox initiators). The liquid medium contains monomers and possibly comonomers for forming the absorbent polymer.
Crosslinkers, further optional additives eg odor inhibitors, thickeners, SAP fine powder, etc may already be present in the liquid medium or only added to it after the treatment of the sheetlike structure. An aftertreatment after the polymerization, for example surface postcrosslinking, can follow. The treatment of the sheetlike structure with the liquid medium can be accomplished by spraying, drenching or other customary treatment methods.
In situ materials are known in the prior art for example in EP 40 087, EP 54 841, EP 123 500, EP 108 637, EP 223 908, EP 315 185, WO 95/33878, WO 01/56625.
Materials formed from SAP and fibers by admixing the SAP to the fibers are known. This can be accomplished in various ways, for example by addition of SAP to the process for producing a sheetlike fibrous material (air laid or wet laid) or by addition of the SAP after the fibrous material has already been shaped into a sheetlike structure. The SAP can then be fixed to the fibers by various methods, for example adhesion agents. The SAP can also be embedded as a layer between two fibrous layers (see for example: WO 95/30396).
There are many applications in the hygiene sector and non-hygiene applications where aqueous fluids are to be absorbed where it would be desirable to have materials which have one or preferably more than one of the following properties: essentially on contact with liquid to expand in one direction only, to be present in compressed form to minimize storage and transportation costs and to retain shape during storage, which have a high absorbency for aqueous solutions, for example measured in the teabag test, which provide fast liquid acquisition without pressure and under pressure, which are suitable for use as a component of laminates. 40 It has been found that, surprisingly, material formed from SAP and fibers that is obtainable by
©. 7. PF54033 pressing at not less than 60°C and not less than 3 bar has the desired properties.
Compression by the action of pressure to produce “ultrathin” hygiene articles is described in
WO 01/56625. However, the material is subjected to a pressure of about 5.5 bar (fabric area: 0.056 m? 7.000 pounds load) and a temperature of 50°C for a period of 48 seconds. This achieves a compression from originally 4.5 mm to 0.67 mm. These experimental conditions were reproduced and two differences and disadvantages compared with the present invention were ascertained: a) the material is not dimensionally stable, ie it expands to as much as 1.5 mm over 2 weeks and to as much as 2.4 mm over 8 weeks. b) The method described in the present invention makes it possible to produce significantly thinner, yet very flexible materials than the material described in WO 01 / 56625.
By application of heat and pressure it is possible to compress materials formed from SAP and fibers, for example SAP-nonwoven composites which can be produced according to
WO 01/ 56625.
The compression takes place in that dimension in which pressure is applied. The other two dimensions are left substantially unchanged by the process of compression.
Compression can be effected by initially heating the material to the requisite temperature and then applying pressure; similarly, the material can first be subjected to an applied pressure before it is heated to the requisite temperature; preferably, however, the material is compressed by the simultaneous application of pressure and heat.
The material may be compressed not only batchwise — using presses for example — but also continuously — using calenders for example.
It can be demonstrated in the context of the present invention that an application of pressure and heat is one way to obtain materials having the desired properties. The material properties are significantly more affected by varying the temperature than by varying the pressure. It has also been determined that even relatively low pressures from 3 bar, eg 3 bar, 3.5 bar, 4 bar or 4.5 bar are sufficient to produce the novel materials. Preference is given to pressures of 5 or morebar,egb,55,6,6.5,7,7.5, 8, 8.5, 9, 9.5 bar and particular preference is given to pressures above 10 bar, eg 10, 11, 12, 13, 14, 15, 20, 25, 30, 25, 40, 45, 50 or more bar.
Pressures of more than 100 bar, in contrast, generally do not lead to a further improvement in material properties. Temperature for the purposes of this invention is the temperature in the
©. PF54033 material pressed or to be pressed. When comparatively long residence times are employed for the pressing operation (1 minute for example), the temperature in the material will be substantially equal to the temperature on the surface of the press. Temperatures below 60°C are generally not sufficient. In general, temperatures of 60°C or more are employed, for example 60°C or 65°C. Preference is given to temperatures of 70°C or more, for example 70°C, 75°C, especially of 80°C or more, eg 80°C, 85°C, 90°C, 95°C, 100°C or more. The maximum temperature is dependent on the residence time of the material at the temperature, since thermal degradation of the material should be avoided. The optimum temperature range is between 80°C and 180°C, for example 110°C, 120°C, 130°C, 140°C, 150°C, 160°C or 170°C as well as the temperatures recited above. At temperatures above 200°C, the properties may deteriorate.
The desired material properties are achievable after very short times of applying pressure and heat. Residence times of 1 minute are generally sufficient. Longer residence times are generally not harmful, but not desirable for economic reasons. Typical residence times are 10 seconds, 20 seconds, 30 seconds, 40 seconds, 50 seconds or 60 seconds. But is it also possible to make the pressing time shorter for industrial fabrication, ie to use pressing times of 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10 seconds for example. Short pressing times are used with the comparatively higher temperatures. The short residence times are responsible for the fact that the compressed material can be produced continuously, using calenders or roll mills for example.
Application of pressure and heat achieves a compression to < 20%, preferably < 15%, and especially < 10% of the original thickness.
As used herein, SAP refers to superabsorbent polymer. Superabsorbent polymer is capable of absorbing at least 10 times its own weight in 0.9% NaCl solution in the CRC test. SAP is known from the prior art and in this invention is preferably based on polyacrylate. The SAP can be present in any desired form, for example in particulate form, as a fiber, film or foam, particulate being preferred. Various SAPs and their production are described for example in WO 01/56625 page 3 line 37 to line 16 on page 19.
Fibers in the context of this invention comprehends all fibers which have been combined with
SAP in the prior art. Preferred fibers are those which are present as a nonwoven. Preferred fibers are described for example in WO 01/56625 page 19 line 40 to line 27 on page 20.
Pressing refers to the application of force to the surface of the material. This can be accomplished by means of classic presses, calenders or other suitable means.
©. 7. PF54033
The present invention is the first to provide a material which expands not less than 5-fold in one dimension and by less than 20% in the other two dimensions on addition of water (distilled water) or aqueous fluids (0.9% NaCl solution).
The material exhibits a substantially one-dimensional swelling performance on application of water or aqueous fluids. The expansion in water is generally not more than 20%, preferably not more than 18%, 16%, 14% or 12%, particularly preferably not more than 10%, 8%, 7%, or 6%, especially not more than 5%, 4%, 3%, 2% or even 1% in the x- and y-axes, while the material swells in the z-axis to more than 5-fold, 6-fold or 7-fold, preferably more than 8-fold or 9-fold, especially more than 10-fold, 11-fold, 12-fold, 13-fold, 14-fold or even 15-fold or more.
The material after the application of pressure and heat is dimensionally stable; that is, little if any expansion takes place in the direction of the dimension in which the material was compressed.
The increase in the thickness of the material according to the present invention 60 days after compression is preferably less than 100%, preferably less than 80%, more preferably less than 60% and especially less than 50% based on the thickness directly after compression.
The material according to the present invention is preferably obtainable by pressure and heat treatment of material obtainable by in situ polymerization (as defined above and known from the prior art) of the SAP.
The ultrathin materials according to the present invention are suitably producible using the wovens recited in WO 01/56625. The SAP is preferably polymerized in situ on this woven, but it is also possible for example for materials to be compressed according to the present invention where the SAP has been sprinkled in or adhered atop the woven. 1t is possible to add additives to the starting material before compression. This can be effected for example by spraying with the additive or an additive solution, by drenching and also by sprinkling solid additives into the starting material or adhering solid additives atop the starting material. Additives refers for example to flavor and aroma chemicals, biocides and other odor- inhibiting materials, other active components, fertilizers and nutrients, dyes, surfactants, salts, polymers, softeners and others. tis further possible to produce laminates (multilayer materials) according to the present invention. Possibilities include not only sandwich structures, where top and bottom layers of the same material enclose a second layer different than the top and bottom layers, but also structures having two or more (partly or partially) different layers.
©. PF54033 —For example;-the starting-material can-be-converted together with cotton wovens, polyester wovens, cotton-polyester blend wovens, paper, paperboard into laminates by one-minute compression at 150°C and 80 bar, the starting material being simultaneously compressed and 5 effective in holding the components together.
By compression the present invention provides a material having a density of not less than 0.5 g/ccm, preferably not less than 0.6 g/ccm, more preferably not less than 0.7 g/ccm, even more preferably 0.8 g/ccm, yet more preferably not less than 0.9 g/ccm and especially up to not less than 1 g/ccm or more. The maximum density is generally not more than 1.2 g/ccm. Pre- compression density is typically about 0.05 g/ccm. Since the material is flexible even after compression, the compressed material occupies a significantly smaller volume than the starting product.
Density refers to the weight of the material per unit volume, volume referring to the expanse of the material (iength*width*thickness).
The ratio of teabag to retention in 0.9% NaCl solution is typically greater than 1.7 preferably greater than 1.9, more preferably greater than 2, especially greater than 2.2 (for granular SAP the value is on the order 1.2 to 1.5). This high value indicates that the compressed material is capable of taking up larger amounts of water than granular SAP. This could be because the higher water uptake is due to the pores in the unfolding woven structure (sponge effect).
Following the rapid uptake of water, the water can subsequently be taken up by the SAP (water storage). The compressed material according to the present invention accordingly has a comparable performance profile to fluff plus SAP.
The material according to the present invention has a retention in 0.9% NaCl solution of preferably more than 3 g/ccm, more preferably more than 5 g/ccm and especially more than 6.5 g/ccm or even 7 g/cem.
Retention (even in the unit g/g) is higher for the pressed material than for the uncompressed, starting material. Compressing consequently leads to a material having better properties than are possessed by the starting material. The higher the temperature at which the compressing is carried out, the higher the retention value.
When the compressed material is placed in an atmosphere containing a high water vapor concentration, the material softens.
©. PF54033
The material according to the present invention preferably has an FSEV after 60 seconds which ~is atleast double that of the uncompressed material. - - TT
The material according to the present invention also preferably has an FSEV after 2 minutes which is at least 60% higher than that of the uncompressed material.
The material according to the present invention preferably has an EVUL after 60 seconds which is at least double that of the uncompressed material.
The material according to the present invention also preferably has an EVUL after 2 minutes which is at least 60% higher than that of the uncompressed material.
The AAP (0.7 psi) value of the material according to the present invention in 0.9% NaCl solution is preferably greater than 5 g/ccm or greater than 6.5 g/cecm, preferably greater than 9 g/ccm, more preferably greater than 10 g/ccm, even more preferably greater than 11 g/ccm, especially greater than 12 g/ccm or even greater than 13 g/ccm.
The materials according to the present invention are also useful as a (multilayer) material to absorb water vapor. This property is reversible and survives a plurality of absorption-drying cycles.
These materials are very useful inter alia in the following applications to absorb water or aqueous fluid, especially body fluid: hygiene articles (for example as absorbent core, storage and/or acquisition layer in infant diapers or adult incontinence articles, sanitary napkins, etc), bed underlays, surgical drapes, wound contact materials, compresses, underiays for animal toilets, doormats, mats for absorbing snow, room climate improvement, climate improvement in seating and lying furniture, shoe soles and inserts, interlinings, garments, tablecloths, serviettes, cleaning cloths, seals or base material for seals, for example in the building sector, inner and outer pipe seals, cable sheaths, insulating and sealing material in the building industry, roof membranes (water and vapor barriers), sealing membranes for landfills, flood control (building protection, tank systems), waterways, tunnel constructions, roadbuilding, pipe liner for drilling, siccatives for transportation and storage (cereals, for example), agricultural films, including erosion control, underlays for plants, encasement of root balls, mats for germinating seed material, mats for decorative plants (windowboxes etc), sealing material in the soil against rising water and percolating water, decontamination of soils (removal of heavy metal salts for example), garbage bags, packaging, absorbent mats for transportation of moist and water- releasing goods, laminates, filters, fire protection.
© +. PF54033
The compressed material naturally has a smaller surface area than the starting material and hence a lower water takeup rate. The absorption rate canbe increased by increasing the surface area for example. Examples of suitable measures are roughening the surface or compressing in the presence of structure-conferring, surface-enlarging elements.
Test results
The base material used was Luquafleece IS from BASF Aktiengesellschaft. It is typically possible to use nonwovens having a basis weight from 20 to 2000 g/m. The examples which follow utilize a PET nonwoven having a basis weight of 100 g/m? (Sawafill 8135 from Sandler).
Luquafleece IS can be produced similarly to Example 9 of WO 01/56625 by loading the abovementioned nonwoven with 200 g/m? of SAP (100 g/m? each on both sides). It is also possible to use other loads, which are generally between 50 g/m? and 1000 g/m. The loads can be applied from one side or from both sides. Preference is given to loads between 100 g/m? and 300 g/mZ
A material was compressed under the conditions described in WO 01 / 56625 and tested for comparison. This material is referred to as “comparative material”.
Samples produced at 5, 10, 80 and 160 bar and 50, 100, 150 and 200°C were each measured in 0.9% NaCl solution and also distilled water. The test results permit the following statements to be made:
Test methods whereby the materials according to the present invention differ most distinctly from Luquafleece and the compressed material produced according to WO 01 / 56625 are CRC and also test methods involving the unit “grams of absorbed fluid/ccm”.
Retention or CRC was measured as described in WO 01/56625 page 30 lines 40 ff.
AUL or AAP were measured as described in WO 01/56625 page 30 lines 16 ff. Teabag was determined in the same way as retention but without centrifugation.
Typical values for the material according to the present invention are reported hereinbelow, the parenthetical values being those of the uncompressed starting material and of the material compressed as per WO 01/56625 at lower temperatures.
Retention (in 0.9% NaCl): 6 - 8.2 g/g (5.8 g/g & 5.9 g/g)
Retention (in 0.9% NaCl): 1500 - 2200 g/m? (1495 g/m? & 1346 g/m?)
I PF 54033
Retention (in 0.9% NaCl): 4 — 7.5 g/cem (0.3 g/ccm & 0.4 g/ccm) “Teabag(in-0.9% NaCl): 10 --20 g/ccm (0.8 g/ccm & 1.3 glccm)
Density: 0.5 — 1.2 g/ccm (0.05 g/ccm & 0.07 g/ccm)
Expansion factor (in 0.9% NaCl): 10 — 21 (1.1 & 1.7) )
AAP (in 0.9% NaCl; 0.7psi): 10.5 - 12.5 g/g (13 g/g & 12.3 g/g)
AAP (in 0.9% NaCl; 0.7psi): 2500 - 3600 g/m? (3300 g/m? & 2968 g/m?)
AAP (in 0.9% NaCl; 0.7psi): 6 — 14 g/lccm (0.6 g/g & 1.0 g/ccm)
Retention (in distilled water): 13.5 - 19 g/g (13.3 g/g & 12.9 g/g)
Retention (in distilled water): 4000 - 5400 g/m? (3455 g/m? & 3106 g/m?)
Retention (in distilled water): 10 — 16.5 g/cem (0.7 g/ccm & 0.9 g/ccm)
Teabag (in distilled water): 15 - 33 g/ccm (1.3 g/ccm & 3.0 g/lcem)
Expansion factor (in distilled water): 15 — 33 (1.5 & 2.2)
AAP (in distilled water). 18 — 22.5 g/g (18.9 g/g & 19.5 g/g)
AAP (in distilled water; 0.7psi): 5000 - 6200 g/m? (4750 g/m? & 4735 g/m?)
AAP (in distilled water; 0.7psi): 10 — 22 g/ccm (0.9 g/g & 1.4 g/ccm)
The nonwoven without SAP exhibits fundamentally different properties than Luquafleece IS.
There are even bigger differences between compressed nonwoven and compressed Luguafleece IS. The pure nonwoven has a high teabag value of 37 g/g in NaCl owing to the sponge effect and since the salt content is immaterial to this effect the same value in distilled water at 38 g/g. For the same reason the CRC value is extremely low in both the media mentioned, at 0.4 g/g; this is because the centrifuging removes substantially all of the liquid from the web.
When the nonwoven is compressed by the application of pressure and heat, it does not swell in the presence of water. The teabag and CRC values are correspondingly low. A nonwoven which had been pressed at 200°C and 80 bar for 1 minute exhibited a teabag value of 1.9 g/g and a
CRC value of 0.3 g/g in 0.9% NaCl. The thickness of the pressed material remained unchanged at0.1 mm. These results show that swelling in the z-axis is only possible in the presence of
SAP.
Ultrathin materials according to the present invention can in principle also be produced by sprinkling SAP granules or powder into a nonwoven, optionally fixing the SAP to the nonwoven using an adhesive or anchoring it to the woven by way of other techniques. Although the physical properties are similar to those of the pressed in situ material, products which have been reversibly fixed on the nonwoven have the disadvantage that the SAP will become detached again from the nonwoven by the swelling in the presence of water. In the case of compressed tL PF 54033 materials which have been polymerized in situ onto fibers, by contrast, the SAP is firmly attached -to the fiber and does not become detached-again-even in the presence of water.
Dimensional stability
The compressed material is dimensionally stable; that is, the material expands insignificantly, if at all, even in the course of prolonged storage at room temperature and relative humidities of preferably less than 60%. This dimensional stability was found with all samples which were compressed at a temperature of more than 60°C and a pressure of more than 5 bar. In the case of the comparative material produced according to WO 01 / 56625, in contrast, an expansion of the material took place under the abovementioned conditions:
Sample [mm] Thickness directly after compression [mm] Thickness after 60 days 1 0.8 24 2 0.7 1.8 3 0.7 1.9 4 0.8 23
Free-swell expansion volume as a function of time
This parameter is described in WO 01 / 56625 at page 31 lines 33 ff — FSEV. An SAP loading of 200 g/m? produced the following values in 0.9% NaCl: 5 seconds 1.4 ml 10 seconds 22ml seconds 4.3 ml 60 seconds 5.9 mi 120 seconds 7.3 mi 300 seconds 8.5 ml 600 seconds 9.0 mi 30
Compressed materials which were compressed at various pressures and temperatures (duration: 1 minute) gave the following measured values. “Comparison” refers to the sampie which was produced according to WO 01 / 56625 (5 bar, 48 s, 50°C).
Determination of free-swell expansion volume (FSEV)
’ PF 54033
Time Sbar 10bar 80bar Sbar 10bar 80bar Comparison - 100°C 100°C 100°C 150°C 150°C 150°C
ELC CT CAL CAT CELL CL CCUM CCU
300 sec [104ml 11.3 ml 11.8 ml 11.5 ml 11.6 ml 11.5 ml 95m 600sec [106ml | 5m {120ml [117ml [118ml [11.8 mI 99m
The data show that the FSEV values of the material according to the present invention (with the exception of 80 bar/150°C) are distinctly higher than those of the compressed material described in WO 01 / 56625 after just 30-60 seconds. The data also show that the final value is almost reached after about 300 seconds.
When the measurement is performed by determining the expansion volume under a load of 0.5 psi (EVUL as per WO 01/56625 page 32 lines 6 ff), a similar picture is obtained:
Determination of expansion volume under load (EVUL) at 0.5 psi
Time Sbar 10bar 80bar Sbar 10bar 80bar Comparison 100°C 100°C 100°C 150°C 150°C 150°C
BCE CL CL EC CCU LL CALL AL se [SOM [em JsBm [60m [sew [sem [stm aa CT ET CEL CL CIN CLL ELL
Ca CT CL CEL CELI CL CL ELL
The samples produced according to the present invention are faster than the comparative sample in water takeup under pressure of 0.5 psi. Only the sample produced at 80°C/150 bar gives the same value after 10 seconds, but here too all the other measured results are better than with the comparative sample.
Absorption of water vapor
The compressed material is capable of absorbing significant amounts of water vapor and rereleasing them at low relative humidities (comparable properties to Luquafleece IS). Various specimens (each 100 x 100 mm) which were compressed for one minute at 160 bar and
’ PF 54033 different temperatures were stored in a desiccator at room temperature and 95% relative ~hurnidity for 24h” The specimens weré then dried in air at 23°C-and 45% relative humidity. The results are discernible from Table A. Subsequently, the specimens were again stored in a desiccator at 95% relative humidity for 24 h and thereafter again dried at room temperature and 45% relative humidity. This cycle was carried out a third time. The results after the third cycle are reported in Table B.
Table A
Moisture absorption Moisture absorption
Sample Weight after 24 h Weight after 24 h
IEEE
TableB
Moisture absorption Moisture absorption
Sample Weight after 3 cycles Weight after 3 cycles
IEEE
PF 54033
The tests were carried out on samples measuring 30 x 50 mm in area. The AAP tests were carried out using a circular piece 6 cm in diameter (area 28.3 cm?). The tests were carried out at 0.7 psi.
The 30 x 50 mm samples were observed to swell essentially in the z-direction. A swelling of about 10% was measured in the x- or y-direction, the third dimension remained unchanged (the woven is more easily extendable in one axis than in the other dimension).
All tests were carried out according to the commonly used standard methods for SAP.
Inventive example 1
Luquafleece 1S was compressed at 100°C and 160 bar for one minute. 30 x 50 mm samples were measured. The following data were obtained in distilled water:
Thickness of compressed material: 0.3 mm
CRC: 156g/g
CRC: 4905g/ m?
Teabag value: 30.6 g / ccm®)
Retention: 16.4 g / ccm*)
Density of material used: 0.984 g/ ccm :
Expansion factor in z-axis: 31.0
AAP (0.7 psi): 19.1g/g
AAP (0.7 psi): 5689 g / m?
AAP (0.7 psi): 19.0g/ ccm *) the reported value refers to the material used
Inventive example 2
Luquafleece IS was compressed at 100°C and 80 bar for one minute. 30 x 50 mm samples were measured. The following data were obtained in distilled water:
Thickness of compressed material: 0.3 mm
CRC:15.7g/g
CRC: 4592 g/ m?
Teabag value: 31.7 g/ ccm?)
Retention: 15.3 g/ ccm*)
Claims (30)
1. Material formed from SAP and fibers that is obtainable by in situ polymerization of the SAP and by pressing at not less than 60°C and not less than 3 bar.
2. Materials as claimed in claim 1 that are obtainable by pressing at not less than 70°C.
3. Materials as claimed in claim 1 that are obtainable by pressing at not less than 80°C.
4. Materials as claimed in any one of claims 1 to 3 that are obtainable by pressing at not less than 5 bar.
5. Materials as claimed in any one of claims 1 to 3 that are obtainable by pressing at not less than 10 bar.
6. Material as claimed in any one of claims 1 to 5 that expands not less than 5-fold in one dimension and by less than 20% in the other two dimensions on addition of water.
7 Material formed from SAP and fibers that expands not less than 5-fold in one dimension and by less than 20% in the other two dimensions on addition of water.
8. Material as claimed in any one of claims 1 to 7 that expands not less than 10-fold in one dimension and by less than 10% in the other two dimensions on addition of water.
9. Material as claimed in any one of claims 1 to 8 that has a density in the range from not less than 0.5 g/lccm to 1.2 g/ccm.
10. Material as claimed in any one of claims 1 to 9 where the ratio of teabag to retention in 0.9% NaCl solution is greater than 2.
11. Material as claimed in any one of claims 1 to 10 where the retention in 0.9% NaCl solution is greater than 3 g/ccm.
12. Material as claimed in any one of claims 1 to 11 where the increase in thickness 60 days after compression is less than 100% based on the thickness directly after compression.
13. Material as claimed in any one of claims 1 to 12 where the FSEV after 60 seconds is at least double that of the uncompressed material. AMENDED SHEET
’ PF 54033
14. Material as claimed in any one of claims 1 to 13 where the FSEV after 2 minutes is at least 60% higher than that of the uncompressed material.
15. Material as claimed in any one of claims 1 to 14 where the EVUL after 60 seconds is at least double that of the uncompressed material.
16. Material as claimed in any one of claims 1 to 15 where the EVUL after 2 minutes is at least 60% higher than that of the uncompressed material.
17. Material as claimed in any one of claims 1 to 16 where the AAP (0.7 psi) in 0.9% NaCl solution is greater than 5 g/ccm.
18. Laminates comprising material as claimed in any one of claims 1 to 17.
19. The use of material and laminate material as claimed in any one of claims 1 to 18 to absorb water vapor.
20. The use of material and laminate material as claimed in any one of claims 1 to 18 to absorb water or aqueous fluid.
21. The use of material and laminate material as claimed in claim 20, wherein the aqueous fluid is body fluid.
22. The process for producing compressed material comprising SAP, obtainable by in situ polymerization of the SAP, and fiber by pressing at above 60°C and above 3 bar.
23. Material as claimed in any one of claims 1 to 17, substantially as hereinbefore described or exemplified.
24. Material according to the invention including any new and inventive integer or combination of integers, substantially as herein described.
25. Laminates as claimed in claim 18, substantially as hereinbefore described or exemplified.
26. Laminates according to the invention including any new and inventive integer or combination of integers, substantially as herein described. AMENDED SHEET
) ‘PF 54033
27. The use of material and laminate material as claimed in any one of claims 19 to 21, substantially as hereinbefore described or exemplified.
28. The use of material and laminate material including any new and inventive integer or combination of integers, substantially as herein described.
29. The process according to the invention for producing compressed material, Substantially as hereinbefore described or exemplified.
30. The process for producing compressed material including any new and inventive integer or combination of integers, substantially as herein described. AMENDED SHEET
Applications Claiming Priority (1)
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DE2002151137 DE10251137A1 (en) | 2002-10-31 | 2002-10-31 | Ultra-thin materials made of fiber and superabsorbent |
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ZA200504380B true ZA200504380B (en) | 2006-08-30 |
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US (1) | US20060014006A1 (en) |
EP (1) | EP1567260B1 (en) |
JP (1) | JP4739756B2 (en) |
KR (1) | KR20050065648A (en) |
CN (1) | CN100377777C (en) |
AT (1) | ATE419058T1 (en) |
AU (1) | AU2003274091A1 (en) |
BR (1) | BR0315726A (en) |
DE (2) | DE10251137A1 (en) |
WO (1) | WO2004039493A1 (en) |
ZA (1) | ZA200504380B (en) |
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ITTV20040095A1 (en) * | 2004-08-05 | 2004-11-05 | Silcart Srl | JACKET OF LAYERED STRUCTURE, PARTICULARLY FOR WALL INSULATION AND BUILDING ATTICS. |
EP1989185B8 (en) * | 2006-02-28 | 2013-06-26 | Dart NeuroScience LLC | Therapeutic compounds |
EP1837172A1 (en) * | 2006-03-22 | 2007-09-26 | Basf Aktiengesellschaft | Heat insulation composite system for interior insulation of buildings |
DK2314264T3 (en) * | 2008-07-11 | 2014-10-27 | Sumitomo Seika Chemicals | Water-absorbing layer composition |
JP2013503214A (en) * | 2009-08-25 | 2013-01-31 | ビーエーエスエフ ソシエタス・ヨーロピア | Soft granular superabsorbent and use thereof |
DE102009055951A1 (en) | 2009-11-27 | 2011-06-01 | Glatfelter Falkenhagen Gmbh | Absorbing structure |
ES2847975T3 (en) | 2010-01-28 | 2021-08-04 | Glatfelter Falkenhagen Gmbh | Flexible, highly absorbent material |
DE102010006228A1 (en) | 2010-01-28 | 2011-08-18 | Glatfelter Falkenhagen GmbH, 16928 | Absorbent structure for use as disposable product, for e.g. for hygiene area, particularly in hygiene product, has sequence of layers, two outer layers and liquid storage layer that is arranged between outer layers |
US20110184365A1 (en) | 2010-01-28 | 2011-07-28 | Glatfelter Falkenhagen Gmbh | Flexible, highly absorbent material |
GB2506653B (en) * | 2012-10-05 | 2017-09-27 | Speciality Fibres And Mat Ltd | Absorbent materials |
DE102013003755A1 (en) * | 2013-03-06 | 2014-09-11 | Carl Freudenberg Kg | ventilation insert |
US20160040352A1 (en) * | 2014-08-05 | 2016-02-11 | Chemstream Bvba | Poly-electrolyte polymer composition and its use |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
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US4186165A (en) * | 1976-06-14 | 1980-01-29 | Johnson & Johnson | Method of producing an absorbent panel having densified portion with hydrocolloid material fixed therein |
JPS61296162A (en) * | 1985-06-22 | 1986-12-26 | マルハ株式会社 | Water absorbability imparted paper and nonwoven fabric |
JP2682576B2 (en) * | 1988-04-28 | 1997-11-26 | 三菱レイヨン株式会社 | Absorbent |
US5100397A (en) * | 1989-06-14 | 1992-03-31 | Mcneil-Ppc, Inc. | Absorbent mixture |
JP2995079B2 (en) * | 1990-08-03 | 1999-12-27 | ユニ・チャーム株式会社 | Liquid absorption block |
US5525407A (en) * | 1994-01-03 | 1996-06-11 | Mcneil-Ppc, Inc. | Integrated absorbent structures with density and liquid affinity gradients |
SE508627C2 (en) * | 1994-05-04 | 1998-10-19 | Sca Hygiene Prod Ab | Process for preparing an absorbent structure comprising a layer of superabsorbent material |
DE4420088C3 (en) * | 1994-06-09 | 2001-02-15 | Stockhausen Chem Fab Gmbh | Process for producing a water-absorbing fabric and its use |
EP1268914A1 (en) * | 1999-09-03 | 2003-01-02 | Rayonier Products and Financial Services Company | Soft, absorbent material for use in absorbent articles and process for making the same |
US6417425B1 (en) * | 2000-02-01 | 2002-07-09 | Basf Corporation | Absorbent article and process for preparing an absorbent article |
WO2002094329A1 (en) * | 2001-05-23 | 2002-11-28 | Basf Aktiengesellschaft | Odor control containing absorbent materials |
US6645407B2 (en) * | 2001-12-14 | 2003-11-11 | Kimberly-Clark Worldwide, Inc. | Process for making absorbent material with in-situ polymerized superabsorbent |
WO2003053487A1 (en) * | 2001-12-20 | 2003-07-03 | Basf Aktiengesellschaft | Absorbent article |
US7115321B2 (en) * | 2002-07-26 | 2006-10-03 | Kimberly-Clark Worldwide, Inc. | Absorbent binder coating |
-
2002
- 2002-10-31 DE DE2002151137 patent/DE10251137A1/en not_active Withdrawn
-
2003
- 2003-10-28 DE DE50311022T patent/DE50311022D1/en not_active Expired - Lifetime
- 2003-10-28 EP EP03758075A patent/EP1567260B1/en not_active Expired - Lifetime
- 2003-10-28 WO PCT/EP2003/011930 patent/WO2004039493A1/en active Application Filing
- 2003-10-28 AU AU2003274091A patent/AU2003274091A1/en not_active Abandoned
- 2003-10-28 BR BR0315726A patent/BR0315726A/en not_active IP Right Cessation
- 2003-10-28 AT AT03758075T patent/ATE419058T1/en not_active IP Right Cessation
- 2003-10-28 JP JP2004547573A patent/JP4739756B2/en not_active Expired - Fee Related
- 2003-10-28 KR KR1020057007576A patent/KR20050065648A/en not_active Application Discontinuation
- 2003-10-28 US US10/532,279 patent/US20060014006A1/en not_active Abandoned
- 2003-10-28 CN CNB2003801024588A patent/CN100377777C/en not_active Expired - Fee Related
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- 2005-05-30 ZA ZA200504830A patent/ZA200504380B/en unknown
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ATE419058T1 (en) | 2009-01-15 |
CN100377777C (en) | 2008-04-02 |
AU2003274091A1 (en) | 2004-05-25 |
JP4739756B2 (en) | 2011-08-03 |
CN1708355A (en) | 2005-12-14 |
JP2006504876A (en) | 2006-02-09 |
WO2004039493A1 (en) | 2004-05-13 |
BR0315726A (en) | 2005-09-06 |
DE10251137A1 (en) | 2004-05-13 |
US20060014006A1 (en) | 2006-01-19 |
EP1567260A1 (en) | 2005-08-31 |
DE50311022D1 (en) | 2009-02-12 |
KR20050065648A (en) | 2005-06-29 |
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