Source: http://www.google.com/patents/US6013587?dq=5,960,411
Timestamp: 2017-08-24 00:09:27
Document Index: 742306306

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Patent US6013587 - Nonwoven articles - Google Patents
Nonwoven articles having high durability and absorbent characteristics, and their methods of manufacture, are presented. One preferred article is characterized by (a) a nonwoven web comprised of organic fibers comprised of polymers having a plurality of pendant hydroxyl groups; and (b) a binder comprising...http://www.google.com/patents/US6013587?utm_source=gb-gplus-sharePatent US6013587 - Nonwoven articles
Publication number US6013587 A
Application number US 08/655,048
Also published as CA2163109A1, CN1044269C, CN1124985A, DE69403797D1, DE69403797T2, EP0705354A1, EP0705354B1, US5641563, US5656333, US5883019, WO1994028223A1
Publication number 08655048, 655048, US 6013587 A, US 6013587A, US-A-6013587, US6013587 A, US6013587A
Inventors Jack G. Truong, Willa M. Studiner, Bradford B. Wright, Michael M. Rock, Jr.
Patent Citations (47), Non-Patent Citations (10), Referenced by (51), Classifications (27), Legal Events (4)
US 6013587 A
1. An absorbent nonwoven article comprising:
(a) a nonwoven web comprised of polyvinyl alcohol fibers; and
(b) a binder coated on at least a portion of said fibers, said binder comprising syndiotactic polyvinyl alcohol having a plurality of hydroxyl groups, said syndiotactic polyvinyl alcohol having a triad syndiotacticity of said hydroxyl groups of at least 30%.
2. An absorbent article in accordance with claim 1 wherein said binder comprises unhydrolyzed polymers derived from monomers selected from the group consisting of monomers within the general formula ##STR5## wherein: X is selected from the group consisting of Si(OR4 OR5 OR6) and OCOR7 ; and
13. An absorbent nonwoven article comprising:
(a) a nonwoven web comprised of organic fibers, said organic fibers comprised of polymers having a plurality of pendant hydroxyl groups; and
(b) a binder coated on at least a portion of said fibers, said binder consisting essentially of syndiotactic polyvinyl alcohol having a plurality of hydroxyl groups, said syndiotactic polyvinyl alcohol having a triad syndiotacticity of said hydroxyl groups of at least 30%.
14. An absorbent nonwoven article comprising:
(b) a binder coated on at least a portion of said fibers, said binder comprising syndiotactic polyvinyl alcohol having a plurality of hydroxyl groups, said syndiotactic polyvinyl alcohol having a triad syndiotacticity of said hydroxyl groups of at least 30%, wherein said binder is essentially free of a chemical crosslinking agent.
15. An absorbent nonwoven article comprising:
(a) a nonwoven web comprised of organic fibers, said organic fibers comprised of a combination of rayon fibers and polyvinyl alcohol fibers; and
To improve the tensile and tear strength of the inventive articles, and to reduce lint on the surface of the articles, it may be desirable to entangle (such as by needletacking, hydroentanglement, and the like) the uncoated web, or calender the uncoated and/or coated and cured nonwoven articles of the invention. Hydroentanglement may be employed in cases where fibers are water insoluble. Calendering of the binder coated web at temperatures from about 5 to about 40° C. below the melting point of the fiber may reduce the likelihood of lint attaching to the surface of the inventive articles and provide a smooth surface. Embossing of a textured pattern onto the wipe may be performed simultaneously with calendering, or in a subsequent step.
Tensile strength measurements were made on 1×3 inch (2.54×7.62 cm) wringer damp, die cut samples using an Instron Model "TM", essentially in accordance with ASTM test method D-5035. A constant rate of extension (CRE) was employed, and jaws were clamp-type. Rate of jaw separation was 9.3 inches/min. (23.6 cm/min).
Elmendorf tear tests were conducted on 2.5×11 inch (6.35×27.94 cm) damp, die-cut, notched (20 mm) samples, essentially in accordance with ASTM D-1424, using an Elmendorf Tear Tester model number 60-32, from Thwing-Albert Co., with a 3200 gram pendulum. An average of four measurements was used. A high value is desired.
Absorption measurements were made on 6×8 inch (15.24×20.32 cm) samples which were die-cut in damp conditions. The absorption measurements are reported using the following terms:
(g) Grams Water Absorbed per Square foot (grams/929 cm2)=3×(No Drip Weight-Dry Weight).
(j) effective water absorption=3×(no drip weight-damp weight).
Silanol modified polyvinyl alcohol granules ("R1130") were added to deionized water in proportions up to 10 wt. % solid in a stirred flask. The flask was then heated to 95° C. until reflux condition is achieved. The polymeric solution was then kept at reflux for a minimum of 45 minutes with adequate mixing. The solution was then cooled down to room temperature (about 25° C). The silanol modified PVA solution was then diluted to 2.5 wt. % solid. Reactants such as Nalco 8676, Tyzor LA, Tyzor 131, and glyoxal were then added to the silanol modified PVA solution at various proportions and combinations as described in the examples to follow.
A 12×15 inch (30.48×38.1 cm) piece of this nonwoven web was placed in a pan and saturated with approximately 200 g of an aqueous coating solution containing 5.00 g of total polymer.
Saturated samples were then dried and cured in a flow-through oven at various conditions to be described in the examples below. When curing was completed, the samples were conditioned for 60 minutes in 60-80° F. (140-176° C.) tap water then dried. Samples were then analyzed for hydrophilicity, water retention and absorption, tensile strength, tear strength, and dry wiping properties.
The test results for the inventive nonwovens of Examples 1-10 are presented in Tables 1 and 2. The nonwovens of Examples 1-10 were prepared as described in General Procedure I. For each example, 200 g of the polymeric solution (2.5 wt. % of R1130) was added with the reactants described below along with 0.1 g of Orcabrite Green BN 4009 pigment. The wt. % designated below represents the wt. % of active reactant (solid) over the R1130 polymer. The coated samples were dried at 150° F. (65.5° C.) for 2 hrs. then 250° F. (121.1° C.) for 2 hrs. and finally cured at 300° F. (148.8° C.) for 10 minutes. All samples had excellent dry wiping properties, low drag, and good feel.
The wipes of Example 11-20 were prepared as described in General Procedure I, and dried and cured as in Examples 1-10, except that the final 10 minute cure at 300° F. (121.1° C.) was eliminated. The absorbency, tensile strength and tear test results are presented in Tables 3 and 4.
It can be seen comparing the data of Tables 3 and 4 with the data of Tables 1 and 2 that addition of Tyzor LA or Tyzor 131, and the final 121.1° C. cure, gave immediate wet-out and consistently higher tensile strength and Elmendorf tear values.
The inventive nonwovens of Examples 21-27 were prepared as described in General Procedure I. For each sample, 200 g of the polymeric solution (2.5 wt. % of R1130) was mixed with 1.54 g of glyoxal (40 wt. % aqueous solution) and 0.25 g of NH4 Cl and then reacted with the reactants described below. The wt. % designated below represents the wt. % of active reactant (solid) over the R1130 polymer. The coated samples were dried at 110° F. (92.2° C.) for 4 hrs. All samples had excellent dry wiping properties, low drag, and good feel. The results of the absorbency, tensile strength, and tear strength are presented in Tables 5 and 6.
Examples 28-29 demonstrated the use of nonwoven web containing 100% PVA fibers. The nonwoven web was made from 100% PVA fibers which were 1.5 denier and 1.5 inch long (3.81 cm), purchased from Kuraray, Japan, with a basis weight of 7.0 g/ft2 (75.3 g/m2) using a carding machine known under the trade designation "Rando-Webber." A 12×15 inch (30.48×38.1 cm) sample of this web was coated with a solution containing: 130 g of R1130 solution (2.5 wt. % solid), 0.16 g of Nalco 8676 (10% solid), 1.63 g of Tyzor 131 (20 wt. % in water), and 0.16 g of Orcobrite Royal blue pigment #R2008. The coated sample was dried at 150° F. (65.5° C.) for 2 hrs. then cured at 300° F. (148.9° C.) for an additional 15 minutes. The coated sample had a rubbery feel. The absorbency and tensile strength data are presented in Tables 7 and 8.
Examples 30-31 demonstrated the use of a nonwoven web containing a blend of PVA and cotton fibers. The nonwoven web was made from 50 wt. % PVA fibers which were 1.5 denier and 1.5 inch (3.81 cm) in length, purchased from Kuraray, Japan, and 50 wt. % cotton fibers with a resultant basis weight of 5.5 g/ft2 (59.2 g/m2) using a web making machine known under the trade designation "Rando-Webber." A 12×15 inch (30.48×38.1 cm) sample of this web was coated with a solution containing: 110 g of R1130 solution (2.5 wt. % solid in H2 O), 0.13 g of Nalco 8676 (10% solid in H2 O), 1.38 g of Tyzor 131 (20% solid in H2 O), and 0.14 g of Orcobrite Royal blue pigment #R2008. The coated sample was dried at 150° F. (65.5° C.) for 2 hours, then cured at 300° F. (148.9° C.) for an additional 15 minutes. The coated sample had excellent dry wiping properties, low drag, and good feel. The absorbency and tensile strength data are presented in Tables 9 and 10.
The nonwoven web used in Example 32 was made from 100% rayon fibers which were 3.0 denier and 2.5 inches (6.35 cm) long from Courtalds Chemical Company, England, using a carding/crosslap/needletacking process. Its basis weight was 16.2 g/ft2 (174.3 g/m2). A 15×15 inch sample of this web (38.1×38.1 cm) was coated with a solution containing: 250 g of R1130 solution (2.5% solid in H2 O), 0.31 g of Nalco 8676 (10% solid in H2 O), 3.13 g of Tyzor 131 (20 wt. % in H2 O), and 0.4 g of Orcobrite Royal blue pigment #R2008. The coated sample was dried at 150° F. (65.5° C.) for 2 hours and then at 250° F. (121.1° C.) for 2 hours, and finally at 300° F. (148.8° C.) for an additional 10 minutes. The coated sample had excellent dry wiping properties, low drag, and soft feel.
An aqueous binder precursor solution was prepared for each example containing various amounts of Airvol 165 (a 99.8% hydrolyzed polyvinyl alcohol with molecular weight 110,000 and degree of polymerization 2500, obtained from Air Products) reacted with Tyzor LA and/or Tyzor 131 and optionally, glyoxal as described in Examples 34-47 and NH4 Cl, an acid catalyst. The binder precursor solutions also may have contained optional crosslinker(s) and pH modifiers as detailed in the Examples. A 12×15 inch (30.48×38.1 cm) piece of this nonwoven web was placed in a pan and saturated with approximately 200 g of an aqueous coating solution containing 5.00 g of total polymer.
Saturated samples were dried in a flow-through oven at 150° F. (65.5° C.), for between 30 minutes and 4 hours, and cured in a flow-through oven, preferably for greater than 10 minutes, at temperatures greater than 220° F. (104° C.). The samples were flipped every 10-30 minutes to aid in even drying conditions. When curing was completed, the samples were conditioned for 60 minutes in 60-80° F. (15.6-26.7° C.) tap water then dried. Samples were then analyzed for hydrophilicity, water retention and absorption, tensile strength, tear strength, and dry wiping properties.
Examples 34-38 illustrated the advantages of employing a titanate crosslinked PVA binder in wiping articles according to the invention. The wipes of Examples 34-38 were prepared as described in General Procedure II with the compositions described below at an initial coating weight of 5 g of polymeric material per 200 g solution and dried slowly at 150° F. (65.5° C.), followed by curing at 300° F. (148.9° C.). The absorbency, tensile strength, and tear data are presented in Tables 11 and 12, respectively.
Examples 39-45 illustrated the advantages of employing a titanate, and optionally, glyoxal crosslinked PVA binder in wiping articles according to the invention. The wipes of Examples 39-45 were prepared at an initial coating weight of 5 g total PVA, 1.59 g glyoxal, and 0.25 g NH4 Cl per 200 g solution and dried slowly at 150° F. (65.5°). The absorbency, tensile strength, and tear data are presented in Tables 13 and 14, respectively.
Example 46 demonstrated the ability to color the wiping articles of this invention made in accordance with General Procedure II in varying colors and shades. A binder precursor solution was prepared consisting of 100 g 5 wt. % Airvol 165, 1.68 g Tyzor LA, 0.03 g, 0.06 g, 0.13 g, 0.25 g, or 0.5 g pigment dispersion, and deionized water to achieve a total solution weight of 200 g for each run. The binder precursor solution was coated onto a 12×15 inch (30.48 cm×38.1 cm) piece of PVA/rayon nonwoven produced as described in General Procedure II, dried at 120° F. (48.9° C.) for 2 hours, and finally cured for one hour at 140° F. (57.0° C.). Upon completion of run, the samples were conditioned for 60 minutes in 60-80° F. (140-176° C.) water and dried. Results are shown below.
The aqueous pigment dispersions known under the trade designation "Aqualor" were obtained from Penn Color (Doylestown, Pa.), while those known under the trade designation Orcobrite aqueous pigment dispersions were obtained from Organic Dyestuffs (Concord, N.C.). Good results were obtained with a wide variety of the "Orcobrite" series of pigments. A major difference between the "Aqualor" and "Orcobrite" pigment dispersions, as supplied, was the substantially higher alkalinity of "Aqualor" pigment dispersions, perhaps leading to insufficient cure by the titanate crosslinking agent. Generally speaking it was found that the best results with regard to coloring were obtained at cure temperatures of 240-250° F. (115.6-121° C.), although higher temperatures were also useful.
A 12 by 15 inch (30.48×38.1 cm) piece of polyvinyl alcohol/rayon (45% polyvinyl alcohol fiber having a denier of 1.5 and a length of 1.5 inch (3.81 cm) purchased from Kuraray KK, and 55% rayon fiber having a denier of 1.5 and a length of 19/16 inch purchased from BASF) blended nonwoven fiber substrate (thickness=56 mil (0.142 cm), basis weight=11.5 g/ft2 (123.8 g/m2), prepared using a web marking of Rando-Webber) was placed in a pan and saturated with 200 g of an aqueous binder precursor solution containing 5.00 g total polyvinyl alcohol and polyacrylic acid, prepared by mixing a 5% aqueous solution of "Airvol 165" with a 2.5% aqueous solution of the polyacrylic acid. "Airvol 165" (a 99.8% hydrolyzed polyvinyl alcohol, MW=110,000, DP=2500 obtained from Air Products) was used in combination with polyacrylic acid (750,000 MW, Aldrich Chemical Co.). The binder precursor solution pH was adjusted with 85% phosphoric acid. The sample and tray were placed in a flow through drying oven at 120-150° F. (48.9-65.5° C.) for 2 hours followed by curing at 300° F. (148.9° C.) as specified in Table 15. The samples were flipped over after about 30 minutes and 60 minutes to aid in maintaining even drying. When curing was completed the samples were conditioned for 60 minutes in 60-80° F. water then dried.
TABLE 15______________________________________                        % Coating                                Conditioned                        Loss During                                Coat Wt.Ex.# Description Cure Conditions                        Conditioning                                (g/m2)______________________________________48   Polyacrylic 2 HR 120° F.                        4       40.5Acid, pH = 3.0,            (48.9° C.)/COMPARATIVE 5 MIN 300° F.            (148.9° C.)49   Airvol 165  2 HR 120° F.                        1       48.4(polyvinyl  (48.9° C.)/alcohol),   5 MIN 300° F.pH = 3.0,   (148.9° C.)COMPARATIVE50   1 part      2 HR 120° F.                        0       49.5Polyacrylic (48.9° C.)/acid/       5 MIN 300° F.2 parts Airvol            (148.9° C.)165, pH = 3.051   1 part      2 HR 120° F.                        0       48.2Polyacrylic (48.9° C.)/acid/       5 MIN 300° F.3 parts Airvol            (148.9° C.)165, pH = 3.052   1 part      2 HR 120° F.                        0       56.9Polyacrylic (48. 9° C.)/acid/       5 MIN 300° F.5 parts Airvol            (148.9° C.)165, pH = 3.053   1 part      2 HR 120° F.                        0       58.5Polyacrylic (48.9° C.)/acid/       5 MIN 300° F.10 parts Airvol            (148.9° C.)165, pH = 3.054   1 part      2 HR 150° F.                        0       52.4Polyacrylic (65.6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.555   1 part      2 HR 150° F.                        0       51.6Polyacrylic (65.6° C.)/acid/       15 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.556   1 part      2 HR 150° F.                        0       55.4Polyacrylic (65.6° C.)/acid/       25 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.557   0.1 part    2 HR 150° F.                        1       49.5Polyacrylic (65.6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.558   0.5 part    2 HR 150° F.                        1       53.5Polyacrylic (65. 6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.559   1 part      2 HR 150° F.                        0       55.4Polyacrylic (65.6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.560   1 part      2 HR 150° F.                        0       49.7Polyacrylic (65.6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 4.061   1 part      2 HR 150° F.                        0       52.3Polyacrylic (65.6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 4.662   1 part      2 HR 150° F.                        1       48.3Polyacrylic (65.6° C.)/acid/       5 MIN 300° F.99 parts Airvol            (148.9° C.)165, pH = 3.3______________________________________
A 12 by 15 inch (30.48×38.1 cm) piece of polyvinyl alcohol/rayon (45% polyvinyl alcohol fiber having a denier of 1.5 and a length of 1.5 in (3.81 cm) purchased from Kuraray KK, and 55% rayon fiber having a denier of 1.5 and a length of 1.56 inch (3.96 cm) purchased from BASF) blended nonwoven fiber substrate (thickness=56 mil (0.142 cm), basis weight 11.5 g/ft2 (123.8 g/cm2), prepared using a web making machine known under the trade designation "Rando-Webber") was placed in a pan and saturated with 200 g of an aqueous binder precursor solution containing 5.00 g total polyvinyl alcohol. "Airvol 165" (a 99.8% hydrolyzed polyvinyl alcohol, MW=110,000, DP=2500 obtained from Air Products) was used in combination with syndiotactic polyvinyl alcohol prepared in Example 64 to comprise the polyvinyl alcohol content in Examples 65-91. The binder precursor solutions may also have contained optional crosslinker(s), and pH modifiers depending on the Example. The sample and tray were placed in a flow through drying oven at 120-50° F. (48.9-65.6° C.) for 3 to 4 hours as specified. The samples were flipped over after about 30 minutes and 60 minutes to aid in maintaining even drying. When curing was completed the samples were conditioned for 60 minutes in 60-80° F. (15.6-26.7° C.) water then dried. Samples were then analyzed for wet out, absorptivity, tensile strength, tear strength, and dry wiping properties, with the results reported in Tables 18-27.
The polyvinyl trifluoroacetate (PVTFA) copolymer described above (300 g) was dissolved in 700 g acetone. This solution was slowly added to 1700 g of 10% methanolic ammonia that had been cooled in ice to 15° C. Despite vigorous mechanical stirring a large ball of solid material formed on the stirrer blade making stirring ineffective. After addition was complete the ball of material was broken up by hand and the mixture was shaken vigorously. The process was repeated twice more (elapsed time was about 3 hr). The divided mass was vigorously mechanically stirred for 20 minutes and allowed to stand at room temperature overnight.
The supernatant liquid was decanted off leaving a mixture of white powder and yellow fibrils. The solids were collected by filtration and spread in a tray at 15.6° C. to evaporate residual solvent. The solids were collected when constant weight over 2 hr was achieved. The solid was chopped in a blender to give 87.3 g of beige powder, 92% yield, referred to hereinafter as "Syn". Analysis of this material was carried out using IR and 1 H NMR spectroscopy, and Gel Permeation Chromatography. The results indicated the likely presence of traces of trifluoroacetate esters and salts. The triad syndiotacticity measured by 1 H NMR in DMSO-d6 was 33%, atacticity=50%, isotacticity=17%, The difference between the hydrolyzed polymer and the trifluoroacetate precursor polymer may be due to acid catalyzed epimerization of hydroxyl groups during drying or solution in boiling water.
Examples 65-70 illustrated the advantages of employing syndiotactic polyvinyl alcohol alone or in blends with atactic polyvinyl alcohol in wiping articles according to the invention. The articles were prepared at an initial coating weight of 5 g total PVA/200 g solution. Curing conditions were 4 hr at 48.9° C.
These examples demonstrated the use of syndiotactic polyvinyl alcohol with chemical crosslinkers (Tyzor LA and/or glyoxal) in wiping articles according to the invention. Curing conditions were 3.5 hr at 150° F. (65.5° C.). Mole % crosslinking amounts for Tyzor LA were based on four bonds between titanium and polyvinyl alcohol. Mole % crosslinking amounts for glyoxal were based on four bonds between glyoxal and polyvinyl alcohol.
TABLE 24__________________________________________________________________________    Tensile          Tensile                % Weight   Elmendorf    Strength          Strength                Loss Elmendorf                           Tear    Machine          Cross During                     Tear  CrossEx.      Direction          Direction                Condition-                     Machine                           Direct-# Description    (KPa) (KPa) ing  Direction                           ion__________________________________________________________________________84  5 g:100% Syn    2661 ± 117          1979 ± 69                5.5  100+  91 ± 085  2 g:100%    2006 ± 131          1351 ± 34                3.3  75 ± 6                           96 ± 2  Syn86  1 g:100%    1441 ± 138          1186 ± 89                2.9  84 ± 9                           100+  syn__________________________________________________________________________
A sample containing 5 g 30% syndiotactic PVA as the only binder component in 200 g total solution was prepared and coated as in Examples 84-86 containing 0.1 g "Orcobrite Blue 2GN" pigment (Organic Dyestuffs Corp., Concord, N.C.). The sample was cured at 250° F. (121° C.) for 2 hours. The sample discolored slightly and had a strong odor, but was colorfast after conditioning in luke-warm water for 2 hours.
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U.S. Classification 442/166, 442/59, 442/104, 442/102
International Classification D04H1/64, D06M101/06, D06M101/18, D06M101/16, D06M101/32, D06M101/00, D06M101/30, D06M15/356, D06M15/333, D06M13/503, D06M13/02, D06M101/02
Cooperative Classification D04H1/64, D04H1/587, Y10T442/20, Y10T442/60, Y10T442/2352, Y10T442/2861, Y10T442/676, Y10T442/2877, Y10T442/2369
European Classification D04H1/64A, D04H1/64C