US3772069A - Bonded nonwoven sheet bearing a lubricating composition of a liquid polysiloxane and a liquid polyoxypropylene compound - Google Patents
Bonded nonwoven sheet bearing a lubricating composition of a liquid polysiloxane and a liquid polyoxypropylene compound Download PDFInfo
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- US3772069A US3772069A US00125355A US3772069DA US3772069A US 3772069 A US3772069 A US 3772069A US 00125355 A US00125355 A US 00125355A US 3772069D A US3772069D A US 3772069DA US 3772069 A US3772069 A US 3772069A
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- polysiloxane
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- -1 polysiloxane Polymers 0.000 title claims abstract description 53
- 229920001451 polypropylene glycol Polymers 0.000 title claims abstract description 33
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 28
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- 150000001875 compounds Chemical class 0.000 title claims abstract description 13
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 title abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 10
- 239000004743 Polypropylene Substances 0.000 claims description 8
- 229920001155 polypropylene Polymers 0.000 claims description 8
- 238000009732 tufting Methods 0.000 abstract description 20
- 238000010014 continuous dyeing Methods 0.000 abstract description 13
- 239000004745 nonwoven fabric Substances 0.000 abstract description 3
- 238000004043 dyeing Methods 0.000 description 17
- 239000000839 emulsion Substances 0.000 description 14
- 239000000975 dye Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 239000000314 lubricant Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000006260 foam Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002562 thickening agent Substances 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 239000004088 foaming agent Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- 229920002176 Pluracol® Polymers 0.000 description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- ZJKLNUHASXGERK-UHFFFAOYSA-M chembl3185301 Chemical compound [Na+].NC1=CC=C2C=C(S([O-])(=O)=O)C=C(O)C2=C1N=NC1=CC=CC=C1C(F)(F)F ZJKLNUHASXGERK-UHFFFAOYSA-M 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 2
- 235000019799 monosodium phosphate Nutrition 0.000 description 2
- 229920006294 polydialkylsiloxane Polymers 0.000 description 2
- 238000009991 scouring Methods 0.000 description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- NTOOJLUHUFUGQI-UHFFFAOYSA-M sodium;4-(4-acetamidoanilino)-1-amino-9,10-dioxoanthracene-2-sulfonate Chemical compound [Na+].C1=CC(NC(=O)C)=CC=C1NC1=CC(S([O-])(=O)=O)=C(N)C2=C1C(=O)C1=CC=CC=C1C2=O NTOOJLUHUFUGQI-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001346 alkyl aryl ethers Chemical class 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- PBOIUUROGJVVNC-UHFFFAOYSA-L disodium 2-hydroxy-5-[[4-[[2-methoxy-4-[(3-sulfonatophenyl)diazenyl]phenyl]carbamoylamino]phenyl]diazenyl]benzoate Chemical compound [Na+].[Na+].COc1cc(ccc1NC(=O)Nc1ccc(cc1)N=Nc1ccc(O)c(c1)C([O-])=O)N=Nc1cccc(c1)S([O-])(=O)=O PBOIUUROGJVVNC-UHFFFAOYSA-L 0.000 description 1
- FPVGTPBMTFTMRT-UHFFFAOYSA-L disodium;2-amino-5-[(4-sulfonatophenyl)diazenyl]benzenesulfonate Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C(N)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 FPVGTPBMTFTMRT-UHFFFAOYSA-L 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 235000019233 fast yellow AB Nutrition 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31667—Next to addition polymer from unsaturated monomers, or aldehyde or ketone condensation product
-
- 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
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
- Y10T428/31938—Polymer of monoethylenically unsaturated hydrocarbon
-
- 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
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- Y10T442/2311—Coating or impregnation is a lubricant or a surface friction reducing agent other than specified as improving the "hand" of the fabric or increasing the softness thereof
- Y10T442/2328—Organosilicon containing
-
- 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
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- Y10T442/2861—Coated or impregnated synthetic organic fiber fabric
- Y10T442/291—Coated or impregnated polyolefin fiber fabric
- Y10T442/2918—Polypropylene fiber fabric
Definitions
- a typical continuous dyeing process comprises the steps of 1) application of about 100 percent wet pickup of a prepad solution to wet all carpet face fibers; 2) application of about 400 percent of a dye solution which is metered onto the carpet face by doctoring the solution from a roll rotating in the dye solution; 3) steaming the carpet at 100C. for about minutes; 4) scouring the carpet; 5) removing excess water with suction; and 6) drying the carpet in an oven.
- the prepad solution generally contains a pH adjustor and a thickener to keep the solution on the carpet face fibers.
- the dye solution contains dyes, foaming agent, pH adjustors, and a thickener.
- the steaming operation is probably the most critical of the entire process. In this operation, condensation of water vapor on the carpet causes a large generation of foam on the carpet surface. This foam distributes the dyestuff evenly throughout the face yarn and helps ensure uniform dyeing. If the foam generation is too low, the surface fibers will not be dyed and the carpet surface will have a frosty appearance. When the foam is uneven, spots of undyed fibers will result.
- the scouring and drying operations are well known in the art.
- the first step in the production of tufted carpets usually involves tufting the face yarns into a primary carpet backing, which is a relatively slow operation. When sufficient yardage of a given style has been produced, the material is stored until dyeing facilities are available. The time elapsed between tufting and dyeing, lag time, of the primary carpet backing may range from l-2 days to 34 weeks. When carpet produced from a primary carpet backing lubricated with a polymethylhydrogensiloxane is lagged more than two to three days before dyeing, poor dyeing performance is obtained in continuous dyeing processes, this typically being characterized by a frosty appearance in the dyed carpet.
- Polydialkylsiloxanes appear to present much less problem than the polyalkylhydrogensiloxanes when applied to carpet backings destined for continuous dyeings; but the dialkyl products present another problem; these products give carpets which are scroopy underfoot, i.e., the carpet pile has an annoying crunchy feel when walked upon.
- the invention provides a bonded nonwoven sheet of synthetic organic fibers having applied thereon a lubricating composition comprising 3-50 percent by weight of a liquid polysiloxane and 50-97 percent by weight of defined liquid polyoxypropylene compound in an amount such that the quantity of polysiloxane present on the sheet is in the range of about 0.06-0.8 percent by weight.
- This lubricated, nonwoven fabric is suitable as a primary carpet backing which has high strength after tufting and performs acceptably in continuous dyeing operations.
- the preferred nonwoven sheets which are lubricated in accordance with this invention are of the type disclosed and claimed in Petersen U.S. Pat. No. 3,502,538.
- the sheets comprise continuous filaments of isotactic polypropylene which have been segmentally drawn by passage over a heated roll adapted with an axially slotted surface to heat only segments of the filaments, followed by passage over unheated draw rolls.
- Other polypropylene filaments for example drawn at a single draw ratio, or at two or more different draw ratios, may be used, as can filaments from other spinnable polymers such as polyesters, polyamides, etc.
- the most preferred lubricated nonwoven sheets of this invention are made from continuous polypropylene filaments which are preferentially aligned in the length and width directions, as disclosed in Edwards U.S. Pat. No. 3,563,838. These sheets, which are particularly suited for use as primary carpet backings due to their high dimensional stability and strength after tufting, may be prepared by the process described in Troth U.S. Pat. No. 3,477,103. In this process, a primary fluid stream containing a plurality of electrostatically charged continuous filaments is forwarded toward a laydown zone on a receiver surface moving away from the laydown zone.
- Two secondary fluid streams are alternately impinged on opposite sides of the primary fluid stream thereby deflecting said primary stream and the contained filaments in opposite directions, the filaments being laid down in swaths on the receiver, aligned in the direction of deflection.
- a plurality of filament deflecting devices can be used and disposed so as to provide filament alignment in the machine (length) and in the cross-machine (width) direction.
- the nonwoven sheets of this invention may be bonded by methods known in the art but are preferably self-bonded by exposure to saturated steam to provide bond-strength distributions as described in Petersen U.S. Pat. No. 3,502,538. Suitable apparatus for effecting this steam-bonding is described in Wyeth U.S. Pat. No. 3,313,002. In the following examples, bonding was accomplished in this manner.
- the lubricating compositions used in accordance with this invention consist of mixtures comprising 3-50 percent and preferably 5-20 percent by weight of liquid polymonoalkyl or polydialkylsiloxane with 50-97 percent and preferably 80-95 percent by weight of liquid polyoxypropylene compound having a viscosity of at least 100 centipoise at 25C.
- the polyoxypropylene component may either have two hydroxy end groups, i.e., the glycol, or may have one hydroxy end group and one alkoxy (preferably from one to six carbon atoms) end group, i.e., the monoalkyl ether.
- the specified polysiloxanes and polyoxypropylene compounds form relatively stable emulsions when combined and other additives are not needed unless the emulsions are expected to stand for several hours before use.
- the emulsion of the invention can be applied to the nonwoven sheets by spraying, gravure coating or other techniques.
- a preferred emulsion for providing high tufted tongue tear strength while avoiding frostiness in continuous dyeing is prepared from a polymethylhydrogensiloxane (available from Dow-Corning Corp. as DC1107) and a polyoxypropylene glycol (a dihydroxy material available from Wyandotte Chemical Corp. as Pluracol P1010).
- a preferred emulsion for high tufted tear strength without development of scroopiness in carpet is a mixture of polydimethylsiloxane (available from Dow- Corning Corp. as DC-200) and the monobutylether of polyoxypropylene glycol (available from Union Carbide Chemical Corp. as Ucon LB385).
- the effectiveness of a tufting lubricant may be determined by tufting the lubricated sheet and measuring the tear strength of the tufted sheet, the more effective the lubricant, the higher the tear strength.
- lubricant effectiveness was measured by tufting the lubricated sheets on a table-top tufter with 3700 denier bulked continuous filament nylon yarn, at 7 tufts/inch (in the machine or length direction) the tufts being spaced three-sixteenths inch apart in the width direction and having a height of sevensixteenths inch.
- the machine direction tufted tongue tear strength was measured in the following manner.
- the tufted nonwoven sheet is cut into a sample 6 inches wide (crossmachine direction, across tufting rows) and 8 inches long (machine direction along tufting rows).
- the sample is cut in the center of the width 4 inches in the machine (tufting) direction.
- the sample is mounted in an Instron" tester using 1.5 inch by 2 inch serrated clamps. With a jaw separation of 3 inches, one side of the sample cut is mounted in the upper jaw and the other side of the sample cut is mounted in the lower jaw.
- the sample is uniformly spaced between the jaws.
- the full scale load is adjusted to a value greater than the tear strength expected for the sample.
- the Instron is started and the sample is torn. An average of the three highest stresses during tearing is taken. The tongue tear strength in pounds is reported as this average divided by 100 and multiplied by the full scale load. In general several determinations are made and the average reported.
- the dyeing tests were carried out in continuous dyeing equipment developed by the Kusters Co., Germany (distributed in the U. S. by Zima Corporation, Spartanburg, S.C.). Most of the tests were carried out in semiworks type equipment capable of continuously dyeing tufted goods about 36 inches wide, but some tests were carried out in commercial size equipment capable of handling tufted goods up to 15 feet wide.
- Emulsions were formed from different amounts of polymethylhydrogensiloxane (DC1107) and polyoxypropylene glycol (Pluracol" P- l 010) described above, the latter having a viscosity of about 155 centipoise at 25C. These were sprayed in an amount of about 2 percent by weight onto a 3.5 oz./yd. bonded nonwoven sheet from segmentally drawn continuous polypropylene filaments, in which the filaments were preferentially aligned in the machine and cross-machine direction, the sheet being prepared by the process described in Troth U.S. Pat. No. 3,477,103. The samples were tufted and the tear strength measured in the manner described above.
- EXAMPLE II A 3.0 oz./yd. nonwoven sheet, produced from continuous polypropylene filaments in the manner generally described in Example I was lubricated with various amounts of an emulsion formed from 95 percent by weight of the polyoxypropylene glycol (Pluracol" P-10l0) and 5 percent by weight of polymethylhydrogensiloxane (DC-1107). Samples of these lubricated sheets were tufted and the tufted tongue tear measured. The results, summarized in Table II, again indicate that the tufted tongue tear starts to decrease sharply when the amount of polysiloxane on the sheet drops below about 0.06 percent.
- Pluracol polyoxypropylene glycol
- DC-1107 polymethylhydrogensiloxane
- DuPonol FAB Foaming Agent E. I. du Pont de Nemours & Co., Inc.
- Polygum 260 Thickener Polymer Industries Incorporated 6 g/l Monosodium Phosphate (PI-I buffer): 2 g/l Color Index Direct Yellow 44 3 g/l Color Index Acid Red 337 0.28 g/l Color Index Acid Blue 40 0.95 g/l Prepad Bath (Pickup 100 percent) Merpol WF (Wetting Agent E. I. du Pont de Nemours & Co., Inc.): 5 g/] DuPonol FAB (Foaming Agent E. I.
- du Pont de Nemours & Co., Inc. 2 g/l All the samples were dyed under essentially the same conditions using a steaming time of about 8 minutes at 100C. After drying, the dyed samples were subjectively evaluated for appearance, dye uniformity, lack of frostiness, etc., the criterion for acceptability being that the product should be free of dyeing defects when dyed at least three weeks and preferably four weeks after tufting.
- EXAMPLE V Additional tests were carried out using a 3 or/yd. nonwoven polypropylene primary carpet backing to which was applied various amounts of an emulsion containing 95 percent polyoxypropylene glycol and 5 percent polymethylhydrogensiloxane previously described. After tufting, the continuous dyeing performance of the various samples was tested every week, for a number of weeks, to determine how many weeks each sample could be lagged and still obtain acceptable dyeing performance.
- Formulations of the baths used in the dyeing operation are listed in Table VI and the dye-quality results are given in Table VI]. These results indicate that acceptable performance is obtained with up to 0.72 percent of polysiloxane on the sheet and that the lag time for acceptable performance increases as the amount of polysiloxane on the sheet decreases.
- Example II produced in the manner generally described in Example I were lubricated (a) with an amount of an emulsion of a polysiloxane and a polyoxypropylene compound, (b) with the polyoxypropylene compound alone and (c) with the polysiloxane alone, the respective amounts of the components in items (b) and (c) being about the same as those present in combination in item (a).
- the actual materials used and the amount of finish by weight are listed in Table VIII which also gives the results of the tufted tongue tear measurements. In each case, it is seen that the tear strength is significantly higher in samples lubricated with the two component emulsion than with either component separately.
- Example VIa The carpet of Example VIa was allowed to stand for three weeks and was then subjected to a continuous dyeing operation as described in previous examples. Dyeing was uniform and acceptable.
- a bonded nonwoven synthetic organic fiber sheet to which has been applied a lubricating composition consisting essentially of 3-50 percent by weight of a liquid polysiloxane selected from the group of polymethyl hydrogen siloxane and polydimethyl siloxane and 50-97 percent by weight of a liquid polyoxypropylene compound having a viscosity of at least 100 centipoises at 25C. and selected from the group of polyoxypropylene glycol and the monobutyl ether thereof, said composition being present in an amount such that the quantity of polysiloxane on the sheet is in the range of about 0.06 and 0.8 percent by weight.
- the sheet of claim 3 wherein the lubricating composition comprises 5-20 percent by weight of polysiloxane and 80-95 percent by weight of polyoxypropylene compound.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Laminated Bodies (AREA)
Abstract
A bonded nonwoven sheet of synthetic organic fibers having applied thereon a lubricating composition comprising 3-50 percent by weight of liquid polysiloxane and 50-97 percent by weight of defined liquid polyoxypropylene compound, in an amount such that the quantity of polysiloxane present on the sheet is in the range of about 0.06 to 0.8 percent by weight. This lubricated nonwoven fabric is suitable as a primary carpet backing which has high strength after tufting and performs acceptably in continuous dyeing operations.
Description
United States Patent [1 1 Daniel [11] 3,772,0 9 [451 Nov. 13, 1973 BONDED NONWOVEN SHEET BEARING A LUBRICATING COMPOSITION OF A LIQUID POLYSILOXANE AND A LIQUID POLYOXYPROPYLENE COMPOUND [75] Inventor: John Lewis Daniel, Hendersonville,
Tenn.
[73] Assignee: E. I. du Pont de Nemours and Company, Wilmington, Del.
{22] Filed: Mar. 17, 1971 21 App]. No.: 125,355
[52] US. Cl. ..1l7/l38.8 E, 9 1 SB, 1. 11139 CQ [51] Int. Cl. B32b 27/06, D06m 13/00 [58] Field of Search 117/138.8 E, 139.5 CQ, 117/140 R; 252/8.9; 106/287 SB [56] References Cited UNITED STATES PATENTS 5/1967 Jung 161/170 X 11/1971 Smith 252/8.9
2,955,047 10/1960 Terry 106/287 3,140,198 7/1964 Dawson et al. 252/8.9 X 2,757,094 7/1956 Guss 106/287 FOREIGN PATENTS OR APPLICATIONS 21,769 8/1961 Germany 828,735 2/1960 Great Britain Primary Examiner-William D Martin Assistant Examiner-Sadie L. Childs Att0rney-Sol Schwartz 57 ABSTRACT A bonded nonwoven sheetof synthetig ganic fibers 4 Claims, N0 Drawings BONDED NONWOVEN SHEET BEARING A LUBRICATING COMPOSITION OF A LIQUID POLYSILOXANE AND A LIQUID POLYOXYPROPYLENE COMPOUND BACKGROUND OF THE INVENTION The invention relates to treated continuous filament nonwoven materials which are suitable as tufting substrates in the production of tufted carpets. Jung, in U.S. Pat. No. 3,322,607, has disclosed continuous filament nonwoven materials which can be used as primary carpet backings in the production of tufted carpets. The same patent also discloses that it is necessary to treat these products with a lubricant prior to tufting, and discloses the use of polysiloxanes as tufting lubricants.
The production of tufted carpets, usually includes a dyeing operation to dye the face yarns. Conventionally, this dyeing operation was effected in dye-becks in which the carpet was formed into a continuous belt and cycled in the dye-beck until the correct face yarn color had been obtained. More recently, however, continuous dyeing processes have been developed in which an undyed, tufted primary carpet backing enters at one end of an apparatus and exits at the other end with dyed face yarns. A typical continuous dyeing process comprises the steps of 1) application of about 100 percent wet pickup of a prepad solution to wet all carpet face fibers; 2) application of about 400 percent of a dye solution which is metered onto the carpet face by doctoring the solution from a roll rotating in the dye solution; 3) steaming the carpet at 100C. for about minutes; 4) scouring the carpet; 5) removing excess water with suction; and 6) drying the carpet in an oven.
The prepad solution generally contains a pH adjustor and a thickener to keep the solution on the carpet face fibers. The dye solution contains dyes, foaming agent, pH adjustors, and a thickener. The steaming operation is probably the most critical of the entire process. In this operation, condensation of water vapor on the carpet causes a large generation of foam on the carpet surface. This foam distributes the dyestuff evenly throughout the face yarn and helps ensure uniform dyeing. If the foam generation is too low, the surface fibers will not be dyed and the carpet surface will have a frosty appearance. When the foam is uneven, spots of undyed fibers will result. The scouring and drying operations are well known in the art.
The first step in the production of tufted carpets usually involves tufting the face yarns into a primary carpet backing, which is a relatively slow operation. When sufficient yardage of a given style has been produced, the material is stored until dyeing facilities are available. The time elapsed between tufting and dyeing, lag time, of the primary carpet backing may range from l-2 days to 34 weeks. When carpet produced from a primary carpet backing lubricated with a polymethylhydrogensiloxane is lagged more than two to three days before dyeing, poor dyeing performance is obtained in continuous dyeing processes, this typically being characterized by a frosty appearance in the dyed carpet.
Investigations revealed that this poor dyeing performance is due to a reduction in the foam level during the steaming operation, and that this is apparently a result of the presence of the polymethylhydrogensiloxane. Although reducing the amount of polysiloxane on the primary carpet backing can provide some improvements in dyeing performance, this reduction has a deleterious effect on the strength of the tufted material. Furthermore, uniform application of very small amounts of a polysiloxane onto a backing is extremely difficult and generally results in areas having a pickup sufficiently high to pose dyeing problems and other areas where the pickup is so low as to be ineffective as a tufting lubricant.
Polydialkylsiloxanes appear to present much less problem than the polyalkylhydrogensiloxanes when applied to carpet backings destined for continuous dyeings; but the dialkyl products present another problem; these products give carpets which are scroopy underfoot, i.e., the carpet pile has an annoying crunchy feel when walked upon.
The problem encountered in continuous dyeing of carpet and the problem relating to feel of the carpet underfoot have both been resolved by the present invention and these problems have been resolved without an appreciable loss in tear strength in the tufted carpet.
SUMMARY OF THE INVENTION The invention provides a bonded nonwoven sheet of synthetic organic fibers having applied thereon a lubricating composition comprising 3-50 percent by weight of a liquid polysiloxane and 50-97 percent by weight of defined liquid polyoxypropylene compound in an amount such that the quantity of polysiloxane present on the sheet is in the range of about 0.06-0.8 percent by weight. This lubricated, nonwoven fabric is suitable as a primary carpet backing which has high strength after tufting and performs acceptably in continuous dyeing operations.
DESCRIPTION OF THE PREFERRED EMBODIMENTS The preferred nonwoven sheets which are lubricated in accordance with this invention are of the type disclosed and claimed in Petersen U.S. Pat. No. 3,502,538. Preferably, the sheets comprise continuous filaments of isotactic polypropylene which have been segmentally drawn by passage over a heated roll adapted with an axially slotted surface to heat only segments of the filaments, followed by passage over unheated draw rolls. Other polypropylene filaments, for example drawn at a single draw ratio, or at two or more different draw ratios, may be used, as can filaments from other spinnable polymers such as polyesters, polyamides, etc.
The most preferred lubricated nonwoven sheets of this invention are made from continuous polypropylene filaments which are preferentially aligned in the length and width directions, as disclosed in Edwards U.S. Pat. No. 3,563,838. These sheets, which are particularly suited for use as primary carpet backings due to their high dimensional stability and strength after tufting, may be prepared by the process described in Troth U.S. Pat. No. 3,477,103. In this process, a primary fluid stream containing a plurality of electrostatically charged continuous filaments is forwarded toward a laydown zone on a receiver surface moving away from the laydown zone. Two secondary fluid streams are alternately impinged on opposite sides of the primary fluid stream thereby deflecting said primary stream and the contained filaments in opposite directions, the filaments being laid down in swaths on the receiver, aligned in the direction of deflection. For the commercial production of nonwoven fabrics, a plurality of filament deflecting devices can be used and disposed so as to provide filament alignment in the machine (length) and in the cross-machine (width) direction.
The nonwoven sheets of this invention may be bonded by methods known in the art but are preferably self-bonded by exposure to saturated steam to provide bond-strength distributions as described in Petersen U.S. Pat. No. 3,502,538. Suitable apparatus for effecting this steam-bonding is described in Wyeth U.S. Pat. No. 3,313,002. In the following examples, bonding was accomplished in this manner.
The lubricating compositions used in accordance with this invention consist of mixtures comprising 3-50 percent and preferably 5-20 percent by weight of liquid polymonoalkyl or polydialkylsiloxane with 50-97 percent and preferably 80-95 percent by weight of liquid polyoxypropylene compound having a viscosity of at least 100 centipoise at 25C. The polyoxypropylene component may either have two hydroxy end groups, i.e., the glycol, or may have one hydroxy end group and one alkoxy (preferably from one to six carbon atoms) end group, i.e., the monoalkyl ether. The specified polysiloxanes and polyoxypropylene compounds form relatively stable emulsions when combined and other additives are not needed unless the emulsions are expected to stand for several hours before use. The emulsion of the invention can be applied to the nonwoven sheets by spraying, gravure coating or other techniques.
A preferred emulsion for providing high tufted tongue tear strength while avoiding frostiness in continuous dyeing is prepared from a polymethylhydrogensiloxane (available from Dow-Corning Corp. as DC1107) and a polyoxypropylene glycol (a dihydroxy material available from Wyandotte Chemical Corp. as Pluracol P1010).
A preferred emulsion for high tufted tear strength without development of scroopiness in carpet is a mixture of polydimethylsiloxane (available from Dow- Corning Corp. as DC-200) and the monobutylether of polyoxypropylene glycol (available from Union Carbide Chemical Corp. as Ucon LB385).
The effectiveness of a tufting lubricant may be determined by tufting the lubricated sheet and measuring the tear strength of the tufted sheet, the more effective the lubricant, the higher the tear strength. In the following examples, lubricant effectiveness was measured by tufting the lubricated sheets on a table-top tufter with 3700 denier bulked continuous filament nylon yarn, at 7 tufts/inch (in the machine or length direction) the tufts being spaced three-sixteenths inch apart in the width direction and having a height of sevensixteenths inch.
The machine direction tufted tongue tear strength was measured in the following manner. The tufted nonwoven sheet is cut into a sample 6 inches wide (crossmachine direction, across tufting rows) and 8 inches long (machine direction along tufting rows). The sample is cut in the center of the width 4 inches in the machine (tufting) direction. The sample is mounted in an Instron" tester using 1.5 inch by 2 inch serrated clamps. With a jaw separation of 3 inches, one side of the sample cut is mounted in the upper jaw and the other side of the sample cut is mounted in the lower jaw. The sample is uniformly spaced between the jaws. The full scale load is adjusted to a value greater than the tear strength expected for the sample. Using a cross head speed of 12 inches per minute and a chart speed of 10 inches per minute, the Instron is started and the sample is torn. An average of the three highest stresses during tearing is taken. The tongue tear strength in pounds is reported as this average divided by 100 and multiplied by the full scale load. In general several determinations are made and the average reported.
The dyeing tests were carried out in continuous dyeing equipment developed by the Kusters Co., Germany (distributed in the U. S. by Zima Corporation, Spartanburg, S.C.). Most of the tests were carried out in semiworks type equipment capable of continuously dyeing tufted goods about 36 inches wide, but some tests were carried out in commercial size equipment capable of handling tufted goods up to 15 feet wide.
EXAMPLE I This example demonstrates the need for a minimum amount of polysiloxane on the nonwoven sheet to provide lubrication during tufting. Emulsions were formed from different amounts of polymethylhydrogensiloxane (DC1107) and polyoxypropylene glycol (Pluracol" P- l 010) described above, the latter having a viscosity of about 155 centipoise at 25C. These were sprayed in an amount of about 2 percent by weight onto a 3.5 oz./yd. bonded nonwoven sheet from segmentally drawn continuous polypropylene filaments, in which the filaments were preferentially aligned in the machine and cross-machine direction, the sheet being prepared by the process described in Troth U.S. Pat. No. 3,477,103. The samples were tufted and the tear strength measured in the manner described above.
TABLE I Finish Composition Polyoxy- Polymethyl- Tufted propylene Polymethylhydrogensiloxane Tongue Glycol hydrogensiloxane on sheet Tear by weight by weight by weight lb. 0 100 2 56 5O 5O 1 55 10 0.2 55 93 7 0.14 57 95 5 0.1 61 96 4 0.08 54 97 3 0.06 53 98 2 0.04 51 99 1 0.02 51 100 0 0 45 Results listed in Table 1 indicate that the tear strength remains high over most of the concentration range, but falls off when the amount of polysiloxane on the sheet drops below about 0.06 percent by weight. For comparative purposes, tufting of a similar nonwoven sheet having no finish applied thereon gave a tufted tongue tear of about 15 lbs.
EXAMPLE II A 3.0 oz./yd. nonwoven sheet, produced from continuous polypropylene filaments in the manner generally described in Example I was lubricated with various amounts of an emulsion formed from 95 percent by weight of the polyoxypropylene glycol (Pluracol" P-10l0) and 5 percent by weight of polymethylhydrogensiloxane (DC-1107). Samples of these lubricated sheets were tufted and the tufted tongue tear measured. The results, summarized in Table II, again indicate that the tufted tongue tear starts to decrease sharply when the amount of polysiloxane on the sheet drops below about 0.06 percent.
TABLE II Polymethylhydrogensiloxane Finish Composition on sheet Tufted Tongue by weight on sheet by weight Tear lbs. 0 17 0.52 0.026 38 1.1 0.055 42 2.0 0.1 48 3.03 0.152 48 4.03 0.202 48 EXAMPLE III The lubricating effect of the mixture of polyoxypropylene glycol and a polysiloxane is demonstrated in this example, in which another nonwoven sheet similar to that in Example I and having a basis weight of about 3.5 oz./yd. was coated (a) with 2 percent ofa 95/5 percent by weight emulsion of polyoxypropylene glycol and polymethylhydrogensiloxane, (b) with 1.9 percent of the polyoxypropylene glycol alone, and (c) with 0.1 percent of the siloxane alone [i.e., the amounts respectively of polyoxypropylene glycol and polymethylhydrogensiloxane in items (b) and (c) being the same as those present in combination in item (a)]. The results shown in Table II indicate that the tufted tongue tear of sample a is significantly higher than that of either sample b or sample 0.
TABLE III Finish Tufted Tongue Sample by weight Tear lbs. a 2% Emulsion 53 b 1.9% Polyoxypropylene Glycol 44 c 0.1% Polymethylhydrogensiloxane 40 EXAMPLE IV This example demonstrates the improved continuous dyeing performance of the primary carpet backing of this invention, compared with one containing a prior art lubricant.
Long yardages of continuous filament nonwoven backing of the type described in Example I were lubricated respectively with 100 percent polymethylhydrogensiloxane, with a 50/50 mixture of polymethylhydrogensiloxane and polyoxypropylene glycol, and a 5/95 percent mixture of the siloxane and polyoxypropylene glycol. After tufting, samples were lagged for various periods of time before being subjected to a typical continuous dyeing operation as earlier described. Formulations of the prepad and dye solutions used in this dyeing operation are listed in Table IV.
TABLE IV Dye Bath Formulation: (Pickup 400 percent) DuPonol FAB (Foaming Agent E. I. du Pont de Nemours & Co., Inc.): 4 g/l Polygum 260 (Thickener Polymer Industries Incorporated 6 g/l Monosodium Phosphate (PI-I buffer): 2 g/l Color Index Direct Yellow 44 3 g/l Color Index Acid Red 337 0.28 g/l Color Index Acid Blue 40 0.95 g/l Prepad Bath (Pickup 100 percent) Merpol WF (Wetting Agent E. I. du Pont de Nemours & Co., Inc.): 5 g/] DuPonol FAB (Foaming Agent E. I. du Pont de Nemours & Co., Inc.) 2 g/l All the samples were dyed under essentially the same conditions using a steaming time of about 8 minutes at 100C. After drying, the dyed samples were subjectively evaluated for appearance, dye uniformity, lack of frostiness, etc., the criterion for acceptability being that the product should be free of dyeing defects when dyed at least three weeks and preferably four weeks after tufting.
TABLE V Tuft Finish Finish on MI'IP" on to dye Dye Type Sheet wt% Sheet lag time Quality 100% M111 1 l 3 days Unacceptable 50/50 PPG"/ MHP" l 0.5 3 weeks Acceptable 50/50 PPG*"/ MP1? 2 l 3 weeks Unacceptable /5 PPG""/ MHP" 1 0.05 4 weeks Acceptable 95/5 PPG"/ MHP' 2 0.1 4 weeks Acceptable Polymethylhydrogensiloxane Polyoxypropylene glycol The results in Table V shows that unacceptable dye quality is obtained with 1 percent by weight of polymethylhydrogensiloxane on the sheet, either alone or in combination with the polyoxypropylene glycol.
EXAMPLE V Additional tests were carried out using a 3 or/yd. nonwoven polypropylene primary carpet backing to which was applied various amounts of an emulsion containing 95 percent polyoxypropylene glycol and 5 percent polymethylhydrogensiloxane previously described. After tufting, the continuous dyeing performance of the various samples was tested every week, for a number of weeks, to determine how many weeks each sample could be lagged and still obtain acceptable dyeing performance.
Formulations of the baths used in the dyeing operation are listed in Table VI and the dye-quality results are given in Table VI]. These results indicate that acceptable performance is obtained with up to 0.72 percent of polysiloxane on the sheet and that the lag time for acceptable performance increases as the amount of polysiloxane on the sheet decreases.
TABLE VI Dye Bath Formulation (Pickup-400 percent) Duponol FAB (Foaming Agent E. I. du Pont de Nemours & Co., Inc.): 3.0 g/l Polygum 260 (Thickener Polymer Industries, Inc.)
5.0 g/l Monosodium Phosphate (PH Buffer) 2.0 g/l Color Index Acid Yellow 174 3 g/l Color Index Acid Blue 40 0.73 g/l Color Index Acid Red 337 0.7 g/l Prepad Bath (Pickup percent) Merpol WF (Wetting Agent E. I. du Pont de Nemours & Co., Inc.) 1 3 g/l Polygum 260 (Thickener Polymer Industries, Inc.)
TABLE VII Polysiloxane Acceptable D e Finish Pickup on Sheet Quality with uftby weight by Weight to-dye lags up to: 14.4 0.72 3 weeks 4 weeks 9 weeks 12 weeks EXAMPLES VI TO VIII These examples demonstrate the lubricating effect obtained with other mixtures of polysiloxanes and polyoxypropylene compounds. Nonwoven sheets having a basis weight of 4 oz./yd. produced in the manner generally described in Example I were lubricated (a) with an amount of an emulsion of a polysiloxane and a polyoxypropylene compound, (b) with the polyoxypropylene compound alone and (c) with the polysiloxane alone, the respective amounts of the components in items (b) and (c) being about the same as those present in combination in item (a). The actual materials used and the amount of finish by weight are listed in Table VIII which also gives the results of the tufted tongue tear measurements. In each case, it is seen that the tear strength is significantly higher in samples lubricated with the two component emulsion than with either component separately.
The carpet of Example VIa was allowed to stand for three weeks and was then subjected to a continuous dyeing operation as described in previous examples. Dyeing was uniform and acceptable. The carpets of Examples VIla and Villa were pleasant to walk upon, being free from the scroopiness exhibited by carpets of Examples VIIc and Y I IIc TABLE VlIL-Tear Tests for Various Emulsions Vll...... 3.0 77
EXAMPLE [X A nonwoven sheet of the type generally described in the preceding examples was lubricated using a gravure coater with varying amounts of the emulsion of Example VII so as to vary the quantity of dimethyl polysiloxane on the sheet from about 0.03 to about 0.1 1 percent by weight. A sharp drop in tufted tongue tear was observed when the amount of polysiloxane on the sheet dropped below about 0.06 percent by weight.
What is claimed is:
l. A bonded nonwoven synthetic organic fiber sheet to which has been applied a lubricating composition consisting essentially of 3-50 percent by weight of a liquid polysiloxane selected from the group of polymethyl hydrogen siloxane and polydimethyl siloxane and 50-97 percent by weight of a liquid polyoxypropylene compound having a viscosity of at least 100 centipoises at 25C. and selected from the group of polyoxypropylene glycol and the monobutyl ether thereof, said composition being present in an amount such that the quantity of polysiloxane on the sheet is in the range of about 0.06 and 0.8 percent by weight.
2. The sheet of claim I wherein the synthetic organic fibers are continuous polypropylene filaments.
3. The sheet of claim 2 wherein the polysiloxane is polymethylhydrogensiloxane.
4. The sheet of claim 3 wherein the lubricating composition comprises 5-20 percent by weight of polysiloxane and 80-95 percent by weight of polyoxypropylene compound.
str teg
Claims (3)
- 2. The sheet of claim 1 wherein the synthetic organic fibers are continuous pOlypropylene filaments.
- 3. The sheet of claim 2 wherein the polysiloxane is polymethylhydrogensiloxane.
- 4. The sheet of claim 3 wherein the lubricating composition comprises 5-20 percent by weight of polysiloxane and 80-95 percent by weight of polyoxypropylene compound.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US12535571A | 1971-03-17 | 1971-03-17 |
Publications (1)
Publication Number | Publication Date |
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US3772069A true US3772069A (en) | 1973-11-13 |
Family
ID=22419357
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00125355A Expired - Lifetime US3772069A (en) | 1971-03-17 | 1971-03-17 | Bonded nonwoven sheet bearing a lubricating composition of a liquid polysiloxane and a liquid polyoxypropylene compound |
Country Status (6)
Country | Link |
---|---|
US (1) | US3772069A (en) |
BE (1) | BE780773A (en) |
CA (1) | CA972911A (en) |
DE (1) | DE2213074A1 (en) |
GB (1) | GB1360524A (en) |
NL (1) | NL7203627A (en) |
Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3867188A (en) * | 1973-07-25 | 1975-02-18 | Dow Corning | Spunbonded nonwoven fabric |
US3968042A (en) * | 1974-09-13 | 1976-07-06 | Phillips Petroleum Company | Finishing agent and nonscroopy polyolefin fibers |
US4919828A (en) * | 1987-10-30 | 1990-04-24 | Henkel Corporation | Fiber lubricants containing high molecular weight polyacrylamido alkane sulfonic acid additives |
US5755984A (en) * | 1996-08-27 | 1998-05-26 | Takemoto Yushi Kabushiki Kaisha | Agents for and methods of lubricating synthetic yarns for heat treatmant process |
US5772910A (en) * | 1996-08-28 | 1998-06-30 | Takemoto Yushi Kabushiki Kaisha | Method of providing lubricity to synthetic yarns to be processed for false twisting with short heater |
KR100438147B1 (en) * | 1996-08-27 | 2004-08-09 | 다케모토 유시 가부시키 가이샤 | Synthetic fiber filaments for heat treatment process Lubricants for sanding and synthetic fiber filaments for heat treatment |
KR100438148B1 (en) * | 1996-08-28 | 2004-08-12 | 다케모토 유시 가부시키 가이샤 | Lubrication Method of Synthetic Fiber Filament Yarn for Shot Heater Processing |
US9618474B2 (en) | 2014-12-18 | 2017-04-11 | Edico Genome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US9857328B2 (en) | 2014-12-18 | 2018-01-02 | Agilome, Inc. | Chemically-sensitive field effect transistors, systems and methods for manufacturing and using the same |
US9859394B2 (en) | 2014-12-18 | 2018-01-02 | Agilome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US10006910B2 (en) | 2014-12-18 | 2018-06-26 | Agilome, Inc. | Chemically-sensitive field effect transistors, systems, and methods for manufacturing and using the same |
US10020300B2 (en) | 2014-12-18 | 2018-07-10 | Agilome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US10429342B2 (en) | 2014-12-18 | 2019-10-01 | Edico Genome Corporation | Chemically-sensitive field effect transistor |
US10811539B2 (en) | 2016-05-16 | 2020-10-20 | Nanomedical Diagnostics, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
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- 1971-03-17 US US00125355A patent/US3772069A/en not_active Expired - Lifetime
-
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- 1972-03-08 CA CA136,728A patent/CA972911A/en not_active Expired
- 1972-03-16 BE BE780773A patent/BE780773A/en unknown
- 1972-03-17 GB GB1265472A patent/GB1360524A/en not_active Expired
- 1972-03-17 DE DE19722213074 patent/DE2213074A1/en active Pending
- 1972-03-22 NL NL7203627A patent/NL7203627A/xx unknown
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US2757094A (en) * | 1953-08-07 | 1956-07-31 | Guss Charles | Liquid cleaner and polisher and method of compounding the same |
US2955047A (en) * | 1957-05-22 | 1960-10-04 | Bon Ami Company | Cleaning compositions |
GB828735A (en) * | 1957-06-03 | 1960-02-24 | Ici Ltd | Lubrication of hydropholic filaments |
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Cited By (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3867188A (en) * | 1973-07-25 | 1975-02-18 | Dow Corning | Spunbonded nonwoven fabric |
US3968042A (en) * | 1974-09-13 | 1976-07-06 | Phillips Petroleum Company | Finishing agent and nonscroopy polyolefin fibers |
US4919828A (en) * | 1987-10-30 | 1990-04-24 | Henkel Corporation | Fiber lubricants containing high molecular weight polyacrylamido alkane sulfonic acid additives |
US5755984A (en) * | 1996-08-27 | 1998-05-26 | Takemoto Yushi Kabushiki Kaisha | Agents for and methods of lubricating synthetic yarns for heat treatmant process |
KR100438147B1 (en) * | 1996-08-27 | 2004-08-09 | 다케모토 유시 가부시키 가이샤 | Synthetic fiber filaments for heat treatment process Lubricants for sanding and synthetic fiber filaments for heat treatment |
US5772910A (en) * | 1996-08-28 | 1998-06-30 | Takemoto Yushi Kabushiki Kaisha | Method of providing lubricity to synthetic yarns to be processed for false twisting with short heater |
KR100438148B1 (en) * | 1996-08-28 | 2004-08-12 | 다케모토 유시 가부시키 가이샤 | Lubrication Method of Synthetic Fiber Filament Yarn for Shot Heater Processing |
US9857328B2 (en) | 2014-12-18 | 2018-01-02 | Agilome, Inc. | Chemically-sensitive field effect transistors, systems and methods for manufacturing and using the same |
US9618474B2 (en) | 2014-12-18 | 2017-04-11 | Edico Genome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US9859394B2 (en) | 2014-12-18 | 2018-01-02 | Agilome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US10006910B2 (en) | 2014-12-18 | 2018-06-26 | Agilome, Inc. | Chemically-sensitive field effect transistors, systems, and methods for manufacturing and using the same |
US10020300B2 (en) | 2014-12-18 | 2018-07-10 | Agilome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US10429342B2 (en) | 2014-12-18 | 2019-10-01 | Edico Genome Corporation | Chemically-sensitive field effect transistor |
US10429381B2 (en) | 2014-12-18 | 2019-10-01 | Agilome, Inc. | Chemically-sensitive field effect transistors, systems, and methods for manufacturing and using the same |
US10494670B2 (en) | 2014-12-18 | 2019-12-03 | Agilome, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US10607989B2 (en) | 2014-12-18 | 2020-03-31 | Nanomedical Diagnostics, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
US10811539B2 (en) | 2016-05-16 | 2020-10-20 | Nanomedical Diagnostics, Inc. | Graphene FET devices, systems, and methods of using the same for sequencing nucleic acids |
Also Published As
Publication number | Publication date |
---|---|
CA972911A (en) | 1975-08-19 |
DE2213074A1 (en) | 1972-09-21 |
GB1360524A (en) | 1974-07-17 |
BE780773A (en) | 1972-07-17 |
NL7203627A (en) | 1972-09-19 |
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