US3575751A - Method of making semiartificial pile fabrics - Google Patents
Method of making semiartificial pile fabrics Download PDFInfo
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- US3575751A US3575751A US3575751DA US3575751A US 3575751 A US3575751 A US 3575751A US 3575751D A US3575751D A US 3575751DA US 3575751 A US3575751 A US 3575751A
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- Prior art keywords
- fibers
- pile
- fabric
- skins
- animal
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H11/00—Non-woven pile fabrics
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H11/00—Non-woven pile fabrics
- D04H11/04—Non-woven pile fabrics formed by zig-zag folding of a fleece or layer of staple fibres, filaments, or yarns, strengthened or consolidated at the folds
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- 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
- Y10T428/23907—Pile or nap type surface or component
- Y10T428/2395—Nap type surface
Definitions
- This invention relates to methods for making fabrics and to the novel fabrics produced thereby.
- the invention relates to methods for making fabrics utilizing woolled or furred animal skins and to the making of pile fabrics.
- Woolled or furred animal skins are superior in many ways to conventional man-made pile fabrics.
- the pile fibers of an animal skin are firmly anchored in the animals hide, and there is substantially no shedding of fibers during use or in cleaning as is the case with almost all artificial pile fabrics.
- the fibers in an animals hide are naturally uniformly distributed throughout the hide in a manner difficult to achieve in synthetic pile fabrics, especially those having longer pile heights.
- Wool has the best resiliency of any fiber known, and woolled or furred animal skins have a soft luxurious feel and appearance. There is, however, a certain amount of wastage in converting animal skins into garment parts and other end use items which tends to increase the cost of the natural material as compared with synthetic fiber pile fabrics and other artificial materials.
- woolled animal skins typified by woolled sheep and amb skins
- haired or furred animal skins in general, such as the haired skins or hides or goats, llamas, vicunas, alpacas, and the like, and to the furred skins of mink, muskrat, rabbit, chinchilla, bear, and the like.
- woolled is intended to be inclusive of the terms haired and furred.
- certain of the methods of the present invention are applicable to synthetic pile fabrics.
- FIG. 1 is a semi-schematic top view of woolled animal skins laid out so as to form a continuous pile fabric
- FIGS. 24 are schematic views showing the adhering of a fabric as shown in FIG. 1 to a second base material.
- Much of the cost of finished sheep and lamb skins is due to processing, i.e., defieshing the hide, scouring the fur, tanning the hide, dyeing the fur, straightening the fur, and shearing the pile, and to wastage during shearing and more particularly when trimming the unevenly shaped skins.
- the average total size, not all of which is useable, of a lamb skin is 6 square feet; that of a sheep is 8 square feet.
- the present invention reduces the cost of processing by avoiding batch operation and by minimizing wastage due to the cutting of uneven skins into end use products.
- the first step in preparing a composite natural pile fabric according to the process of the present invention is to adhere or attach the defleshed woolled hides to a carrier material which may be a porous plastic film, a perforated foil or a woven or non-woven textile fabric pervious to the pickling, tanning and other chemical solutions used in subsequent treatment of the skins.
- a carrier material which may be a porous plastic film, a perforated foil or a woven or non-woven textile fabric pervious to the pickling, tanning and other chemical solutions used in subsequent treatment of the skins.
- a relatively inexpensive stiffened resin coated cotton scrim, woven jute fabric or a pervious plastic film is preferred.
- the carrier should be at least about 60 inches wide by about 20 to 50 yards long or in other convenient dimensions to accommodate 2 to 4 full width skins when laid side by side and a large number of full lengths of skins laid end to end on the carrier.
- the resultant composite natural pile fabric should be of such dimensions that will permit it to be processed using conventional
- the adhesive may be either water or organic solvent solutions or dispersions of resins, rubbers, copolymers and the like.
- the polymeric or elastomeric adhesive can be either natural or synthetic, thermoplastic or thermosetting, or mixtures of these. It is preferable to employ a relatively inexpensive adhesive which does not require a heat treatment to fix it on the material but which will withstand subsequent wet processing of the composite natural pile fabric.
- the adhesive is either knife coated or sprayed onto one side of the carrier material or brush coated on sprayed onto the back or hide side of the animal skins.
- One possible advantage of applying the adhesive to the hide of the woolled skins is that, in certain cases, the hide may not then have to be tanned to prevent it from shrinking in subsequent hot treatments.
- a pressure-sensitive adhesive should be used on the carrier material when it is desired that the carrier be peeled off the hide component at a later stage.
- one of the simplest and easiest ways of forming a composite natural pile fabric for processing, and to permit the chemical treating solutions to pass freely through the carrier is to attach the woolled skins to a woven stainless-steel wire belt by means of toggles or clamps in much the same way the sheep shearlings are now stretched and attached to individual metal screen racks for drying, except that the wool skins should be fitted close together to permit a semi-artificial pile fabric to be made from the composite natural pile fabric.
- the animal skins are removed from the metal screen conveyor belt and used in the normal way.
- the woolled skins 1 are placed on the carrier fabric 3 having thereon a layer of adhesive 2 with the wool pile pointing up.
- the skins are positioned in such a way that the irregular edges of the skins approximate or bed in with each other so as not to leave any significant space between individual skins.
- the pile at the edges of the skins extends over the edges of the hide to close any gap between individual skins. This gives the impression of, and actually achieves, an uninterrupted pile fabric surface appearance.
- the resultant composite natural pile fabric is finished utilizing conventional methods and apparatus.
- the fabric is first scoured to remove wool grease from the pile fibers and from the skin by running it continuously through bowls of luke warm aqueous solutions of detergent and squeeze rolls as though it were woven wool piece goods. Care is taken so as not to felt or excessively entangle the pile fibers.
- the hide portion is tanned by running the composite pile fabric through a chrome or vegetable or glutaraldehyde tanning solution in a dolly washer or other type of textile fabric washer.
- the hide portion of the Wool skins can be tanned by running the composite pile fabric over a conveyor or screen through an aqueous solution of a phenolic compound and an aldehyde such as a solution containing resorcinol and formaldehyde, in such a Way that only the carrier material and the hide portion, and not the wool fiber portion, are immersed in the tanning solution.
- the resorcinol and formaldehyde or like agents chemically combine with the protein structures of the hide and, subsequently, on curing of the treated material, form a durable, insoluble polymer of resorcinol-formaldehyde within the structure of the hide to stabilize the hide against shrinkage and against attack by microorganisms.
- Running the entire composite pile fabric through such a phenol and aldehyde solution also stiffens and prevents felting of the fibers.
- This latter treatment which is particularly useful with fabrics having long length fibers, results in the formation of polymer within the fibers as well as within the hide structure.
- the whole pile fabric is dyed, using conventional Wool or fur dyes in regular wool fabric dyeing machines.
- the wool can be dyed and the skin chrome tanned at the same time.
- the fabric is then dried, with or without prior straightening of the pile fibers by running it continuously through an oven at a low temperature of about 1l0150 F. while passing air at a high velocity through the oven.
- the natural pile fabric is first carded on a machine of the same type as, but wider than, that used to remove entanglements from the pile of individual wooled sheep skins. Then, either a so-called electrifying machine or vibrating comb may be employed to permanently straighten the pile fibers.
- the electrifying machine is designed to operate continuously to remove fiber crimp and to straighten the fibers by the rubbing and heating action of a heated, rotating, slotted metal cylinder which is brought to bear against the pile surface.
- a vibrating comb extending across the width of the pile fabric may be employed to straighten and disentangle the pile fibers.
- the pile fabric moves slowly through and past the comb, which, like the cylinder of the electrifying machine, may be heated to a temperature of about 30O500 F.
- formaldehyde is general y applied to the wool together with an alcohol to assist penetration of the formaldehyde and a strong organic acid, e.g., trichloroacetic acid, as a catalyst.
- Reducing agents and ethanolamines have also been used for imparting a permanent set to pile fabrics during electrification.
- the resultant long length of natural pile fabric preferably about 6070 inches in width and most usually with a dyed and straightened Wool fiber pile in a pile length in the range of from about 2 inches to about 6 inches, may be cut into convenient dimensions for garments and other uses with a minimum wastage of animal skin material.
- the resultant natural pile fabric may be converted into one natural pile fabric and one man-made pile fabric, or otherwise utilized according to the various embodiments of the present invention.
- the method of making a second pile fabric from the finished natural pile fabric or from finished individual animal skins or other sets of skins is accompilshed by first firmly adhering the loose ends of the wool fibers present in the animal skins onto or into a second base material.
- the second base material e.g., a polyurethane foam
- the second base material may be formed in situ onto the free ends of the pre-sheared and straightened wool fibers of the animal skin.
- adhesion gives rise to a fabric wherein one end of the pile fibers remains in the animal hide base and the other end of those fibers is adhered to a second base material.
- This fabric is useful per se; it can, for example, form the basis of wearing apparel insulated against extreme cold by virtue of the air space between the inner and outer layers of base materials. Since the dense wool pile fibers at this stage are firmly held perpendicular between two base materials, the product has extraordinarily good resiliency or springiness, and hence it may be used for bed mattresses, furniture padding, pillows and the like, merely by enclosing the double-based pile fabric with a case or cover. Most often, however, the pile fibers are cut at some point along their lengths between the animal hide ond the second base material to produce two separate pile fabrics, one natural and one semiartificial.
- a Woven, non-woven, or knitted fabric, a plastic film or sheet, an animal hide such as split cowhide or dehaired sheep skins, plastic foam, metal foil, a needled fibrous web or batt, or a paper sheet may be employed as the second base material.
- a rather viscous adhesive such as that used in making flocked fabrics, is spread upon one side of the second base material which is approximately the same length and width as the composite natural pile fabric.
- the adhesive coated base, together with the composite animal skin pile fabric, is then passed through the electrostatic field of an electrostatic flocking machine to cause the loose ends of the pile fibers in the animal skins to embed into the adhesive layer of the second base fabric.
- the animal hides 6 attached or adhered to carrier fabric 5 and bearing Wool fibers 7 are passed by means of conveyor belt 18 between electrodes 11 and 12.
- the second base material -9, having thereon a previously applied coating of adhesive 10, is passed simultaneously in the same direction between these electrodes.
- the animal hides 6 and the sec-nd base material 9 are spaced at a distance approximately equal to the length of the fibers 7.
- the action of the electrostatic field passing between electrodes 11 and 12 causes the fibers to align themselves with the field and adhere to the second base material 10.
- the fibers 7 are then cut by means of knife 14 to give a second pile fabric 13 comprising the second base material having evenly spaced fibers adhered thereto as well as the natural pile fabric 15.
- the knife or wire cutting device is set to give preselected lengths of pile fibers in the natural and semiartificial fabrics.
- the arrangement of the composite animal skin pile fabric and the second base material, as shown in FIG. 2, can be reversed. That is, the composite fabric with the fibers pointing downward can be placed above the second 'base material with the adhesive coating on its upper surface as the two materials pass together through the electrostatic field.
- the intensity of the electrostatic field, the moisture content of the fibers, the conductivity of the adhesive film, and the distance between the positive and negative electrodes must be controlled in order to get satisfactory adhesion of the fibers to the second base layer.
- air suction is employed to draw the free ends of fibers in an animal skin composite fabric into the second base material.
- the free ends of the pile fibers are sucked into and through the open spaces in the second base material, which is an open-weave fabric, a perforated film or foil, or an opencell foam.
- the composite hide structure 6 and attached carrier is passed parallel to a sheet of open-weave second base material 15.
- a suction or vacuum box '17 is located behind the open-Weave base material. Both the composite hide structure 6 and the open weave material 16 move slowly together over vacuum box 17.
- suction causes the fibers 7 to stand erect and at the same time causes their free ends to be sucked through the thickness of the second base material.
- the back of the open-weave material 16 containing the ends of the animal fibers 7 passing therethrough is coated with a rubber or resin emulsion or solution by means of coating box 18.
- the adhesive back-coating is then dried and cured by means of heat lamp 19. This treatment permanently anchors the ends of the fibers into the second base in a manner analogous to that in which knitted or tufted pile fibers are bonded into their bases.
- the fibers 7 are then split by means of knife 14 to give semiartificial pile fabric 13 and sheared natural pile fabric 15.
- both air suction and electrostatic methods can be employed together to orient the pile fibers and cause the ends of these fibers to strike the adhesive on, or pass through, the new base material either perpendicularly or at an angle to the second base material.
- air can be blown over the animal skin to aid either the air suction or electrostatic field in forcing the pile fibers to strike or penetrate the second base fabric in either a perpendicular or randomly blown manner.
- the electrostatic method and vibration of the composite fabric for example, by the beater bar technique, can be used together. In the beater bar technique, a series of bars rotate at several hundred r.p.m. against the hide side of the woolled animal skin. This action, together with electrostatic forces, enhances the perpendicular orientation of the pile fibers and helps them penetrate into the adhesive of the second base fabric.
- a composite pile fabric material according to the present invention having dyed, straightened and sheared pile fibers is placed fiber side up on a moving conveyor belt. Sideboards are placed against the outer edges of the material to keep the fiber ends there in an upright position, i.e., to prevent the fibers at the edges of the pelts from bending over.
- the resultant semiartificial pile fabrics can be given a final brushing or vacuuming to remove any unbonded fibers from the pile.
- a flexible polymeric foam is foamed in place on the free ends of a sheared animal skin, set of animal skins or composite fabric by spraying.
- the foam preferably of the polyurethane type, serves as the base of the synthetic pile fabric.
- foam bases are formed over the ends of the wool fibers by spraying methods involving either a one-component system or a twocomponent system.
- the active urethane foam ingredients are sprayed onto the ends of the fibers in the form of a film or droplets.
- the treated material is then either heated at a controlled predetermined temperature or exposed to a controlled moist atmosphere to activate the system and cause it to foam.
- a fairly viscous organic solvent solution of an isocyanateterminated urethane pre-polymer is sprayed over the ends of the upright fibers until a thin coating is applied.
- the material is then passed through a high humidity chamber which causes the formation of a cellular foam structure over the ends of the fur fibers.
- a solution containing a blocked isocyanate compound, a hydroxyl bearing component (a diol or triol) and a catalyst, e.g., a tertiary amine or a metal salt of a carboxylic acid is sprayed at room temperature over the surface of the animal hide or composite pile fabric at the free ends of the wool fibers.
- a catalyst e.g., a tertiary amine or a metal salt of a carboxylic acid
- the flexible urethane foam base components are sprayed onto the fiber ends by means of a twin feed or double barrel spray gun.
- one spray component is a premix of a polyester and catalyst together with acetone as a diluent
- the second component is a diisocyanate such as tolylene diisocyanate.
- the two components are metered by means of air or motor driven gear pumps and mixed immediately after leaving the gun to form the urethane foam backing on contact with the fiber ends.
- the adhesive solution or emulsion is sprayed from one side of the pile fabric toward the opposite side with the nozzle of the spray gun several feet from the fibers and on a level with the free ends of the pile fibers.
- a fluid adhesive in the form of a fine mist or fog is first sprayed over the ends of the pile fibers to bond the ends of the fibers together in a thin web with droplets of adhesive between the fibers without causing any of the fibers to stick together in the form of tufts; a more viscous film or foam is then sprayed or knife coated over the web.
- the chemical base after the chemical base has been dried and set, and firmly bonded to the ends of the pile fibers, it may be sheared or sliced, or sanded to make it uniform in thickness.
- the ends of the fibers may be dipped into the adhesive or the adhesive may be applied to the ends of the pile fibers by means of a rotating brush or roller.
- An embodiment utilizing this approach which coats the free end of individual fibers in a pile fabric and at the same time mechanically forces these fiber ends into an adhesive layer on a base material is illustrated in FIG. 4.
- a composite animal skin pile fabric comprising a carrier fabric having attached thereto a multiplicity of animal hides 6 with straightened and sheared pile fibers 7 is passed over roller 20. Passage of the pile fabric around small diameter roller 20 so that the material makes about a 90 turn, opens up the pile and the fibers of the pile become separate from each other at the point where the backing material is bent.
- the adhesive from trough 22 is applied to the open ends of the fibers 7 at the apex of the angle bend by means of a roller or brush 21 dipping into trough 22.
- the second base material may have a layer of adhesive applied thereto or may be coated by means of roller or brush 23 dipping into the same trough.
- the pile fabric having its fibers in contact with the second base material passes heat lamp 19 which dries and cures the adhesive to permanently bond the fibers to the second base material.
- Cutting of the fibers at a predetermined length by means of knife 14 produces semiartificial pile fabric 13 and natural pile fabric shorter in pile fiber length than in the original fabric.
- the woolled skins of Merino sheep contain an average pile fiber length greater than about 3 inches. In other breeds, the fiber length may average 6 inches or more. It is apparent that more than one semiartificial pile fabric may be produced from one animal skin or natural pile fabric when the pile fiber of the man-made fabric is to be only 1-2 inches in length and when starting with a pile fiber length of six inches or more in the original animal skins.
- the number of synthetic pile fabrics that can be made is determined by the starting length of the pile in the woolled animal skins, the desired finished fiber lengths in the synthetic pile fabrics, and the average pile fiber length desired in the finished natural pile fabric.
- a typical sheared natural pile fabric having an average length of sheared pile fibers of 1% inches and approximately 33,820 fibers per square inch weighs 168.5 grams per square foot; the wool fibers themselves weigh 110.3 grams per square foot.
- the animal skin employed was a sheep skin having approximately 35,000 pile fibers 1% inches in length per square inch of hide.
- the adhesive employed contained about 95.2 parts of an aqueous acrylic emulsion, 3 parts of Xylene, 0.8 part of a methylcellulose thickening agent (Methocel, 4,000 cps. viscosity), and 1.0 part of a 10% aqueous oxalic acid solution catalyst added just prior to using.
- the second base material was knife coated with the adhesive to a thickness of about A; inch.
- the free fiber ends of the woolled sheep skin were lightly knife coated or brushed with the same adhesive and placed in perpendicular contact with the adhesive coated second base material. After the adhesive had dried, the sample was cured for several minutes at C. to produce a doublebased fabric. After cutting at a point midway between the two bases, the double-based fabric yielded a semiartificial pile fabric having fibers approximately inch in length attached to the second base material.
- the original sheep skin was recovered intact except that its fiber pile was now also approximately inch in length.
- Example 8 the adhesive was applied only to the second base material and not to the free ends of the wool fibers.
- Example 9 the adhesive was applied in a layer inch thick to give a flexible acrylate base; no second base material as such was employed.
- Example 10 a two-component, self-foaming urethane was spread on aluminum foil coated with a releasing agent, and the rapidly foaming mixture was used in place of the second base material.
- the adhesion of the Wool fibers to the second base material was good, and the fiber density of the semiartificial pile fabric was about the same as that of the original woolled sheep skin.
- the processes of the present invention offer numerous possibilities for new and old pile fabric designs and construction to those skilled in the arts of fur finishing, synthetic pile fabric manufacturing and finishing, differential dying, printing, flocking, flock printing, etc.
- pile fiber length for either the natural or semiartificial pile fabrics
- various animal fur simulants such as beaver, mink, otter, seal, zebra, etc.
- coarse straightfibered New Zealand sheep skins can be used to form fabrics with the pile laid down and set almost flat against the base material. When properly dyed this will simulate a South American otter fur.
- a mink or other animal fur simulant which contains both ground fur and guard hairs may be made by starting with a conventional knitted or woven type pile fabric containing a short, dense synthetic fiber pile as the ground or under fur. Dyed guard hairs from a sheep skin are then transposed into this modified base. Blankets or other fleece type fabrics can be produced from synthetic pile fabric merely by tucking the pile fibers into the base fabric by running the pile fabric through a needle punch machine.
- a pile may be formed on one surface of a needle punched or mechanically interlocked non-woven batt of animal or synthetic fibers, or a resilient polyurethane foam, using a sheep skin pile fabric to produce soft, resilient, longor short-pile rugs and carpets or linings for garments.
- Synthetic lamb skins which are practically mirror images of the natural material, can be made from lamb skins in which the wool pile is intentionally allowed to remain in curled or entangled tuft form.
- pile fabrics may be made from sheep skins which have interesting raised fiber patterns on their surfaces, such as diamond shapes, squares, flower designs, and other patterns. This can be done by applying adhesive to the second base fabric in the particular pattern desired, using printing rolls to apply the adhesive. Fibers from the woolled animal skin are then drawn into this adhesive. The pile fibers will, of course, adhere to the base material only where the adhesive has been applied thereby forming the pattern desired.
- the base material may also be dyed or undyed to create color contrasts between the pile fibers and base fabric.
- novel three-dimensional fabrics may be made for use as floor coverings, wall coverings, toys, wearing apparel such as coats, jackets, hats, etc.
- the base material, fabric, film, foam or foil, either dyed or natural color is printed on one side with various objects or forms, a portion of which utilizes animal skin fibers to make the printed objects appear realistic.
- one base material is printed with human body forms, both male and female. Openings in the base material are provided around the top of the heads of the human figures. Fibers from animal skins are drawn through these openings to form the hair on the heads of the printed human figures.
- Similar perforations can appear in the base material at the chins of male figures to produce real fiber beards from the wool pile of sheep skins
- Openings in the base material can also be present at the legs, collars, jackets, etc., of the human forms so that when fibers from animal skins such as sheep skins are drawn through these openings, and the fibers cut and anchored to the base fabric, the human forms will have fur-like clothing and the figures will give a three-dimensional appearance.
- the fiber hair or fur can be dyed or printed in different colors.
- Another base material can contain prints of sheep, dogs, cows, or other furry animals with perforations in the base throughout the animals bodies.
- Fibers from an animal skin are then sucked or drawn through the perforations to the desired height, cut, and attached to the base material to produce fur on the printed animals.
- Other base materials can contain printed scenes of animals grazing in pasture lands wherein green-dyed animal skin fibers will be drawn through the base material around the printed animals to serve as grass, shrubs, or a fence, etc. There is, of course, no limit to the other three-dimensional scenes or designs that may be produced by this general method.
- the fibers from the animal skin After the fibers from the animal skin have been drawn through the openings in the man-made base to the desired height above the printed pattern on the face of the base, the fibers are cut below the back side of the man-made base and well above the animal skin base in order to allow the natural woolled animal skin to be useable for other purposes.
- the cut fibers are then bent over against the back of the man-made base and firmly anchored to this base material by either a preformed adhesive film or by coating the back side of the base with an adhesive.
- these tufts of fibers can be laid down and permanently set nearly flat against the surface of the face of the base material.
- the fibers for the hair and beards can be straight or they can be crimped or curled.
- the pile fibers in animal skins can be utilized to produce artificial leather materials with various types of surface finishes, smooth and glossy, embossed, or suede.
- the best grades of natural leathers made from dehaired hides of calves or cattle have on their finished grain layer surfaces between 6,000 and 19,000 hair follicles per square inch. These tiny holes are visible on the surface of the natural leather with the aid of a microscope and they extend practically all the way through the epidermis or grain layer of the leather to the porous corium or fibrous layer of the animal hide.
- follicles contribute to the excellent water vapor permeability of natural leather, a property highly desired, for example, in material used in shoe uppers.
- the number and arrange ment of follicles in natural leather is also believed to contribute to the desired time creasing or break characteristics of the finished surface of good leathers.
- the properties of good water vapor permeability and genuine leather-like-break are highly desired and avidly sought.
- an artificial leather may be made from a porous, flexible, fibrous textile substrate such as a nonwoven felt or a Woven and felted wool fabric, and a flexible, flex-resistant elastomeric polymer or plastic grain layer such as a polyether or polyester urethane or plasticized polyvinyl chloride.
- the elastomeric or plastic grain layer is applied to the substrate, felt, fabric or needled fiber batt, Weighing between 6 and 18 ounces per square yard and with a thickness of approximately 0.05 to 0.2 inch, in the form of an organic solvent solution which may contain a heat-activated blowing agent or in the form of an emulsion or precipitate.
- the grain layer material should impregnate the substrate at least part way through its thickness and form a smooth coating with a thickness of from about 2 mils to about 25 mils on the surface of the substrate.
- the wool pile fibers present in animal skins such as sheep skins are employed either to form thousands of tiny holes or follicles per square inch in the polymeric grain layer, or to deposit thousands of short wool fibers per square inch in the grain layer perpendicular to the surface of the grain layer and substrate.
- the thousands of wool fibers running perpendicular or at a slight angle practically through the thickness of the grain layer serve to absorb moisture from the substrate and aid in the transporting water vapor through the thickness of the artificial leather.
- the follicles are formed in the grain layer of the artificial leather product as follows: the polymeric grain layer in a fluid state is applied to a surface of the porous fibrous textile substrate. Then the ends of the fibers of the scoured and straightened animal skin or composite are embedded deeply into the grain layer coating by either electrostatic means or by one of the other methods described above. The grain layer coating is then partially dried and/ or partially cured. The animal fibers are pulled out of the grain layer after the grain layer no longer flows but before the polymeric grain layer coating has completely dried or set, leaving between about 7,000 and 56,000 tiny holes or follicles, depending on the breed of animal and grade of wool used, in the grain layer of the artificial leather. For example, sheep hides have the following number of fibers per square inch in their skins:
- the pile fibers In order to form tiny microscopic holes through the thickness of the grain layer, the pile fibers should be embedded virtually all the way through the thickness of the grain layer down to the surface of the substrate.
- One way to accomplish this is to first coat the substrate with a very thin layer of grain layer adhesive and attach the pile fibers to this adhesive layer. After the adhesive has dried, the synthetic substrate and animal skin pile fabric are held up on their sides or ends. A second thicker coating of grain layer is then flowed over the first adhesive layer until from about 2 mils to about 25 mils of the lengths of the pile fibers attached to the substrate are covered with grain layer. After the grain layer has partially dried, the fibers are removed to leave the thousands of tiny microscopic pores running through the grain layer to the substate. After curing or setting is complete, the grain layer surface is sanded or buffed, plated or embossed to produce uniform, leather-like surfaces.
- the fibers can be left in the grain layer as follows: After embedding the ends of the pile from the woolled animal skin or composite pile fabric into the grain layer of the artificial leather material, the grain layer is dried or cured and permanently set. Then the pile fibers are cut off either flush with the grain surface or just above that surface.
- the resultant material with thousands of fiber ends per square inch protruding from its surface, can be finished with conventional leather finishing agents or dressings to produce smooth, glossy surfaces.
- the Wool fibers in the grain layer absorb and transport water vapor through the artificial leather.
- the processes of the present invention which involve adhering woolled, haired or furred animal skins to a second base material, usually followed by one or more cuttings of the animal fibers, and the preparation of artificial porous leather may utilize single animal skins or sets of woolled, haired or furred animal skins of any sort.
- the use of composite natural animal pile fabrics made as described herein is to be preferred.
- a method of making a semiartificial pile fabric comprising the steps:
- a method of making a semiartificial pile fabric comprising the steps:
- a method of making a semiartificial pile fabric comprising the steps:
- a method of making a semiartificial pile fabric comprising the steps:
- a method of making a semiartificial pile fabric comprising the steps:
- the invention defined in claim 10 including also applying the adhesive to the free ends of the woolled animal skin.
- a method of making semiartificial pile fabrics comprising the steps:
- a method of making semiartificial pile fabrics comprising the steps:
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Abstract
PILE FABRICS OR POROUS ARTIFICIAL LEATHER IS MADE UTILIZING WOOLLED OR FURRED ANIMAL SKINS WITHOUT DETACHING THE WOOL OR FUR FROM THE SKINS PRIOR TOATTACHING THE FREE ENDS OF THE WOOL OR FUR TO A SECOND BASE THUS RESULTING IN A THICKER, FULLER MORE NATURAL APPEARING PRODUCT.
Description
2 Sheets-g 1 Apr-i120, 1971 L. MIZELL METHOD OF MAKING S'EMIARTIFICIAL FILE FABRICS Original fiiled Sept. 1; 1966 Aprifi 2% 1W7 L, MlZELL 3,575,75H
METHOD 0F MAKING- SEMIARTIFICIAL FILE FABRICS Original Fi led Sept. 1' 1966 I 2 Sheets-Sheet 2 I NVENTOR 2B LOUIS R. MIZELL ATTORNEYS United States Patent 3,575,751 METHOD OF MAKING SEMIARTIFICIAL PILE FABRICS Louis R. Mizell, Montgomery County, Md., assignor to I.W.S. Nominee Company Limited, London, England Continuation of application Ser. No. 484,240, Sept. 1, 1966. This application Jan. 15, 1969, Ser. No. 796,276 Int. Cl. C14b 1/02, 15/00; 1332b /24 US. Cl. 156-68 18 Claims ABSTRACT OF THE DISCLOSURE Pile fabrics or porous artificial leather is made utilizing woolled or furred animal skins without detaching the wool or fur from the skins prior to attaching the free ends of the wool or fur to a second base thus resulting in a thicker, fuller more natural appearing product.
This application is a continuation of application Ser. No. 484,240, filed Sept. 1, 1966, now abandoned.
This invention relates to methods for making fabrics and to the novel fabrics produced thereby. In its more specific aspects, the invention relates to methods for making fabrics utilizing woolled or furred animal skins and to the making of pile fabrics.
Woolled or furred animal skins are superior in many ways to conventional man-made pile fabrics. The pile fibers of an animal skin are firmly anchored in the animals hide, and there is substantially no shedding of fibers during use or in cleaning as is the case with almost all artificial pile fabrics. The fibers in an animals hide are naturally uniformly distributed throughout the hide in a manner difficult to achieve in synthetic pile fabrics, especially those having longer pile heights. Wool has the best resiliency of any fiber known, and woolled or furred animal skins have a soft luxurious feel and appearance. There is, however, a certain amount of wastage in converting animal skins into garment parts and other end use items which tends to increase the cost of the natural material as compared with synthetic fiber pile fabrics and other artificial materials. I
It is an object of the present invention to provide an improved method for producing finished woolled skins.
It is a further object of the invention to provide a method for processing woolled skins as pile fabrics, rather than as individual furs, thereby minimizing handling and wastage of material.
It is yet another object of the present invention to provide for producing two or more pile fabrics from one woolled animal skin or set of woolled animal skins.
It is still another object of the invention to provide a novel method for making artificial leather materials utilizing woolled animal skins.
I have discovered that certain objectives and advantages of the present invention are obtained when woolled or furred animal skins are put in a form so that they may be processed as pile fabrics in continuous or semi-continuous operations using conventional or' modified textile pile fabric equipment. Moreover, since the animal pile fibers are already ideally distributed on their ends with respect to pile density and fiber spacing, a portion of the length of this natural pile, as well as that of single skins or another set of woolled animal skins, may be adhered to a second base material to make at least one other pile fabric from a single skin or set of woolled or furred animal skins. And, utilizing the fiber spacing present, one or more artificial leather fabrics can be made from a single skin or set of woolled or furred skins leaving the single skin or set intact for further use.
While the following discussion will apply primarily to woolled animal skins typified by woolled sheep and amb skins, it pertains to haired or furred animal skins in general, such as the haired skins or hides or goats, llamas, vicunas, alpacas, and the like, and to the furred skins of mink, muskrat, rabbit, chinchilla, bear, and the like. As used herein the term woolled is intended to be inclusive of the terms haired and furred. And, while it would not ordinarily be economically advantageous, certain of the methods of the present invention are applicable to synthetic pile fabrics.
My invention will be more particularly described in the discussion which follows and by means of the specific embodiments thereof shown in the accompanying drawings wherein:
FIG. 1 is a semi-schematic top view of woolled animal skins laid out so as to form a continuous pile fabric; and
FIGS. 24 are schematic views showing the adhering of a fabric as shown in FIG. 1 to a second base material.
Much of the cost of finished sheep and lamb skins is due to processing, i.e., defieshing the hide, scouring the fur, tanning the hide, dyeing the fur, straightening the fur, and shearing the pile, and to wastage during shearing and more particularly when trimming the unevenly shaped skins. The average total size, not all of which is useable, of a lamb skin is 6 square feet; that of a sheep is 8 square feet. In one specific aspect, the present invention reduces the cost of processing by avoiding batch operation and by minimizing wastage due to the cutting of uneven skins into end use products.
The first step in preparing a composite natural pile fabric according to the process of the present invention is to adhere or attach the defleshed woolled hides to a carrier material which may be a porous plastic film, a perforated foil or a woven or non-woven textile fabric pervious to the pickling, tanning and other chemical solutions used in subsequent treatment of the skins. For economic reasons, a relatively inexpensive stiffened resin coated cotton scrim, woven jute fabric or a pervious plastic film is preferred. The carrier should be at least about 60 inches wide by about 20 to 50 yards long or in other convenient dimensions to accommodate 2 to 4 full width skins when laid side by side and a large number of full lengths of skins laid end to end on the carrier. The resultant composite natural pile fabric should be of such dimensions that will permit it to be processed using conventional pile fabric equipment.
If an adhesive material is used to bond the skins to the carrier material, the adhesive may be either water or organic solvent solutions or dispersions of resins, rubbers, copolymers and the like. The polymeric or elastomeric adhesive can be either natural or synthetic, thermoplastic or thermosetting, or mixtures of these. It is preferable to employ a relatively inexpensive adhesive which does not require a heat treatment to fix it on the material but which will withstand subsequent wet processing of the composite natural pile fabric. The adhesive is either knife coated or sprayed onto one side of the carrier material or brush coated on sprayed onto the back or hide side of the animal skins. One possible advantage of applying the adhesive to the hide of the woolled skins is that, in certain cases, the hide may not then have to be tanned to prevent it from shrinking in subsequent hot treatments. On the other hand, a pressure-sensitive adhesive should be used on the carrier material when it is desired that the carrier be peeled off the hide component at a later stage.
In this latter connection, one of the simplest and easiest ways of forming a composite natural pile fabric for processing, and to permit the chemical treating solutions to pass freely through the carrier, is to attach the woolled skins to a woven stainless-steel wire belt by means of toggles or clamps in much the same way the sheep shearlings are now stretched and attached to individual metal screen racks for drying, except that the wool skins should be fitted close together to permit a semi-artificial pile fabric to be made from the composite natural pile fabric. After the skins are processed on the belt and the semiartificial pile fabric is made, the animal skins are removed from the metal screen conveyor belt and used in the normal way.
In the embodiment illustrated in FIG. 1, the woolled skins 1 are placed on the carrier fabric 3 having thereon a layer of adhesive 2 with the wool pile pointing up. The skins are positioned in such a way that the irregular edges of the skins approximate or bed in with each other so as not to leave any significant space between individual skins. The pile at the edges of the skins extends over the edges of the hide to close any gap between individual skins. This gives the impression of, and actually achieves, an uninterrupted pile fabric surface appearance.
Usually, skins of the same type and origin, i.e., Australian Merino, New Zealand, Romney, South African, Leicester, etc., will be placed on one particular carrier material to achieve the similar normal variation in pile character throughout the whole fabric that exists throughout a single sheep skin of a given type and grade. However, to achieve interesting appearance effects in ultimate pile fabric carpeting, it may be desirable to alternate an Australian sheep skin with a South African skin, for example, on the same carrier material.
The resultant composite natural pile fabric is finished utilizing conventional methods and apparatus. The fabric is first scoured to remove wool grease from the pile fibers and from the skin by running it continuously through bowls of luke warm aqueous solutions of detergent and squeeze rolls as though it were woven wool piece goods. Care is taken so as not to felt or excessively entangle the pile fibers. Next, if necessary for stabilization, the hide portion is tanned by running the composite pile fabric through a chrome or vegetable or glutaraldehyde tanning solution in a dolly washer or other type of textile fabric washer. Alternatively, the hide portion of the Wool skins can be tanned by running the composite pile fabric over a conveyor or screen through an aqueous solution of a phenolic compound and an aldehyde such as a solution containing resorcinol and formaldehyde, in such a Way that only the carrier material and the hide portion, and not the wool fiber portion, are immersed in the tanning solution. The resorcinol and formaldehyde or like agents chemically combine with the protein structures of the hide and, subsequently, on curing of the treated material, form a durable, insoluble polymer of resorcinol-formaldehyde within the structure of the hide to stabilize the hide against shrinkage and against attack by microorganisms. Running the entire composite pile fabric through such a phenol and aldehyde solution also stiffens and prevents felting of the fibers. This latter treatment, which is particularly useful with fabrics having long length fibers, results in the formation of polymer within the fibers as well as within the hide structure.
If the fibers are to be dyed and not left in their natural color, the whole pile fabric is dyed, using conventional Wool or fur dyes in regular wool fabric dyeing machines. In certain types of dyeings, such as premetallized dyeing, the wool can be dyed and the skin chrome tanned at the same time. The fabric is then dried, with or without prior straightening of the pile fibers by running it continuously through an oven at a low temperature of about 1l0150 F. while passing air at a high velocity through the oven. After drying, it may be desirable to soften the tanned skin component by applying a controlled amount of moisture to the skin and then exposing the material to mechanical softening techniques, such as staking or beat- After dyeing, it is usually desirable to straighten and disentangle the fibers in a relatively long-haired pile fabric. To do this, the natural pile fabric is first carded on a machine of the same type as, but wider than, that used to remove entanglements from the pile of individual wooled sheep skins. Then, either a so-called electrifying machine or vibrating comb may be employed to permanently straighten the pile fibers. The electrifying machine is designed to operate continuously to remove fiber crimp and to straighten the fibers by the rubbing and heating action of a heated, rotating, slotted metal cylinder which is brought to bear against the pile surface. Alternatively, a vibrating comb extending across the width of the pile fabric may be employed to straighten and disentangle the pile fibers. The pile fabric moves slowly through and past the comb, which, like the cylinder of the electrifying machine, may be heated to a temperature of about 30O500 F. In straightening the animal fibers, formaldehyde is general y applied to the wool together with an alcohol to assist penetration of the formaldehyde and a strong organic acid, e.g., trichloroacetic acid, as a catalyst. Reducing agents and ethanolamines have also been used for imparting a permanent set to pile fabrics during electrification.
The resultant long length of natural pile fabric, preferably about 6070 inches in width and most usually with a dyed and straightened Wool fiber pile in a pile length in the range of from about 2 inches to about 6 inches, may be cut into convenient dimensions for garments and other uses with a minimum wastage of animal skin material. Or the resultant natural pile fabric may be converted into one natural pile fabric and one man-made pile fabric, or otherwise utilized according to the various embodiments of the present invention.
The method of making a second pile fabric from the finished natural pile fabric or from finished individual animal skins or other sets of skins is accompilshed by first firmly adhering the loose ends of the wool fibers present in the animal skins onto or into a second base material. Alternatively, for many applications and specifially when starting with animal skins having a very dense pile, the second base material, e.g., a polyurethane foam, may be formed in situ onto the free ends of the pre-sheared and straightened wool fibers of the animal skin. Such adhesion gives rise to a fabric wherein one end of the pile fibers remains in the animal hide base and the other end of those fibers is adhered to a second base material. This fabric is useful per se; it can, for example, form the basis of wearing apparel insulated against extreme cold by virtue of the air space between the inner and outer layers of base materials. Since the dense wool pile fibers at this stage are firmly held perpendicular between two base materials, the product has extraordinarily good resiliency or springiness, and hence it may be used for bed mattresses, furniture padding, pillows and the like, merely by enclosing the double-based pile fabric with a case or cover. Most often, however, the pile fibers are cut at some point along their lengths between the animal hide ond the second base material to produce two separate pile fabrics, one natural and one semiartificial.
In making the second or semiartificial pile fabric, a Woven, non-woven, or knitted fabric, a plastic film or sheet, an animal hide such as split cowhide or dehaired sheep skins, plastic foam, metal foil, a needled fibrous web or batt, or a paper sheet, may be employed as the second base material. In the specific embodiment illustrated in FIG. 2, a rather viscous adhesive, such as that used in making flocked fabrics, is spread upon one side of the second base material which is approximately the same length and width as the composite natural pile fabric. The adhesive coated base, together with the composite animal skin pile fabric, is then passed through the electrostatic field of an electrostatic flocking machine to cause the loose ends of the pile fibers in the animal skins to embed into the adhesive layer of the second base fabric.
As shown in FIG. 2, the animal hides 6 attached or adhered to carrier fabric 5 and bearing Wool fibers 7 are passed by means of conveyor belt 18 between electrodes 11 and 12. The second base material -9, having thereon a previously applied coating of adhesive 10, is passed simultaneously in the same direction between these electrodes. The animal hides 6 and the sec-nd base material 9 are spaced at a distance approximately equal to the length of the fibers 7. The action of the electrostatic field passing between electrodes 11 and 12 causes the fibers to align themselves with the field and adhere to the second base material 10. The fibers 7 are then cut by means of knife 14 to give a second pile fabric 13 comprising the second base material having evenly spaced fibers adhered thereto as well as the natural pile fabric 15. The knife or wire cutting device is set to give preselected lengths of pile fibers in the natural and semiartificial fabrics.
The arrangement of the composite animal skin pile fabric and the second base material, as shown in FIG. 2, can be reversed. That is, the composite fabric with the fibers pointing downward can be placed above the second 'base material with the adhesive coating on its upper surface as the two materials pass together through the electrostatic field. The intensity of the electrostatic field, the moisture content of the fibers, the conductivity of the adhesive film, and the distance between the positive and negative electrodes must be controlled in order to get satisfactory adhesion of the fibers to the second base layer.
In the specific embodiment illustrated in FIG. 3, air suction is employed to draw the free ends of fibers in an animal skin composite fabric into the second base material. The free ends of the pile fibers are sucked into and through the open spaces in the second base material, which is an open-weave fabric, a perforated film or foil, or an opencell foam. As shown in FIG. 3, the composite hide structure 6 and attached carrier is passed parallel to a sheet of open-weave second base material 15. A suction or vacuum box '17 is located behind the open-Weave base material. Both the composite hide structure 6 and the open weave material 16 move slowly together over vacuum box 17. As they do so, suction causes the fibers 7 to stand erect and at the same time causes their free ends to be sucked through the thickness of the second base material. The back of the open-weave material 16 containing the ends of the animal fibers 7 passing therethrough is coated with a rubber or resin emulsion or solution by means of coating box 18. The adhesive back-coating is then dried and cured by means of heat lamp 19. This treatment permanently anchors the ends of the fibers into the second base in a manner analogous to that in which knitted or tufted pile fibers are bonded into their bases. The fibers 7 are then split by means of knife 14 to give semiartificial pile fabric 13 and sheared natural pile fabric 15.
A number of variations or modifications of these embodiments is possible. For example, both air suction and electrostatic methods can be employed together to orient the pile fibers and cause the ends of these fibers to strike the adhesive on, or pass through, the new base material either perpendicularly or at an angle to the second base material. Further, air can be blown over the animal skin to aid either the air suction or electrostatic field in forcing the pile fibers to strike or penetrate the second base fabric in either a perpendicular or randomly blown manner. In addition, the electrostatic method and vibration of the composite fabric, for example, by the beater bar technique, can be used together. In the beater bar technique, a series of bars rotate at several hundred r.p.m. against the hide side of the woolled animal skin. This action, together with electrostatic forces, enhances the perpendicular orientation of the pile fibers and helps them penetrate into the adhesive of the second base fabric.
Other methods may be employed to attach the free ends of the pile fibers in woolled animal Skins to a base material. For example, a composite pile fabric material according to the present invention having dyed, straightened and sheared pile fibers, is placed fiber side up on a moving conveyor belt. Sideboards are placed against the outer edges of the material to keep the fiber ends there in an upright position, i.e., to prevent the fibers at the edges of the pelts from bending over. A viscous pasty adhesive that will not run down the length of the fibers into the hide backing, such as a thickened acrylic latex, is then knife coated over the surface at the free fiber ends of the sheared pile. A separate base material of approximately the same length and with as the composite animal skin pile fabric, which may also be coated with a thin layer of adhesive, is laid firmly onto the adhesive coated ends of the pile of the composite pile fabric. After the adhesive has dried, the pile fibers are cut or severed by means of a rotating or oscillating knife or with an electrically heated wire to give pile fibers of uniform predetermined length in both base materials. The resultant semiartificial pile fabrics can be given a final brushing or vacuuming to remove any unbonded fibers from the pile.
In another embodiment, a flexible polymeric foam is foamed in place on the free ends of a sheared animal skin, set of animal skins or composite fabric by spraying. The foam, preferably of the polyurethane type, serves as the base of the synthetic pile fabric. Such foam bases are formed over the ends of the wool fibers by spraying methods involving either a one-component system or a twocomponent system.
In one-component systems, the active urethane foam ingredients are sprayed onto the ends of the fibers in the form of a film or droplets. The treated material is then either heated at a controlled predetermined temperature or exposed to a controlled moist atmosphere to activate the system and cause it to foam. For example, a fairly viscous organic solvent solution of an isocyanateterminated urethane pre-polymer is sprayed over the ends of the upright fibers until a thin coating is applied. The material is then passed through a high humidity chamber which causes the formation of a cellular foam structure over the ends of the fur fibers. Or a solution containing a blocked isocyanate compound, a hydroxyl bearing component (a diol or triol) and a catalyst, e.g., a tertiary amine or a metal salt of a carboxylic acid is sprayed at room temperature over the surface of the animal hide or composite pile fabric at the free ends of the wool fibers. The treated material is then heated to cause the adhesive to foam into a resilient flexible base for the semiartificial pile fabric.
Using a two-component system, the flexible urethane foam base components are sprayed onto the fiber ends by means of a twin feed or double barrel spray gun. For example, one spray component is a premix of a polyester and catalyst together with acetone as a diluent, and the second component is a diisocyanate such as tolylene diisocyanate. The two components are metered by means of air or motor driven gear pumps and mixed immediately after leaving the gun to form the urethane foam backing on contact with the fiber ends. Other chemical formulations that can be sprayed or coated directly onto the fiber or wool surface include solutions containing plasticized polyvinyl chloride with or without a blowing agent, and various emulsified elastomers containing conventional foaming or blowing agents. The application of heat causes the coating to foam when a foaming or blowing agent is present.
In the above embodiments involving the spraying of solutions to form a film or foam over level fiber ends, care should be taken not to blow the fibers around or to disrupt the wool pile, except in a controlled way, until after the free ends of the fibers have been firmly bonded to the adhesive layerfVarious approaches are known by means of which an adhesive or foam can be sprayed onto the fiber end surface of a pile fabric without disrupting the spatial arrangement of the pile fibers. In one approach, a rather viscous solution is sprayed under low air pressure while moving the pile fabric by the spray system so that all of the fibers across the width of the fabric and directly under the spray move slightly in the same direction. Or the adhesive solution or emulsion is sprayed from one side of the pile fabric toward the opposite side with the nozzle of the spray gun several feet from the fibers and on a level with the free ends of the pile fibers. Or a fluid adhesive in the form of a fine mist or fog is first sprayed over the ends of the pile fibers to bond the ends of the fibers together in a thin web with droplets of adhesive between the fibers without causing any of the fibers to stick together in the form of tufts; a more viscous film or foam is then sprayed or knife coated over the web. In general, after the chemical base has been dried and set, and firmly bonded to the ends of the pile fibers, it may be sheared or sliced, or sanded to make it uniform in thickness.
Using another approach, the ends of the fibers may be dipped into the adhesive or the adhesive may be applied to the ends of the pile fibers by means of a rotating brush or roller. An embodiment utilizing this approach which coats the free end of individual fibers in a pile fabric and at the same time mechanically forces these fiber ends into an adhesive layer on a base material is illustrated in FIG. 4. A composite animal skin pile fabric comprising a carrier fabric having attached thereto a multiplicity of animal hides 6 with straightened and sheared pile fibers 7 is passed over roller 20. Passage of the pile fabric around small diameter roller 20 so that the material makes about a 90 turn, opens up the pile and the fibers of the pile become separate from each other at the point where the backing material is bent. The adhesive from trough 22 is applied to the open ends of the fibers 7 at the apex of the angle bend by means of a roller or brush 21 dipping into trough 22. The second base material may have a layer of adhesive applied thereto or may be coated by means of roller or brush 23 dipping into the same trough. As the composite pile fabric passes around roller 20 and resumes a straight path, the fibers 7 assume their original spacing. This results in the adhesive-coated fibers being flipped onto the second base material. The pile fabric having its fibers in contact with the second base material passes heat lamp 19 which dries and cures the adhesive to permanently bond the fibers to the second base material. Cutting of the fibers at a predetermined length by means of knife 14 produces semiartificial pile fabric 13 and natural pile fabric shorter in pile fiber length than in the original fabric.
The woolled skins of Merino sheep, for example, contain an average pile fiber length greater than about 3 inches. In other breeds, the fiber length may average 6 inches or more. It is apparent that more than one semiartificial pile fabric may be produced from one animal skin or natural pile fabric when the pile fiber of the man-made fabric is to be only 1-2 inches in length and when starting with a pile fiber length of six inches or more in the original animal skins. The number of synthetic pile fabrics that can be made is determined by the starting length of the pile in the woolled animal skins, the desired finished fiber lengths in the synthetic pile fabrics, and the average pile fiber length desired in the finished natural pile fabric. A typical sheared natural pile fabric having an average length of sheared pile fibers of 1% inches and approximately 33,820 fibers per square inch weighs 168.5 grams per square foot; the wool fibers themselves weigh 110.3 grams per square foot.
The following examples further illustrate the preparation of double-based fabrics and semiartificial pile fabrics according to the present invention The animal skin employed was a sheep skin having approximately 35,000 pile fibers 1% inches in length per square inch of hide. The adhesive employed contained about 95.2 parts of an aqueous acrylic emulsion, 3 parts of Xylene, 0.8 part of a methylcellulose thickening agent (Methocel, 4,000 cps. viscosity), and 1.0 part of a 10% aqueous oxalic acid solution catalyst added just prior to using.
The second base material was knife coated with the adhesive to a thickness of about A; inch. The free fiber ends of the woolled sheep skin were lightly knife coated or brushed with the same adhesive and placed in perpendicular contact with the adhesive coated second base material. After the adhesive had dried, the sample was cured for several minutes at C. to produce a doublebased fabric. After cutting at a point midway between the two bases, the double-based fabric yielded a semiartificial pile fabric having fibers approximately inch in length attached to the second base material. The original sheep skin was recovered intact except that its fiber pile was now also approximately inch in length.
The above method was employed using the following second base materials:
Curing Example time No. Second base material (min.)
1 Dehaired sheep skin 4.0 2. Woven nylon fabric l. 5 3 Open cell urethane foam" l. 5 4 Knitted jersey fabric 1.5 5 Woven nylon taffeta- 1. 5 6 Knitted jersey fabric 1. 5 7. Woven w0ol1'abric 1.5 8 Non-woven wool felt 1. 5 9. Acrylate 1. 5 10 Polyurethane foam... 4.0
In Example 8, the adhesive was applied only to the second base material and not to the free ends of the wool fibers. In Example 9, the adhesive was applied in a layer inch thick to give a flexible acrylate base; no second base material as such was employed. In Example 10, a two-component, self-foaming urethane was spread on aluminum foil coated with a releasing agent, and the rapidly foaming mixture was used in place of the second base material. In each of the examples described, the adhesion of the Wool fibers to the second base material was good, and the fiber density of the semiartificial pile fabric was about the same as that of the original woolled sheep skin.
The processes of the present invention offer numerous possibilities for new and old pile fabric designs and construction to those skilled in the arts of fur finishing, synthetic pile fabric manufacturing and finishing, differential dying, printing, flocking, flock printing, etc. For example, by proper selection of pile fiber length for either the natural or semiartificial pile fabrics, by setting the pile at the proper angle to the base material, and by appropriate known dyeing or printing techniques, various animal fur simulants, such as beaver, mink, otter, seal, zebra, etc., can be made. For instance, coarse straightfibered New Zealand sheep skins can be used to form fabrics with the pile laid down and set almost flat against the base material. When properly dyed this will simulate a South American otter fur. A mink or other animal fur simulant which contains both ground fur and guard hairs may be made by starting with a conventional knitted or woven type pile fabric containing a short, dense synthetic fiber pile as the ground or under fur. Dyed guard hairs from a sheep skin are then transposed into this modified base. Blankets or other fleece type fabrics can be produced from synthetic pile fabric merely by tucking the pile fibers into the base fabric by running the pile fabric through a needle punch machine.
Also, a pile may be formed on one surface of a needle punched or mechanically interlocked non-woven batt of animal or synthetic fibers, or a resilient polyurethane foam, using a sheep skin pile fabric to produce soft, resilient, longor short-pile rugs and carpets or linings for garments.
Synthetic lamb skins, which are practically mirror images of the natural material, can be made from lamb skins in which the wool pile is intentionally allowed to remain in curled or entangled tuft form. By employing techniques known in the art of flock printing, pile fabrics may be made from sheep skins which have interesting raised fiber patterns on their surfaces, such as diamond shapes, squares, flower designs, and other patterns. This can be done by applying adhesive to the second base fabric in the particular pattern desired, using printing rolls to apply the adhesive. Fibers from the woolled animal skin are then drawn into this adhesive. The pile fibers will, of course, adhere to the base material only where the adhesive has been applied thereby forming the pattern desired. The base material may also be dyed or undyed to create color contrasts between the pile fibers and base fabric.
In addition to the many fur simulants and other types of conventional pile fabrics that can be made by the processes described, novel three-dimensional fabrics may be made for use as floor coverings, wall coverings, toys, wearing apparel such as coats, jackets, hats, etc, The base material, fabric, film, foam or foil, either dyed or natural color, is printed on one side with various objects or forms, a portion of which utilizes animal skin fibers to make the printed objects appear realistic. For example, one base material is printed with human body forms, both male and female. Openings in the base material are provided around the top of the heads of the human figures. Fibers from animal skins are drawn through these openings to form the hair on the heads of the printed human figures. Similar perforations can appear in the base material at the chins of male figures to produce real fiber beards from the wool pile of sheep skins Openings in the base material can also be present at the legs, collars, jackets, etc., of the human forms so that when fibers from animal skins such as sheep skins are drawn through these openings, and the fibers cut and anchored to the base fabric, the human forms will have fur-like clothing and the figures will give a three-dimensional appearance. The fiber hair or fur can be dyed or printed in different colors. Another base material can contain prints of sheep, dogs, cows, or other furry animals with perforations in the base throughout the animals bodies. Fibers from an animal skin are then sucked or drawn through the perforations to the desired height, cut, and attached to the base material to produce fur on the printed animals. Other base materials can contain printed scenes of animals grazing in pasture lands wherein green-dyed animal skin fibers will be drawn through the base material around the printed animals to serve as grass, shrubs, or a fence, etc. There is, of course, no limit to the other three-dimensional scenes or designs that may be produced by this general method.
After the fibers from the animal skin have been drawn through the openings in the man-made base to the desired height above the printed pattern on the face of the base, the fibers are cut below the back side of the man-made base and well above the animal skin base in order to allow the natural woolled animal skin to be useable for other purposes. The cut fibers are then bent over against the back of the man-made base and firmly anchored to this base material by either a preformed adhesive film or by coating the back side of the base with an adhesive.
On the printed human forms where tufts of fibers serve as the hair or heard, these tufts of fibers can be laid down and permanently set nearly flat against the surface of the face of the base material. Also, the fibers for the hair and beards can be straight or they can be crimped or curled. These novel three-dimensional fabrics composed of printed objects with appropriately interspersed pile fibers may be used as made for purposes previously noted, or the patterns or forms produced in the fabric may be cut or stamped out and then sewn or glued to wearing apparel, bcd clothing, drapes, etc., for decorative purposes.
In addition to making one or more serniartificial pile fabrics from animal skins by the processes and procedures described above, the pile fibers in animal skins can be utilized to produce artificial leather materials with various types of surface finishes, smooth and glossy, embossed, or suede. The best grades of natural leathers made from dehaired hides of calves or cattle have on their finished grain layer surfaces between 6,000 and 19,000 hair follicles per square inch. These tiny holes are visible on the surface of the natural leather with the aid of a microscope and they extend practically all the way through the epidermis or grain layer of the leather to the porous corium or fibrous layer of the animal hide. These follicles contribute to the excellent water vapor permeability of natural leather, a property highly desired, for example, in material used in shoe uppers. The number and arrange ment of follicles in natural leather is also believed to contribute to the desired time creasing or break characteristics of the finished surface of good leathers. In the development and production of substitute or artificial leathers for making shoe uppers, the properties of good water vapor permeability and genuine leather-like-break are highly desired and avidly sought.
Utilizing woolled animal skins or sets and preferably the animal skin pile fabrics of the present invention, an artificial leather may be made from a porous, flexible, fibrous textile substrate such as a nonwoven felt or a Woven and felted wool fabric, and a flexible, flex-resistant elastomeric polymer or plastic grain layer such as a polyether or polyester urethane or plasticized polyvinyl chloride. The elastomeric or plastic grain layer is applied to the substrate, felt, fabric or needled fiber batt, Weighing between 6 and 18 ounces per square yard and with a thickness of approximately 0.05 to 0.2 inch, in the form of an organic solvent solution which may contain a heat-activated blowing agent or in the form of an emulsion or precipitate. The grain layer material should impregnate the substrate at least part way through its thickness and form a smooth coating with a thickness of from about 2 mils to about 25 mils on the surface of the substrate. The wool pile fibers present in animal skins such as sheep skins are employed either to form thousands of tiny holes or follicles per square inch in the polymeric grain layer, or to deposit thousands of short wool fibers per square inch in the grain layer perpendicular to the surface of the grain layer and substrate. The thousands of wool fibers running perpendicular or at a slight angle practically through the thickness of the grain layer serve to absorb moisture from the substrate and aid in the transporting water vapor through the thickness of the artificial leather.
The follicles are formed in the grain layer of the artificial leather product as follows: the polymeric grain layer in a fluid state is applied to a surface of the porous fibrous textile substrate. Then the ends of the fibers of the scoured and straightened animal skin or composite are embedded deeply into the grain layer coating by either electrostatic means or by one of the other methods described above. The grain layer coating is then partially dried and/ or partially cured. The animal fibers are pulled out of the grain layer after the grain layer no longer flows but before the polymeric grain layer coating has completely dried or set, leaving between about 7,000 and 56,000 tiny holes or follicles, depending on the breed of animal and grade of wool used, in the grain layer of the artificial leather. For example, sheep hides have the following number of fibers per square inch in their skins:
Number of fibers per Sheep breed: square inch of skin Merino (fine wool) 37,00056,000 Merino (medium wool) 36,000-52,000 Corriedale L 15,00019,000 Southdown 18,000 Suflolk 13,000 Border Leicester 10,000 Lincoln 9,000 Wiltshire 7,000
In order to form tiny microscopic holes through the thickness of the grain layer, the pile fibers should be embedded virtually all the way through the thickness of the grain layer down to the surface of the substrate. One way to accomplish this is to first coat the substrate with a very thin layer of grain layer adhesive and attach the pile fibers to this adhesive layer. After the adhesive has dried, the synthetic substrate and animal skin pile fabric are held up on their sides or ends. A second thicker coating of grain layer is then flowed over the first adhesive layer until from about 2 mils to about 25 mils of the lengths of the pile fibers attached to the substrate are covered with grain layer. After the grain layer has partially dried, the fibers are removed to leave the thousands of tiny microscopic pores running through the grain layer to the substate. After curing or setting is complete, the grain layer surface is sanded or buffed, plated or embossed to produce uniform, leather-like surfaces.
Instead of forming microscopic holes through the grain layer, the fibers can be left in the grain layer as follows: After embedding the ends of the pile from the woolled animal skin or composite pile fabric into the grain layer of the artificial leather material, the grain layer is dried or cured and permanently set. Then the pile fibers are cut off either flush with the grain surface or just above that surface. The resultant material, with thousands of fiber ends per square inch protruding from its surface, can be finished with conventional leather finishing agents or dressings to produce smooth, glossy surfaces. The Wool fibers in the grain layer absorb and transport water vapor through the artificial leather.
The processes of the present invention which involve adhering woolled, haired or furred animal skins to a second base material, usually followed by one or more cuttings of the animal fibers, and the preparation of artificial porous leather may utilize single animal skins or sets of woolled, haired or furred animal skins of any sort. For reasons of economy and ease in handling, the use of composite natural animal pile fabrics made as described herein is to be preferred.
I claim:
1. A method of making semiartificial prising the steps of:
(a) attaching a multiplicity of woolled animal skins to a carrier in such a manner that their edges approximate and form an uninterrupted fiber pile;
(b) applying an adhesive to at least a second base material;
(c) straightening and aligning the wool fibers of the woolled animal skins by passing the carrier and the skins through an electrostatic field established generally normally to the skins of the carrier;
((1) causing the free ends of the wool fibers and the second base material to come into contact with the adhesive; and thereafter (e) severing the fibers between the animal skin and the second base material.
2. The invention defined in claim 1, wherein the adhesive is applied in the form of a pattern or design.
3. The invention defined in claim 1 wherein the adhesive is applied to both the second base material and the free ends of the fibers.
4. The invention defined in claim 1 wherein a curable polymer composition is sprayed onto the free ends of the fibers of woolled animal skins and then curing the ploymer composition.
5. A method of making a semiartificial pile fabric comprising the steps:
(a) straightening and aligning the undetached fibers of a woolled animal skin by placing the skin with the undetached fibers about a small diameter roller so that the skin makes about a 90 turn, opens up the undetached fibers and the fibers become separated from each other;
(b) providing a second base material;
(c) applying an adhesive to the free ends of the fibers of the woolled animal skin;
(d) causing the free rectified ends of the fibers of the animal skin and the second base material to come pile fabrics com- 12 into contact and become adhesively joined; and thereafter (e) severing the fibers between the animal skin and the base materials.
6. A method of making a semiartificial pile fabric comprising the steps:
(a) providing a second base material;
(b) applying an adhesive to the second base material;
(c) drawing the free ends of the undetached fibers of the animal skin through open spaces in an openweave base material by applying suction to the opposite face of the base material; thereby to cause the free rectified ends of the fibers of the animal skin and the second base material to come into contact and become adhesively joined; and thereafter (d) severing the fibers between the animal skin and the base materials.
7. A method of making a semiartificial pile fabric comprising the steps:
(a) straightening and aligning the undetached fibers of a woolled animal skin by placing the woolled animal skin with the undetached fibers through an electrostatic field established generally normal to the plane of the skin;
(b) providing a second base material;
(c) applying an adhesive to the second base material;
((1) causing the free rectified ends of the fibers of the animal skin and the second base material to come into contact and become adhesively joined; and thereafter (e) severing the fibers between the animal skin and the base materials.
8. The invention defined in claim 7 including also applying the adhesive to the free ends of the fibers of the woolled animal skin.
9. A method of making a semiartificial pile fabric comprising the steps:
.(a) straightening and aligning the undetached fibers of a woolled animal skin by placing the woolled animal skin with the undetached fibers through an electrostatic field established generally normal to the plane of the skin;
(b) providing a second base material;
(c) applying an adhesive to the free ends of the fibers of the woolled animal skin;
(d) causing the free recitified ends of the fibers of the animal skin and the second base material to come into contact and become adhesively joined; and thereafter (e) severing the fibers between the animal skin and the base materials.
10. A method of making a semiartificial pile fabric comprising the steps:
(a) straightening and aligning the undetached fibers of a woolled animal skin by placing the skin with the undetached fibers about a small diameter roller so that the skin makes about a turn, opens up the undetached fibers and the fibers become separated from each other;
(b) providing a second base material;
(c) applying an adhesive to the second base material;
(d) causing the free rectified ends of the fibers of the animal skin and the second base material to come into contact and become adhesively joined; and thereafter (e) severing the fibers between the animal skin and the base materials.
11. The invention defined in claim 10 including also applying the adhesive to the free ends of the woolled animal skin.
12. A method of making semiartificial pile fabrics comprising the steps:
(a) attaching a multiplicity of woolled animal skins to a carrier in such a manner that their edges approximate and form an uninterrupted fiber pile;
(b) drawing the free ends of the wool fibers into and through the open spaces in an open-weave second base material by applying suction to the underside of the second base material;
((2) applying an adhesive to the free ends of the wool fibers; and thereafter (d) severing the fibers between the animal skin and the second base material.
13. The invention defined in claim 12 wherein the adhesive is applied in the form of a pattern or design.
14. The invention defined in claim 12 wherein a curable polymer composition is sprayed onto the free ends of the fibers of woolled animal skins and then curing the polymer composition.
15. A method of making semiartificial pile fabrics comprising the steps:
(a) attaching a multiplicity of wooled animal skins to a carrier in such a manner that their edges approximate and form an uninterrupted fiber pile;
(b) applying an adhesive to at least a second base material;
(c) straightening and aligning the wool fibers of the woolled animal skins by passing the carrier and the skins about a small diameter roller so that the material makes about a 90' turn, opens up the pile and the fibers of the pile become separated from each other;
(d) causing the free ends of the wool fibers and the second base material to come into contact with the adhesive; and thereafter (e) severing the fibers between the animal skins and the second base material. 16. The invention defined in claim 15 wherein the adhesive is applied in the form of a pattern or design.
17. The invention defined in claim 15 wherein the ad hesive is applied to both the second base material and the free ends of the fibers.
18. The invention defined in claim 15 wherein a curable polymer composition is sprayed onto the free ends of the fibers of woolled animal skins and then curing the polymer composition.
References Cited UNITED STATES PATENTS BENJAMIN R. PADGETT, Primary Examiner R. S. GAITHER, Assistant Examiner US. Cl. X.R.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US48424065A | 1965-09-01 | 1965-09-01 | |
US79627669A | 1969-01-15 | 1969-01-15 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3575751A true US3575751A (en) | 1971-04-20 |
Family
ID=27047922
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US3575751D Expired - Lifetime US3575751A (en) | 1965-09-01 | 1969-01-15 | Method of making semiartificial pile fabrics |
Country Status (8)
Country | Link |
---|---|
US (1) | US3575751A (en) |
BE (1) | BE686204A (en) |
CH (1) | CH482049A (en) |
DE (1) | DE1560865C3 (en) |
DK (1) | DK134163B (en) |
GB (1) | GB1160723A (en) |
NL (1) | NL152613B (en) |
SE (1) | SE342256B (en) |
Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3772108A (en) * | 1970-12-21 | 1973-11-13 | I Lezhen | Method of producing fur products and a device for carrying out the method |
US3816204A (en) * | 1970-03-16 | 1974-06-11 | Mitsubishi Petrochemical Co | Process for preparing mats having cushion |
US4120713A (en) * | 1976-06-21 | 1978-10-17 | A/S Weston Taeppefabrik | Process and apparatus for the continuous production of a fibrous web-like pile product |
US4147575A (en) * | 1973-02-12 | 1979-04-03 | Walter Hurtes | Manufacture of nonwoven pile articles |
US20090271914A1 (en) * | 2008-05-02 | 2009-11-05 | Ntt New Textile Technologies Gmbh | Flocked elastomeric coated garments |
US20100173119A1 (en) * | 2008-05-02 | 2010-07-08 | New Textile Technologies Gmbh | Narrow fabric with elastomeric coating and flock |
US20110020590A1 (en) * | 2008-03-24 | 2011-01-27 | Kuraray Co., Ltd. | Split leather product and manufacturing method therefor |
US20110083246A1 (en) * | 2009-10-14 | 2011-04-14 | Ranil Kirthi Vitarana | Garment with Elastomeric Coating |
WO2012046073A1 (en) * | 2010-10-07 | 2012-04-12 | Julia Elaine Macintyre-Cathles | Fabric |
EP2831321A4 (en) * | 2012-03-30 | 2016-05-25 | Deckers Outdoor Corp | Natural wool pile fabric and method for making wool pile fabric |
US9596897B2 (en) | 2013-01-28 | 2017-03-21 | Nike, Inc. | Flocked waistband |
US10801139B2 (en) | 2017-01-27 | 2020-10-13 | Deckers Outdoor Corporation | Sheared wool fleece and method for making sheared wool fleece utilizing yarn knitting |
CN113151616A (en) * | 2020-03-25 | 2021-07-23 | 施远国 | Box-type leather fabric processing thickness control device |
US20210352969A1 (en) * | 2018-09-07 | 2021-11-18 | Fortiac Corporation Dba Téchin New York | Soft Fabric Garment Having Stiff Fabric Structural Elements |
US11713524B2 (en) | 2017-01-27 | 2023-08-01 | Deckers Outdoor Corporation | Sheared wool fleece and method for making sheared wool fleece utilizing yarn knitting |
-
1966
- 1966-08-22 GB GB3744966A patent/GB1160723A/en not_active Expired
- 1966-08-29 DE DE1560865A patent/DE1560865C3/en not_active Expired
- 1966-08-29 SE SE1159866A patent/SE342256B/xx unknown
- 1966-08-31 DK DK446766A patent/DK134163B/en unknown
- 1966-08-31 BE BE686204D patent/BE686204A/xx unknown
- 1966-08-31 NL NL6612282A patent/NL152613B/en unknown
- 1966-09-01 CH CH1275566A patent/CH482049A/en not_active IP Right Cessation
-
1969
- 1969-01-15 US US3575751D patent/US3575751A/en not_active Expired - Lifetime
Cited By (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3816204A (en) * | 1970-03-16 | 1974-06-11 | Mitsubishi Petrochemical Co | Process for preparing mats having cushion |
US3772108A (en) * | 1970-12-21 | 1973-11-13 | I Lezhen | Method of producing fur products and a device for carrying out the method |
US4147575A (en) * | 1973-02-12 | 1979-04-03 | Walter Hurtes | Manufacture of nonwoven pile articles |
US4120713A (en) * | 1976-06-21 | 1978-10-17 | A/S Weston Taeppefabrik | Process and apparatus for the continuous production of a fibrous web-like pile product |
US20110020590A1 (en) * | 2008-03-24 | 2011-01-27 | Kuraray Co., Ltd. | Split leather product and manufacturing method therefor |
US20090271914A1 (en) * | 2008-05-02 | 2009-11-05 | Ntt New Textile Technologies Gmbh | Flocked elastomeric coated garments |
US20100173119A1 (en) * | 2008-05-02 | 2010-07-08 | New Textile Technologies Gmbh | Narrow fabric with elastomeric coating and flock |
US20110083246A1 (en) * | 2009-10-14 | 2011-04-14 | Ranil Kirthi Vitarana | Garment with Elastomeric Coating |
WO2012046073A1 (en) * | 2010-10-07 | 2012-04-12 | Julia Elaine Macintyre-Cathles | Fabric |
EP2831321A4 (en) * | 2012-03-30 | 2016-05-25 | Deckers Outdoor Corp | Natural wool pile fabric and method for making wool pile fabric |
US10287720B2 (en) | 2012-03-30 | 2019-05-14 | Deckers Outdoor Corporation | Natural wool pile fabric and method for making wool pile fabric |
US9596897B2 (en) | 2013-01-28 | 2017-03-21 | Nike, Inc. | Flocked waistband |
US10080395B2 (en) | 2013-01-28 | 2018-09-25 | Nike, Inc. | Flocked waistband |
US10801139B2 (en) | 2017-01-27 | 2020-10-13 | Deckers Outdoor Corporation | Sheared wool fleece and method for making sheared wool fleece utilizing yarn knitting |
US11713524B2 (en) | 2017-01-27 | 2023-08-01 | Deckers Outdoor Corporation | Sheared wool fleece and method for making sheared wool fleece utilizing yarn knitting |
US20210352969A1 (en) * | 2018-09-07 | 2021-11-18 | Fortiac Corporation Dba Téchin New York | Soft Fabric Garment Having Stiff Fabric Structural Elements |
CN113151616A (en) * | 2020-03-25 | 2021-07-23 | 施远国 | Box-type leather fabric processing thickness control device |
CN113151616B (en) * | 2020-03-25 | 2022-10-28 | 施远国 | Box-type leather fabric processing thickness control device |
Also Published As
Publication number | Publication date |
---|---|
NL152613B (en) | 1977-03-15 |
CH482049A (en) | 1969-11-30 |
DK134163B (en) | 1976-09-20 |
SE342256B (en) | 1972-01-31 |
DE1560865B2 (en) | 1975-05-28 |
BE686204A (en) | 1967-02-01 |
GB1160723A (en) | 1969-08-06 |
DK134163C (en) | 1977-02-21 |
NL6612282A (en) | 1967-03-02 |
DE1560865A1 (en) | 1970-12-17 |
DE1560865C3 (en) | 1976-01-08 |
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