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Publication numberUS3149906 A
Publication typeGrant
Publication dateSep 22, 1964
Filing dateMar 11, 1963
Priority dateMar 11, 1963
Publication numberUS 3149906 A, US 3149906A, US-A-3149906, US3149906 A, US3149906A
InventorsThorsen Walter J
Original AssigneeThorsen Walter J
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Process for treating animal fibers with ozone
US 3149906 A
Abstract  available in
Previous page
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Claims  available in
Description  (OCR text may contain errors)

United States Patent 3,149,906 PREECEflS FGR TREATING ANIMAL FEBERS 'VETH QZQNE Waiter .l. Thorsen, El Cerrlto, Calif., assignor to the United States of America as represented by the Secretary of Agriculture N0 Drawing. Filed Mar. 11, 1963, Ser. No. 255,588 3 Qlairns. (Ci. 8-l2fi) (Granted under Title 35, US. Code (1952), sec. 265) A non-exclusive, irrevocable, royalty-free license in the invention herein described, throughout the world for all purposes of the United States Government, with the power to grant sublicenses for such purposes, is hereby granted to the Government of the United States of America.

wool, mohair, and the like, with ozone in order to improve their properties. Further objects of the invention will be evident from the following descrip tion wherein parts and percentages are by weight unless otherwise specified.

As a general proposition, the treatment of wool with ozone has been described heretofore and has been suggested as a means of improving the shrinkage properties of the textile and increasing its affinity for dyes. Various investigators have explored the situation and have advocated different techniques for accomplishing their desired ends. A typical procedure is that described in British Patent No. 242,027, November 5, 1925. In this process, wool is soaked in 5% ammonia solution for a few minutes, hydro-extracted (centrifuged) to remove excess liquid, then placed while damp in a chamber wherein it is exposed to air containing ozone in a concentration of about 1 part per 1000. The process is exceedingly slow as evidenced by the fact that the patentees suggest removing samples of the wool at intervals of a few hours to test them for acidity. (if acid, the wool is again soaked in ammonia solution prior to further ozone treatment.) The procedure of the British patent, termed the Zair process, was further investigated by Brown (Journal of the Society of Dyers and Colourists, vol. 44, pp. 230233, 1928), who illustrates the long duration of the procedure, i.e. 5 to 20 hours, and suggests that ties is attained when 15 hours. In addition to requiring long processing times, the various prior procedures have involved such disadvantages as erratic and non-uniform results, decrease in abrasion resistance of the treated wool, and even loss of material during processing by dissolving of a portion of the fibers. As a net result the ozone treatment of wool has not met with commercial acceptance.

The process of the invention surmounts the difliculties above and leads to the following particular advantages:

A primary item is that the process of the invention requires a brief period of time, that is, usually about 3 to 6 minutes and at most about 10 minutes. Despite this short processing time, the treated fibers display many improvements in their properties, namely:

The resistance of the fibers to felting and shrinking is markedly improved.

The treated fibers are treated) fibers.

The treated fibers take up dyes more rapidly than the untreated fibers. In addition, the fastness of the dyes to the ozone-treated wool is unchanged and fading resistance is equal to or better than with the dyed untreated wool.

whiter than the original (un- The treated product displays increased fiber forces; that is, the indivdual fibers cling more tenaciously than is the case with the untreated material. in turn provides these benefits: Yarns can be spun to a higher count, that is, to finer diameter or fewer fibers per cr ss-section. Yarns can be fabricated with less twist than from the untreated fibers, yet without any loss in yarn tensile strength. (Yarns with less twist are especially desirable for faricating garments as the products have improved wrinkle recovery). Finer yarns can be spun from the treated fibers and with greater efllciency, e.g., with fewer breaks.

In addition to these advantages noted above, the treatment accordance with the invention does not produce any degradative ellect so that there is no detriment in what may be termed the purely mechanical properties of the material. Thus, there is no loss in tensile strength or abrasion resistance. In addition, the material retains its original hand so that it is suitable for fabrication of garments of all kinds such as suits, skirts, shirts, etc.

in essence, the process of the invention involves contactiru the fibrous material with a current of steam and ozone. Various conventional types of textile-treating de- VlCES can be adapted for achieving the desired contact between the material and the steam-ozone mixture. Typically, for batch operations one may provide a chamber supplied with perforated shelves, a gas inlet, exhaust vent, and a discharge outlet for condensed water. The fibrous material to be treated is laid on these shelves and a stream of the steam-ozone mixture is directed into the chamber, preferably in such a manner that it actually passes through the material, or, more accurately, through the interstices between individual fibrous elements. For continuous treatment of long lengths of material such as yarns, slivers, top, cloth, etc., the material can be threaded over a series of perforated rollers supplied, through hollow shafts, with the steam-ozone mixture which then flows through the material as it passes over each roller.

Generally, the ozone is produced in a conventional device wherein oxygen is passed through an electrical system involving a high-voltage silent discharge. The eflluent gas from this device contains, for example, about from 10 to 100 mg. of ozone per liter, depending on the circuit adjustments of the device. (The portion of this gas stream which is not ozone is, of course, oxygen.) This gas stream is mixed with a stream of steam produced by a conventional steam generator. The relative proportions of steam and ozone are so adjusted that the steam-ozone mixture has an ozone concentration of about 10 to 50 mg. per liter. The temperature at which the process of the invention is carried out may be varied from about 60 to C. Temperature control of the treatment is most readily achieved by adjustment of the temperature of the steam-ozone stream. This in turn is readily controlled by adjustment of the proportions of steam and ozone which are combined. For example, by increasing the proportion of steam in relation to the proportion of ozone coming from the ozone generator, the temperature of the steam-ozone composite stream may be increased.

The time of contact between the fibrous material and the steam-ozone mixture may be varied depending on such conditions as the reaction temperature, the concentration of ozone in the steam-ozone mixture, the type of fibrous material being treated, and the degree of modification of the fibrous material which is desired. example, an increase in reaction temperature or an incohesive to one another crease in ozone concentration will increase the speed of modification, In any particular case, pilot trials may be conducted with the material to be treated, employing various conditions and testing the properties of the product. From such tests the appropriate conditions may be easily derived. In such trials, the shrinkage characteristics of the product may, for example, be used as the criterion and the conditions of reaction selected so that the area shrinkage of the product (tested by a standard method) is markedly improved, i.e. reduced to at least one-half, preferably at least one-tenth, of that displayed by the starting (untreated) material. it is, of course, obvious that the process should not be continued for such a long period as to cause degradation of the fibers. As noted above, the process of the invention is rapid so that effective results are obtained in a matter of minutes, for example 2 to 6 minutes, and in no case is the time of reaction more than 1.0 minutes.

Following the treatment with the steam-ozone mixture, the treated material may be acidified, for example, by dipping it into a bath of dilute hydrochloric or sulphuric acid. Typically, this step is accomplished by immersing the material in 0.1 N HCl for 1 to 3 minutes. This acidification acts to restore softness of hand to the treated material and to restore its original resistance to abrasion. The acidification procedure is, however, optional and need not be applied if subsequent dyeing is planned as the acid or salt used in the dyebath accomplishes the same purpose.

The process of the invention is applicable to animal fibrous materials such as wool and mohair and these materials may be in any of various physical forms, e.g. bulk fibers, slivers, roving, top, yarns, felts, woven textiles, knitted textiles, or even garments or garment parts.

The invention is further demonstrated by the following illustrative examples:

Example 1 Steam at 100 C. was mixed with a stream of ozone gas (50 mg. ozone per liter) issuing from an ozone generator. In the different runs the proportions of the two initial streams (steam and ozone) were varied to provide difierent ozone concentrations in the composite stream.

In each run, steam-ozone mixture was introduced at a fiow rate of about 0.1 cu. ft./rnin. into a chamber wherein it was forced through a sample of wool cloth. In each case the time of treatment was 3 minutes.

Following the treatment, the treated wool samples were tested for shrinkage by the following test:

Standard shrinkage test.--The tests for shrinkage referred to below were conducted in the following way: The wool samples were milled at 1700 rpm. for 2 minutes at 40-42 C. in an Accelerotor with 0.5% sodium oleate solution, using a liquor-to-wool ratio of 50 to 1. After this washing operation the samples were measured to etermine their area and the shrinkage was calculated from the original area. With this washing method, samples of control (untreated) wool gave an area shrinkage of 42%. The Accelerotor is described in the American Dyestuff Reporter, vol. 45, p. 685, Sept. 10, 1956.

' 4 The results obtained are summarized below:

Ozone con- Ternpercentration Area Run ature of in steamshrinktreatment, ozone mixage,*

C. ture, percent mgJliter Shrinkage of untreated wool was 42%.

Example 11 A sample of mohair top was treated as described above in Example I, run 4, Le. temperature C., time 3 minutes, ozone concentration 31.4 rug/liter. (The expression top is used in the trade to designate the fiber product which has been produced by scouring the raw fleece, applying carding, combing and doubling to produce a thick strand, about 1 /2 in diameter, of fibers in more or less parallel arrangement, i.e. with no twist. Top is thus the refined material which is eventually treated by roving and spinning to make yarns.)

In order to test the cohesive forces between the individual fibers in the treated top, the material was placed in a test instrument where it was clamped between jaws spaced 8 apart and subjected to elongation While measuring the tensile force. Because of the wide spacing of the jaws, the results do not relate to tensile strength of individual fibers but rather to the degree to which the fibers hold to another by cohesive forces. It was found that the treated top broke at 6.5 lbs. whereas untreated top broke at 1.5 lbs.

Having thus described the invention, what is claimed is:

1. A process for improving the properties of animal fibers selected from the group consisting of wool and mohair, in particular to improve their shrinkage resistance, enhance their rate of dye absorption, and increase the cohesive forces between individual fibers which comprises mixing a stream of steam with a stream of ozone to provide a composite steam-ozone stream having 'a temperature about from 60 to C. and an ozone concentration about from 10 to 50 mg./liter, blowing said composite stream through a mass of animal fibers for a period in the range about from 1 to 10 minutes, sufficient to attain said improvements but insufficient to cause degradation of the fibers.

2. The process of claim 1 wherein the animal fibers are wool.

3. The process of claim 1 wherein the animal fibers are mohair.

References Cited in the file of this patent UNITED STATES PATENTS 1,628,484 Wilkinson May 10, 1927 1,825,178 Coghill Sept. 29, 1931 3,086,534 De Gorter et al Apr. 23, 1963 FOREIGN PATENTS 593,933 Sept. 2, 1925 France

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
US1628484 *Sep 10, 1925May 10, 1927Zair Syndicate LtdDyeing of animal fibers and fabrics of alpha protein nature
US1825178 *Dec 26, 1929Sep 29, 1931Coghill Robert DouglasProcess for the treatment of fibers or fibrous materials
US3086534 *Dec 20, 1956Apr 23, 1963Antoine DalkMethod of bleaching hair with a bleaching agent and ozonized steam
FR593933A * Title not available
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US3391986 *Apr 6, 1967Jul 9, 1968Agriculture UsaProcess for shrinkproofing animal fibers
US4189303 *May 10, 1978Feb 19, 1980The United States Of America As Represented By The Secretary Of AgricultureMethod of shrinkproofing animal fibers with ozone
US4214330 *Feb 23, 1979Jul 29, 1980The United States Of America As Represented By The Secretary Of AgricultureMethod for treatment of fibers with ozone-steam mixtures
US4300367 *Dec 24, 1980Nov 17, 1981The United States Of America As Represented By The Secretary Of The Department Of AgricultureApparatus for treatment of fibers with ozone-steam mixtures
US4410397 *Dec 24, 1980Oct 18, 1983International Paper CompanyDelignification and bleaching process and solution for lignocellulosic pulp with peroxide in the presence of metal additives
US4631836 *Jul 30, 1985Dec 30, 1986Iwata Co. Ltd.Method of activating down and fiber materials
US6113854 *Aug 1, 1995Sep 5, 2000Milum; CraigMethod and apparatus for treatment of infectious medical waste
US6346218Aug 8, 2000Feb 12, 2002Craig MilumPliable container for treatment of infectious medical waste
US6964182 *Mar 24, 2003Nov 15, 2005Kurabo Industries Ltd.Treatment apparatus for chemical modification of animal fibers of continuous web form
US20030182977 *Mar 24, 2003Oct 2, 2003Tadashi KarakawaTreatment apparatus for chemical modification of animal fibers of continuous web form
U.S. Classification8/128.1, 8/149.3, 68/13.00R, 8/127.5, 422/27, 8/111
International ClassificationD06M11/34, D06M11/00
Cooperative ClassificationD06M11/34
European ClassificationD06M11/34