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    • 专利摘要:
    Surface discoloration process of natural and synthetic tissues, especially denim type, by means of ultraviolet radiation and an ecological oxidant. This patent proposes the application of uv-c ultraviolet radiation and an oxidant composed of an organic inorganic salt, such as peroxymonosulfate in order to produce in textiles, whether natural or synthetic fibers (both fabrics and ready-made garments), appreciable advantages over the treatments that are applied at present to obtain a superficial discoloration (or wear) on the tissues, total or located in the desired areas. In the case of non-dyed fabrics this process can be used to effect a pre-treatment before dyeing and finishing. Such application is more efficient, with lower cost (less energy consumption) and with respect for the environment, all of this, improved with respect to current methods. Preferably in denim fabrics (for various ready-made garments) it is necessary to obtain methods to achieve these various effects of decolouration by fashion requirements, without the dangerousness of the treatments currently proposed. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2638843A1
    申请号:ES201630514
    申请日:2016-04-22
    公开日:2017-10-24
    发明作者:Francisco Javier CARRIÓN FITÉ
    申请人:Universitat Politecnica de Catalunya UPC；
    IPC主号:
    专利说明:

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    D E S C R I P C I O N
    SURFACE DECOLORATION PROCEDURE OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM TYPE, THROUGH ULTRAVIOLET RADIATIONS AND AN ECOLOGICAL OXIDIZER
    TECHNICAL SECTOR
    Procedure for decolorization of textile materials as well as for the superficial pretreatment of untreated tissues, before dyeing.
    BACKGROUND OF THE INVENTION
    With reference to the electromagnetic spectrum, ultraviolet or UV-C light is the part of electromagnetic radiation located below the range of the visible light spectrum, with a wavelength from 180 nm to 400 nm. This ultraviolet radiation can be subdivided into a varied number of intervals, according to their wavelengths. a) Ultraviolet A of 400-315 nm; b) ultraviolet B from 315 to 280 nm and c) ultraviolet C from 280 to 200 nm. and from 100 nm to 200 nm, it corresponds to the UV vacuum (extreme).
    UV-C ultraviolet radiation has a high energy that decays as soon as it hits any surface. In the industry it is used for “surface curing.” It is also widely used in germicidal applications, effectively eliminating viruses and bacteria.
    Textile articles with natural fibers, especially cotton fabric, are highly sought after by consumers due to their excellent properties, such as their softness, hygroscopicity, affinity or compatibility with human skin, biodegradability and regeneration, good wetting, good comfort , etc..
    On the other hand, synthetic textile materials have many desirable physical properties, such as low dielectric constant, high relationship between strength and weight, durability, tensile strength, incogibility etc, and being important
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    its low cost (compared to natural fibers). They have intrinsically a low humidity (hydrophobic character) and low adhesion for various materials, for that reason they require surface treatments to increase surface energy, such as corona plasma treatments, already developed for many years and that have not yet reached the industrial application that popularizes them. The treatment that we propose to develop in this patent, is totally new for the industry, and consists in proposing the action of UV-C, with the appropriate wavelength, (by means of lamps that provide a short wavelength). This non-destructive treatment allows a high percentage of functional oxygen groups to be introduced on the surface of the polymer to improve its surface treatment and improve its wetting, aspects that are normally desired to be improved in synthetic polymers for dyeing and / or finishing process.
    DENIM fabric is a conventional fabric with a high density twill structure. This fabric usually has an indigo colored warp (blue tub dye) and with or without sulphurous dye (black to provide the desired dark blue color). For example: tub dye to provide 70 or 80% final color and the sulphurous dye will vary from 5 to 20%, according to the desired hue in its warp and the white weft. At the beginning of the twentieth century this fabric began to be used traditionally in garments for farm workers, farmers, etc., in the USA, however, since the decade of the 30's of that century, its convensional use was transferred in the work in the field to be a fashionable garment for all consumers, including everyday use, mainly as pants (Jeans manufactured, initially, in the 30s by Levi Strauss and Co. and Lee® and Wrangler® and. from eighty for many others). In its industrial finishing process, several procedures have been applied to give the consumer a more suitable and better-looking fabric, according to their demands and changing fashion. To this end, several industrial finishing and washing methodologies have been applied with technologies that have shown their disadvantages, as well! such as danger to the health of workers, tissue deterioration, non-ecological oxidizing reagents, etc. The requirement of the current consumer asks for DENIM garments that appear worn, worn, discolored in certain areas, and with holes in some cases. In order to achieve these effects, various industrial technologies have been required such as: washing of garments with small particles in the form of sand that provide friction to the fabric (sandblasting treatment, very harmful for
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    the lungs of the workers), using bleaching agents, or with enzymes that can provide a bio-polishing of the tissue, All this provides a designated color and appearance of wear of the color and the tissue, with an appearance of uneven discoloration.
    The indicated DENIM fabrics, or similar ones, are transformed into washed and finished garments.The final washing processes of the garment are carried out with two objectives: The first objective is to obtain the desired color on the surface of the denim fabric, with the bright appearance , and with its designated appearance, (by means of the so-called DE Fading) .The second objective on denim fabric is to obtain some special appearance effects: such as surface polishing, water repellency and also antimicrobial finishes and other properties.
    The abrasive action on the fabric has been developed using the action of small sand particles in an appropriate washing machine (stone washing), with or without oxidizing agent, such as potassium permanganate (US Pat. No. 4,816,033 and US Patent No. 4,740,231 proposed using a bleaching agent, such as sodium hypochlorite). This treatment allowed to discolor the tissue and reduce its resistance to the desired limit. This washing effect, called stone washing (USPat No. 7,347,878), in which DENIM tissue can be discolored from its initial color, also, this effect can be achieved with or without the use of the cellulase enzyme (Majid Montazer and Maryan Ali Sadeghian Maryan, Appl. Biochem. Biotechnol (2010) 160: 2114-2128; DOI 10.1007 / s12010-009-8727-4) in acidic or neutral medium, and with or without the stones for tissue friction but Its effect is less effective. Depending on the concentration of the enzyme and the pH, the desired surface effect of greater fluff with variation of brightness and some variation of color is produced. The laser is another technique that is used to discolor the tissue through a sweep over the garment, providing an aspect of color wear with the consequent loss of resistance and slowness in production, as it is performed for each garment with successive sweeps of the laser beam on it programmed to cover the entire garment or area to discolor, so many successive sweeps are required on the garment.
    In the previous washing processes, to the stone and with enzymes or with oxidizing agents, a series of variations of their properties occur in the garment
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    Physics such as decreased permeability, stiffness, loss of resistance, wrinkle recovery. All this has been the origin of various studies, for example, if we add fabric softener, a decrease in air permeability and folding stiffness of DENIM tissue will result. An oxidizing action (permanganate or chlorinated bleaching) and enzymes provide a decrease in resistance and increase in the wrinkle angle. On the contrary, the treatment of the fabric with softeners, such as silicones or cationic softeners, improves the feel and cadent of the same and the thermal conduction.
    With reference to the indicated washing of the fabric to the stone, called sandblasting, about 47 years ago it was banned in Europe, but the exportation of large cowboy productions to developing countries has allowed this technique to survive. In the factories that apply this technique workers must withstand the sand dust that is generated to wear the cloth. This sandblasting technique will not only be present in China; according to reports from various NGOs, it will also be applied in Turkey (illegally, because the government banned this technique in 2005), Bangladesh, Mexico, Cambodia, Pakistan India and Indonesia. The workers who apply this technique under undesirable conditions, suffer significant damage to their respiratory health, such as silicosis disease and in many cases death. These serious damages make it necessary to obtain different new procedures to achieve these degradative effects requested by manufacturers and consumers without the disadvantages of current procedures.
    This innovation presented in this patent allows to obtain notable advantages over traditional and usual decoloration procedures. As they are for example: wear with the conventional method of sandblasting, or little ecological oxidants (sodium permanganate, hydrogen peroxide); and that reduce the tensile strength of the garments (fabrics or fibers) treated by moisturizing the oxidant in all its volume, and other methods such as utilization of enzymes (degrading the substrate) or laser beams to discolor the tissues (through paths of the lightning by the areas to discolor, more expensive technique of amortization due to its expensive tooling).
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    EXPLANATION OF THE INVENTION
    This patent proposes innovative technologies to produce the same effect as traditional sandblasting, presenting as an alternative the action of ultraviolet radiation of type C and an inorganic oxidant that is proposed for this purpose.
    Also, in addition, a more ecological oxidant reagents than those normally used (permanganate, hypochlorite, ozone with steam, etc.) are proposed, such as potassium peroxymethyl sulfate (KHSO5, xKHSO4 .. xK2SO4), an inorganic product in aqueous solution to wet previously the tissue on the face of the same to be discolored, which together with the treatment with ultraviolet energy type C, is capable of producing the desired discoloration, depending on its concentration and treatment time of UV-C radiation. It can also be a superficial pretreatment before dyeing or finishing the tissue.
    Through the application of UV-C radiation, the surface characteristics of untreated or tended tissues, consisting of natural or synthetic fibers, preferably of cotton or polyester, are modified in order to obtain changes in the improvement of wettability that benefit their dye absorption processes in dyeing, stamping and finishing thereof, with respect to conventional processes, and performed only with the application of UV-C radiation or enhanced its action with the proposed oxidant.
    Enhancement of the action of UV-C radiation with an oxidizing agent, preferably for the discoloration of cotton and polyester fabrics and synthetic fibers held with different families of dyes. by means of the UV-C radiation action, together with the proposed oxidant action, the salts of the potassium peroxymethyl sulfate type. The application is proposed in cotton fabrics and their mixtures and, preferably for discoloration in DENIM type fabrics, (much requested by the current fashion in garments with worn appearance), as well as synthetic fibers had. The proposed inorganic oxidant is decomposed by the action of UV-C radiation, once it is present on the surface of the tissue, all the two actions contribute to the discoloration of the textile material.
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    Three factors have been considered to control the process of discoloration of tissues: the concentration of the oxidizing product potassium peroxymethyl sulfate, the treatment time of UV-C radiation and the weight of the aqueous solution of the oxidant by wetting part of the substrate (face of the irradiated tissue), this weight is that of the oxidizing solution per square meter of the tissue, in this case on one side thereof, by spray application. The complete imbibition of the tissue by the oxidant could also be carried out, which would cause it to be further degraded with the consequent loss of tensile strength and polymerization degree of the textile material, which may reach undesired limits, as has been proven. The ranges of the quantities of the following indicated factors are proposed:
    a) Concentration of the oxidant of the potassium peroxydonosulfate salt (or sodium): from 0 to 300 g.L "1, with this oxidizing agent, or in the absence thereof simply wet with water.
    b) The UV-C type ultraviolet radiation treatment time up to a maximum of 300 minutes, may be longer times if the tissue does not degrade in an undesired way.
    c) The amount of water absorbed, when applying the oxidizing solution to a face of the fabric by means of spray: from 0 to 400 g.m "2, capable of causing a superficial attack of the same, keeping its interior structure practically unalterable.
    d) Heraeus GPH356T5VH / 4 ultraviolet lamps, which are intended to be used with an applied potential of 17 watts each, and an emission of UV radiation, from 4.7 W at 254 nm and 1.9 W at 185 nm for Each lamp
    For its industrial application, ultraviolet PUV-S 60/09 XL lamps are proposed that were selected with a power of each of 105 W and a UV-C emission of 30 W at 254 nm. These lamps were enclosed in a hermetically enclosed cabin with a gas extractor outside, given the possibility that the result of oxidation produced ozone gas appears.
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    The new process of decolorization of the tissue (DENIM or other tissues), with UV-C radiation and the oxidant potassium peroxymethyl sulfate PS, implies the following advantages:
    a) A low temperature, with the consequent saving of energy and time.
    b) Discoloration on one side of the fabric (with loss of acceptable tensile strength, as has been proven) without damage to its internal structure or in selected areas with a template designed for this purpose to cover the area not exposed to the UV-C radiation of the tissue.
    c) Environmental improvements by reducing the consumption of auxiliary products, which could be toxic and not biodegradable.
    c) Utilization of an inorganic oxidant harmful to the environment.
    e) With lower process costs than current processes, thereby increasing industrial competitiveness.
    f) Possibility of selecting the areas of a face of the tissue to be discolored,
    keeping the rest unchanged.
    g) In case of tissues without having, perform a superficial treatment that improves its. surface and / or dye absorption and / or finishing processes
    BRIEF DESCRIPTION OF THE FIGURES
    Fig. 1.-. UV-C UV lamps used GPH356T5VH / 4 in these tests. (first practical example)
    Fig.2.- Color differences of the blue DENIM tissue, wetted in water (sprayed on the face of the tissue to be treated), depending on the treatment time of the UV-C radiation action
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    Fig. 3.- Color differences of the blue DENIM tissue, previously moistened (sprayed on the face of the treated tissue) with potassium peroxymethyl sulfate (PS, commercial denomination Caroat) (140 gL-1), depending on the treatment time (min), response of the UV-C radiation action
    Fig. 4.- Color differences of the DENIM blue tissue, previously moistened, depending on the concentration of potassium peroximonosulfate (PS, trade name Caroat) (on the face of the tissue to be treated), after 60 minutes with UV treatment radiation -C.
    Fig 5- Color differences of the DENIM blue tissue, previously moistened, depending on the concentration of potassium peroxymethyl sulfate (PS, trade name Caroat), after 240 minutes with UV-C radiation.
    Fig. 6.- Photographs of discolored samples of DENIM tissues (positive and negative discoloration effects, according to the design of letters made), applying the appropriate template to select the area treated with UV-C radiation, and enhance its action with a solution of 140 gL-1 of potassium peroximonosulfate (PS, trade name Caroat), in an amount of 100 gm-2, spray applied for 180 minutes.
    Figure 7.- Estimated response surface of the color difference in the tissue for 230 g.m-2 of oxidizing solution (practical example 2)
    Figure 8.- Estimated response surface of the color difference in the tissue for a time of 115 minutes (Practical example 2)
    h)
    Figure 9.- Estimated response surface of the color difference for an oxidizing solution concentration of 100 g.L-1 of potassium peroximonosulfate (PS, trade name Oxone)
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    PREFERRED EMBODIMENT OF THE INVENTION.
    PRACTICAL TESTS:
    1. Practical test first Experimental part and results
    a) Materials and equipment used
    Fabric used
    A blue DENIM fabric was used, with the dye 100g / L DIRESUL INDANAVY RDT-B liq and subsequent oxidation with H202. supplied by Archroma Iberica. The characteristics of the fabric were: warp density 30 threads.cm-1 and per weft 15 threads.cm "1, the number of the yarn per warp was 87.8 regular TEX and per weft of 85.6 regular TEX with a weight of 363 gm "2.
    Oxidizing agent proposed in the patent:
    Potassium peroxonosulfate (PS), 2KHSO5.KHSO4.K2SO4, under the trade name Caroat, supplied by Degussa Iniators GmBH & Co. With 4.5% active oxygen. CAS number 70693-62-8.
    Water used for oxidizing agent solutions:
    The water for the oxidizing agent solutions was obtained by passing the distilled water in a subsequent process of reverse osmosis Milli-A devices system. Water purity was checked by conductivity
    Equipment used for evaluations
    UV-C lamps for the proposed treatments
    Four GPH356T5VH / 4 lamps of ultraviolet radiation were arranged, showing a power in each of them of 17 W and a UV-C emission of 4.7 W at 254 nm and 1.9 W at 185 nm. Figure 1 the appearance of said
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    lamps, which were placed for the treatments inside a gas extractor hood in the Laboratory.
    Spectrophotometer used to evaluate color differences:
    The reflectance of the tissues was determined using a spectrophotometer, provided with a standard iQC color software supplied by X.-Rite Incorporated (USA), distributed in Europe by Regensdorf (Switzerland). This equipment is equipped with a Xenon D65 lamp and was used with a measuring range of 360 to 750 nm (visible spectrum), in 10 nm intervals and reproducibility of 0.01 RMS AE CIELAB.
    Procedures:
    Previous washing of the fabric.
    The previous washing of the DENIM fabric (initially obtained free of impurities) was produced by using a domestic washing machine, Miele Hydromatic with 2 gL "1 of ECE detergent, ref A, supplied by SDC Enterprises Limited of Bradford (UK), using a washing program for cotton at 30 ° C, 60 minutes long.
    UV-C radiation treatment for DENIM tissue.
    The tissue samples (10 x 4 cm), were subjected, in the Laboratory, inside a fume hood, to the radiation of the four UV-C lamps, with the technical specifications contained in the previous section: They were arranged at the same time in a horizontal position at a distance of 5 cm, above the fabric, during the different selected times, in ambient atmospheric conditions 60 ° RH of relative humidity and 20 ° C of ambient temperature. The tests were carried out in duplicate and the average value and corresponding deviation of the color differences obtained were obtained in each test.
    DENIM tissue treatments before being subjected to UV-C radiation.
    From wetting with water on one side by means of spray of the DENIM fabrics, impregnating an amount greater than 100 g.m "2, the samples of the indicated tissue were placed at the action of UV-C radiation, at different treatment times
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    (tested for 30 to 240 minutes), as indicated for the differences in color in Figure 2. With the same treatment times and amount of wetting in the tissue, a solution of 140 gL-1 of potassium peroximonosulfate (PS), the color differences obtained in Figure 3 were indicated.
    With the application. by spray, on one side of the DENIM fabric, of different concentrations of PS, from 0 to 140 g.L-1, in a variation of times up to 140 minutes, the results of color differences are shown in Figures 4 and 5 respectively
    All the color differences obtained were the average result of duplicating all the tests, the results of which are indicated in the cited figures.
    UV-C ultraviolet radiation treatments
    All previous tissue samples previously treated with the PS oxidant, at different times, were subjected to UV-C ultraviolet radiation on the wet tissue face, at variable times up to a maximum of 240 minutes.
    Said treatment can be carried out on the entire surface of the fabric, on a whole face or in an area previously designed in a template, placed on the fabric, with the drawing considered, to allow radiation to pass in the area not covered by the template (negative of the drawing).
    Evaluation of the results Chromatic coordinates:
    The CIElab color coordinates (L *, a * and b *) * 1 were determined by subjecting the tissue sample to the measure of a 10 ° observer and a D65 illuminant
    The color coordinate values were evaluated in the CIELAB color space, according to the three axes L *, a * and b *. L * is the color coordinate that represents the brightness of the samples and can be measured independently of the color hue. Any decrease in the luminosity of the samples was interpreted as a lower textile reflectance. In each plane, perpendicular to the L * axis (luminosity), there are chromaticity coordinates, which are the + b * a * -b axis "y" and
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    the perpendicular to + a * -a * axis "x", where b * represents the yellow color (90 °) and -b * represents the blue color at 270 °, and + a * represents the red color at (0 ° = 360 °) and -a * represents the color green at 180 ° * 1 (. McDonald Roderick, Physics Color of Industry, Bradford. Second edition. Society of Dyers and Colorists (1997), ISBN 090195670-8 pp 136-147)
    Color differences:
    The color coordinates were precise enough to be used to quantify the color differences between two standards (without having and untreated sample and the treated UV-C sample).
    Color differences were calculated using the color coordinates in the equation.
    1 1 1 * - 2 * - 3 * - 4 *:
    A E = {(A L *) 2 + (A a *) 2 + (A b *) 2}% (1.1)
    where A L *, a * A and A b * represent the differences between the corresponding color coordinates of the DENIM cotton fabric, without treatment and the cotton treated with UV-C.
    These values were the average of four reflectance readings obtained with the rotation of the sample through 90 ° after each measurement. The samples tested of the cotton tissues had, after being treated with UV-C radiation and the results were the average of two repeated tests.
    * [1] CIE. Improvement to Industrial Color Difference Evaluation. ICD 142 - (2001) Commission Internationale de l'Eclairage. Vienna 2001 * [2] Standard ISO-105-J03: 2009 or UNE ISO-105: J03
    * [3] Robertson Ar, 1990 Historical development CIE recommended color difference equations, Color Res. Apll, 15 (1990) pp 167-170 * 4] Chodhury, Asim Kumar Roy, foreword by Gary N. Mock, Modern Concepts of Color and Appearance, Raleigh NC, USA Science Publishers (2000), Inc ISBN-157808-078-9
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    When comparing the results of the blue DENIM fabric, previously wetted with water (Fig 2), by spray, on the face to be treated with UV-C, and in the same way with a treatment with the solution of potassium peroxonosultafo (PS) at 140 g. L "1 (Fig. 3), applying UV-C radiation at different times, it can be observed, by difference in behavior, the effect produced by this proposed oxidant enhancing the discoloration obtained from the tissue at all times tested. Asl for example , considering the 200 minutes of UV-C radiation treatment, in the previous graphs, corresponding to the color differences obtained in the indicated tissue, previously treated with this oxidant and UV-C, their color differences (value of 45,) It was slightly more than 5 times greater than treatment with UV-C and water alone (value of 8.5) (absence of oxidant).
    In this figure 4, corresponding to the color difference of DENIM tissue, after a 60-minute treatment of UV-C radiation, as a function of the concentration of potassium peroximonosulfate (PS) it can be seen that such differences increased with increasing concentration from 0 to 140 gL-1. the treatment with water alone being the lowest value obtained, with a color difference of 2.5 (not very significant) and at the highest concentration of PS tested, in general, a color difference value of 28 (very significant) was obtained.
    In this figure 5, corresponding to the color difference of DENIM tissue, after a UV-C treatment of 240 minutes in all the treated samples, depending on the concentration of potassium peroximonosulfate it can be seen that such differences increased with the increase of the concentration of 0 to 140 gL-1 of the oxidant PS, the treatment being only with water, the lowest value obtained with a color difference of 10 (not very significant, without PS) and the highest tested concentration of PS, in general, obtained a color difference value of 48 approx (extremely significant with the action of the PS, enhanced by UV-C radiation)
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    2. Second practical test
    a) Material: Same blue DENIM fabric indicated above in practical test 1
    b) Oxidizing agent proposed in the patent:
    Another commercial version of the following proposed oxidant: Potassium Peroxonosulfate (PS), KHSO5.0.5KHSO4. 0.5K2SO4, under the trade name OXONE® supplied by Sigma-Aldrich, pure reagent of molecular weight 307.38. CAS Number 70693-62-8.
    c) Application of UV-C lamps
    Six ultraviolet PUV-S 60/09 XL lamps were disposed that were selected with a power of each of 105 W and a UV-C emission of 30 W at 254 nm. These lamps were enclosed in a hermetically enclosed cabin with a gas extractor outside to evacuate the gases produced in the oxidation of the dyes of the tissue.
    d) Evaluation of color differences: with the same spectrophotometer used in the previous practical test 1 and with the same procedure for assessing the color differences indicated above.
    d) Procedure:
    Samples of 75 cm, 750 cm 2 with dimensions of 25 x 30 cm.
    The tissue samples (25 x 30 cm) were subjected to the radiation of the six UV-C lamps with the indicated specifications, at a distance, in a horizontal position of 5 cm of the tissue sample, for the different selected times under ambient conditions of the atmosphere 60 ° relative humidity and 20 ° C temperature. The tests were performed with two different repetitions and the average value and the corresponding deviation were obtained.
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    Analysis of the results
    Three factors were considered to control the degradation process: the concentration of the potassium peroximonosulfate (PS) product, the UV-C treatment time and the amount of oxidant solution considered by wetting the substrate by spray (it was verified by weight difference of the wet sample). The operating region was defined with the following factor levels:
    - Product concentration PS (g.L-1): 40, 100, 160.
    - UV-C treatment time (min): 10, 115, 220.
    - Amount of water from the oxidant solution (g.m-2): 100, 230, 360.
    Two replications of a factorial design were made with these three factors, therefore, 32, resulting in the (27 x duplicate) 54 randomized trials.
    The response observed was the difference in color between two samples, 1 (the reference) and 2 (the one tested, degraded sample). The CIELAB color difference was given by the equation indicated above for the measurement of the color difference from the color chromatic coordinates of the tissue. These color parameters were the average of four determinations by rotating the sample to be evaluated 90 ° C. All color difference values were the average of two different repeats of the same test conditions.
    The relationship between the response and the process variables was unknown, therefore, now, an approach to the true functional relationship was intended. In industrial practice, a polynomial of order two defined in the operating region is usually used.
    The polynomial model indicated is represented in the form of equation (2.1) and the coefficients found are indicated in Table 1.
    and -P0 + ^ 1x1 + ^ 2x2 + ^ 3x3 + Pnx2 + P22x2 + P
    + P12x1x2 + P- | 3x- | x3 + P23x2x3 + ^
    image 1
    (2.1)
    The method of least squares is used to estimate the regression coefficients (P) of equation 2. These coefficients of the fitted model were indicated in table 5. It was observed that the concentration-time interaction is not given since it is not significant (it has been detected in the factorial design made previously).
    The significance of each term in the equation is shown in table 2 (analysis of the variance of the regression). In this case, 7 effects had a P-value less than 10 0.05, indicating that they are significantly different from zero with a level of
    95.0% confidence.
    Table 1: Regression coefficients
     Equation Term  P
     Constant  -3,42262
     Xi: CONCENTRATION ON  0,0995416
     X2TIME  0,0923535
     Xa: WATER  0.0514217
     X12  0.000511728
     X1X3  0.00030414
     X22  -0,00036479
     X2X3  0.000125382
     X32  0.000091946 1
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    Table 2: Analysis of the regression variance
     Source  Sum of Gl Square Reason- P-Value
     Squares Medium F
     Xi: PS CONCENTRATION  584.35 1 584.35 76.92 0.0000
     X2 UV-C TIME  551,898 1 551,898 72.65 0.0000
     X3: PS SOLUTION WEIGHT IN FABRIC  1771.43 1 1771.43 233.18 0.0000
     X12  40.7254 1 40.7254 5.36 0.0252
     X1X3  135,066 1 135,066 17.78 0.0001
     X22  194,099 1 194,099 25.55 0.0000
     X2X3  70.2982 1 70.2982 9.25 0.0039
     X32  28.9748 1 28.9748 3.81 0.0571
     Total error  341,862 45 7.59694
     Total (corr.)  3718.7 53
    The combination of the levels of the variables that maximizes equation 2.1, in the operational region is indicated in table 3 (optimization of the response of the color difference 5), and provided a maximum value of 36.4731.
    Table 3: Optimization of the color difference response g. m "2
     Factor  Low High Optimum
     CONCENTRATION Potassium peroximonosulfate (PS)  40.0 160.0 160.0
     g.mTITIME treatment  10.0 220.0 188,465
     g. m "2 solution PS in fabric  100.0 360.0 360.0
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    The optimization of the color differences obtained as a function of the concentration of potassium peroximonosulfate (PS) time and weight of the solution in the tissue were indicated in Table 3.
    The response surfaces corresponding to the adjusted polynomial (equation 2.1 and table 1) were shown in Figures 7, 8 and 9 and help to visualize the optimal calculated value.
    权利要求:
    Claims (1)
    [1]
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    1a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, PREFERENTLY DENIM FABRICS”, also in the form of flock, wick, thread or fabric, or ready-made garments, after their dyeing and / or finishing, or to carry out a previous treatment of textile material before dyeing, characterized by the following treatment stages:
    Moisturized, preferably by a total or partial face (in the area to be discolored), of the textile material with an inorganic oxidant, preferably with a salt of the potassium or sodium peroximonosulfate (PS) type, with a percentage on the weight of the material of its aqueous solution, in the desired concentrations in the range indicated in the following claims.
    Exposure to UV-C ultraviolet radiation of the wetted face of the textile material with the inorganic oxidizing salt PS according to the chosen concentration. The exposure time will be chosen, according to the range indicated in the following claims, according to the desired degree of discoloration. The UV-C radiation exposure zone can be total or partial (selected zone).
    Subsequent rinsing and conventional washing and / or softening treatments.
    2a) “ALTERNATIVE FABRIC DECOLORATION PROCEDURE
    NATURAL AND SYNTHETIC, SPECIFICALLY DENIM FABRICS ”, according to the first claim, characterized by the use of concentrations of potassium peroximonosulfate from 0 to 300 gL-1, to wet the tissue with spray, by fine dispersion of said solution on the tissue side treat with UV-C. In case of using the non-woven fabric, it will be performed in the same way, if such an energetic surface oxidation is not required, only with the UV-C treatment, will it be sufficient to produce such oxidation of the tissue surface and produce an improvement of the affinity for the dye in the dye or improvement of the finish.
    3a) “ALTERNATIVE FABRIC DECOLORATION PROCEDURE
    NATURAL AND SYNTHETIC, ESPECIALLY FABRICS DENIM ", according to the first and second claims, characterized by the use of
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    concentrations of potassium or sodium peroximonosulfate from 0 to 300 g.L-1 to moisturize the tissue by a fine dispersion on one side thereof; The aqueous solution in the tissue will be applied before said UV-C treatment, at different optional times, with weights of said solution absorbed on the tissue to be treated, which will range from 0 to 400 g.m-2.
    4a) "ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS", according to the first, second and third claims, characterized by the use of potassium peroximonosulfate concentrations from 0 to 300 gL-1 to wet the tissue by fine dispersion of the same for the face of tissue that will be treated with UV-C, with total weights in the tissue of this aqueous solution of the oxidant PS of 0 to 400 gm-2, and with UV-C treatment times that can range from 0 to 300 minutes, and with an optional domestic-type backwash, without altering the discoloration produced, smoothing and finishing processes can be carried out as appropriate.
    5a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS”, by means of the first, second, third and fourth preceding claims, characterized by their application to natural or synthetic fiber fabrics, previously had, according to the type of matter , with direct dyes, azoic, tub, sulphurous, sulphurous, more indigo, indigools, reagents, dispersed and basic, separately, or in a mixture, used in their different processes of continuous, semi-continuous or exhaustion dyeing, through the methodologies of formulating conventional dyeing, according to dyes used. A mercerizing prior to the dyeing of sulfurous dyes will provide a better shine of the fabric and also facilitate a better ironing after the washing of the fabric had, all this without diminishing the effect of discoloration produced of the fabric had.
    6a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS” by means of the first, second, third and fourth and fifth preceding claims, characterized by its application to DENIM fabrics, held with Indigo dyes, or sulphurous or more indigo sulphides For example, Diresul RDT (Archroma) dyes, applied to
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    fabrics in the form of rope or wide fabric, according to the appropriate machinery and conventional dyeing procedures and subsequent oxidation, preferably with hydrogen peroxide, discolorations occurring under the conditions indicated in the previous claims with the process of this patent. Subsequently, optionally, it can be washed and finished as desired.
    7a) "ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS", by means of the first, second, third, fourth, fifth and sixth previous claims, characterized to be applied to DENIM fabrics held, with a variation of tissue weights in the following ranges: light fabrics from 136 to 237 gm-2; light 237 to 373 g.m-2; average weight 373 to 475 gm-2 and heavy from 475 to 542 gm-2, with any fabric structure, preferably with twill-type tissue structures of structures: 2/1 or 3/1 (two or three yarns above and one below at the intersection of the tissue). The same effect is produced with knitting structures. in any of its spinning cross-linking variants. In the case of non-woven fabric, the oxidizing agent can be used, with the application of the UV-C action, to oxidize the surface of the fabric, thereby modifying its absorbent capacity posterior dye during dyeing or subsequent finishing.
    8a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS”, by the claims of the first to the seventh, characterized by its application to yarn fabrics of natural fibers or synthetic fibers of continuous filament or cut fibers, of any number of yarn or fiber, had or not had and / or finished.
    9a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS”, according to the previous claims of the first to the eighth, characterized by the production of its effects by a face of the fabric, corresponding to the face treated with UV- C over its entire surface, or with effects located in certain areas of the tissue selected according to design, or by selecting different bleaching effects produced by different times of treatment of UV-C radiation in the same tissue, or with concentrations of the oxidizing potassium peroximonosulfate or sodium with different amounts of its aqueous solution sprayed on the surface
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    of the fabric, at different times, within the range of the range indicated in the fourth claim.
    10 °) "ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS", according to the previous claims of the first to the ninth, characterized by the post-dye finish can be performed before or after the indicated discoloration, having Note that it is necessary to obtain an optimal behavior of the fabric, or of the garment, during domestic washing in terms of dimensional stability, tensile strength and elasticity. It should be noted that any finish of the DENIM garment is based on the trends and effects requested by fashion and is suitable for the application of this indicated bleaching procedure. For the finishes can be used mechanical processes (treatments of dry textile material) or chemical (textile material with application of products by wetting)
    11a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS”. According to the preceding claims from one to the tenth, characterized in that the post-dye finishing can be performed before or after the indicated discoloration. The basic basic finishing operations are carried out before the weaving process (decoupling, mercerizing, etc.). The process of making garments requires that the fabric conform to the design of the garment and without loss of color and stability when it reaches the consumer. Finishes such as brushing and gassing (removal of surface fibers) with subsequent washing to remove loose fiber fabric, sanforming to avoid compression shrinkage, during this process the width and length of the fabric must be controlled and other subsequent process, as calendering may be necessary for tissue shine. The heat setting of the fabric and the time will depend on the type of elastomer in the fabric fiber mixture. Before making, a smoothing will facilitate the falling of the required fabric, with the touch desired by the consumer.
    12a) “ALTERNATIVE PROCEDURE FOR DECOLORATION OF NATURAL AND SYNTHETIC FABRICS, ESPECIALLY DENIM FABRICS”. according to the preceding claims from one to the eleventh, characterized in that the finish
    post-dyeing can be done before or after the indicated discoloration, and most mechanical finishes, such as breaks in the fabric or warp yarn, pocket wear on its edges or seams, etc., can be planned with the procedure indicated in this patent, increasing the concentration of the oxidizing product potassium peroximonosulfate to high
    concentrations and prolonged times of treatment with UV-C, to get to adjust the breaks by excess of oxidation of the textile material or the desired discoloration of the fabric, in the suitable conditions (demanded by the design in each moment).
    FIGURES
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    同族专利:
    公开号 | 公开日
    ES2638843B1|2018-09-11|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO1992015744A1|1991-03-05|1992-09-17|Lappage, James|Photobleaching process for natural fibres|
    ES2109678T3|1993-02-16|1998-01-16|Commw Scient Ind Res Org|TREATMENT OF WOOL FABRIC AND WOOL BLEND.|
    EP1584736A2|2004-03-24|2005-10-12|National Institute of Advanced Industrial Science and Technology|Method for bleaching fibrous articles|
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