TW200804645A - Control of PH in the treatment of fabric - Google Patents

Abstract

This invention relates to the treatment of fabric, particularly cellulosic and cotton fabric, in which the pH in the treatment liquid is controlled. According to the present invention there is provided a process for the treatment of fabric under alkaline conditions which process comprises treating the fabric with a treatment liquor to which has been added an aqueous alkali solution comprising (i) 9 to 36% wt% of a borate selected from an alkali metal and ammonium borate, or boric acid; and (ii) 8 to 35 wt% of at least one alkali metal, ammonium or organoquaternary ammonium hydroxide. The present invention provides an alternative to previous methods and which may avoid or mitigate disadvantages associated with the previous methods.

Description

200804645 IX. Description of the invention: The invention relates to the treatment of fabrics, in particular cellulose fabrics and cotton fabrics, wherein the pH value in the treatment liquid is controlled. Most particularly, the present invention relates to the control of the pH of a treatment liquid for dyeing cotton fibers and cellulose fibers using a reactive dye.

L J Spring Carefully controls the pH of the liquid used in textile preparation and dyeing operations, including printing operations and finishing operations. In addition to dyeing, the present invention is also applicable to, for example, cellulosic or cotton fabrics such as scouring and mercerizing. ^ A number of such operations require that the pH of the treatment fluid be set within the narrow limits. For example, the dyeing of wool fibers or nylon fibers is usually carried out in a mild acidic solution using a homogenous acid dye or a 1:1 metal complex dye; while the poly-15 ester fibers are dyed using a disperse dye, which is conventionally employed by ρΗΜ4· 5_5·5fan_ surrounding solution, but more recently asked the city's higher ΡΗ (8·7 to 9.5) dyeing method. Since the invention of reactive dyes in the 1950s, cotton fabrics and cellulosic fabrics have been dyed in dye baths having a pH in the range of 11-11.5. This is required to perform the cellulose-dye reaction. What is the reaction between the dye and the fabric? 11 must be high enough to be carried out at a sufficiently fast rate at the actual 2 〇 dyeing temperature, but not so high that a competitive dye-consuming hydrolysis reaction may occur in the dyebath. In addition to these a cases, there is a method of dyeing the sputum, which is required to maintain a very special pH condition during the dyeing operation. There are indeed a number of cases that are not simply maintained in the fixed range during the dyeing process, but are deliberately processed through processing 5 200804645 to change with the duration of the dye process. In order to maintain the pH of the liquid or the pH of the liquid, it is often necessary to use a simple strong acid and an early pure test such as hydrochloric acid and sulfuric acid or sodium hydroxide. The sodium oxychloride is used, for example, for scouring and mercerizing of cotton, scouring and mercerizing as examples of preparation steps used prior to dyeing 5 or printing. However, in order to maintain the pH at a lower limit, pH buffers are required in the absence of complex automated metering systems and monitoring systems. pH buffers are primarily salts of strong acids and weak bases, or vice versa. A common example of a weakly acidic buffer is sulphate and acetaminophen 4, while sodium acetate is used as a weak buffer. For example, a sulphate buffer of the base 10 in the self-salt or pyrosulfate can be operated over a wide pH range (2.5-11). However, environmental considerations have increased the acceptability of phosphates, so alternative materials must be sought. The pH is deliberately adjusted during the dyeing process, using chemical means, and often by changing the temperature to trigger the adjustment of ρΉ, depending on the volatile acid component of the buffer system and the evaporation of the component, or relying on the use of 15 hydrolyzable esters To release acid. In order to dye reactive dyes on cotton textiles and cellulose textiles, soda ash (de-saturated acid) is often used as the source of the test and the pH buffer of the dyebath. The pH is required to be maintained in the range of 1M1.5. Get the best results. The soda ash is inexpensive, and the pH of the dilute sodium carbonate solution is in the range of ΐι·5 to 11.8, and the optimum buffering efficiency in the solution is about pH 1〇3, thus making the sodium carbonate very suitable for this application. . Although this is the case, the use of associated copper carbonate has its drawbacks. Sodium carbonate is a solid experience and requires proper dissolution prior to use to avoid clogging the feed line and creating spots on the textile. This requires the use of a premix tank. The alkaline material is supplied in bags and must be handled manually. 6 200804645 The correct amount of bagged strong alkali is fed into the premix tank, posing a risk of a sinister error due to human error. The empty bag needs to be disposed of properly. In addition, 8 to 20 grams per liter of soda ash is often used in dye baths, which means that there is a considerable amount of chemical consumption, which may increase the environmental load. 5 Attempts to overcome some of the problems caused by the use of solid soda ash in the dyeing of cotton fabrics and cellulosic fabrics by reactive dyes have prompted the idea of using pre-dissolved and carefully selected mixtures and assay buffers. It is claimed that it is easier to accurately and accurately feed the material in modern dyeing. In addition, it is designed to compare soda ash and work in lower concentration dye baths. These products are referred to as Formulation 10 liquid bases, for example as disclosed in EP-A-0165079. This specification discloses a high pH formulation, mainly based on a phytate, which contains a small amount of potassium hydroxide and optionally contains borax pentahydrate and triethanolamine. In view of environmental concerns about phosphates, US 5,327,611 discloses a liquid test based on bismuth citrate. Such a small amount of borate 15 (metaborate, perborate) may be contained as needed. However, bismuth sulphate-based products often have disadvantages. A compelling disadvantage is the formation of insoluble magnesium silicate residues, which are difficult to remove from dyed textiles. In addition to the previously described liquid bases designed for reactive dyes in cotton textiles and cellulosic textiles, batch-based depleted dyeing, 20 GB-A-2006837 reveals the use of more concentrated metal silicate solutions. The combination of low/minus alkali metal borate is used for the crosslinking of reactive dyes on cellulosic materials, shell liner batching or human dyeing or printing. Embossing is a procedure involving the application of a dye to a fabric in a mechanical manner, drying, and then applying a salt and a base to fix it. The batch-like depletion of the dye procedure involves soaking the textile in a large amount of dye liquor. 7 200804645 The dyeing procedure uses a small amount of water to obtain a more concentrated dye liquor. The use of borate is usually more specific than the formulated liquid assay for pH buffering in the dye bath, which is well known but not common (eg reference colorants and supplements, organic chemistry and application properties, Phase 2 adjuvants, edit JSh〇) Re, 5th edition, Society of Stainers and Colorists (2002), ΡΡ 499·505).

10 The use of hydrolyzable ester butyrolactone and sand blasting in the dyeing of wool to achieve a pH shift from 8 to 5.6 is disclosed in DE 2354728. It has been reported that borax is occasionally used to control the pH of alkaline dyeing of polyesters, which contain a large number of cyclic ridges (M Dohmen, Knitting Technology, 4-99, July 1999, 3 pp.). When the sand or acid salt is used for pH buffering of the dyeing process, the target pH of the % is in the range of 8.5-9.5. No evidence has been found. When the target is beyond the pH value of this range, borax is used as the main buffer component. [After the accident, it was unexpectedly found that an aqueous borate-containing alkali solution can be used for the alkali. Treatment of fabrics under special conditions, especially cellulose textiles and cotton textiles, most particularly by dyeing, scouring and mercerizing, controlling the pH in the range of 1 to 12 5, especially 11 to 12·5, for example 11 to The scope of 11·5. This document provides an alternative to the prior art methods discussed above, and avoids and mitigates the shortcomings discussed in the previous section. According to an aspect of the present invention, there is provided a method of treating a fabric under an experimental condition, the method comprising treating a fabric using a treatment liquid in which an aqueous test solution has been added, the aqueous alkaline solution comprising (1) 9 to 36 wt% selected from Metallic borate and ammonium borate of the acid 8 200804645 salt, or boric acid; and (8) 8 to 35 wt% of at least one alkali metal hydroxide, hydrogen peroxide or organic hydrogen hydroxide fourth money. According to a preferred aspect of the present invention, there is provided a method of treating a cellulosic fabric or a cotton fabric, for example by dyeing, scouring 5 or mercerizing, which comprises treating the fabric with a treatment liquid in which an aqueous test solution has been added. The aqueous test solution comprises (I) 9 to 36 wt% of a borate selected from the group consisting of alkali metal borate and ammonium borate, or boric acid; and ίο (8) 8 to 35 wt% of at least one metal hydroxide, ammonium hydroxide or organic Tetraammonium hydroxide. According to another aspect of the present invention, there is provided a method of adding an aqueous test solution to a treatment liquid for controlling pH in a fabric, particularly for treatment of a cellulosic fabric or cotton fabric. The aqueous test solution comprises 15 (1) 9 Up to 36% by weight selected from the group consisting of metal sulphates and ammonium sulphates, or boric acid; and (II) 8 to 35 wt/. At least - a metal hydroxide, a hydroxide or an organic ruthenium tetraammonium oxide. The aqueous secret solution according to the invention (4) preferably has the following composition: 20 (i) 9 to 36 wt% selected from the group consisting of metal sulphate and sulphate, or boric acid; (9) 8 to 35 wt% of at least one type of metal hydrogen Oxide, oxynitride or tetraammonium hydroxide; (ill) optionally, a weak acid having a pKa in the range of from 1 to 118, preferably 9 200804645 - 5 organic weak acid; (iv) optionally, for example Up to 1 wt% adjuvant component; the difference is water. The weak acid is usually used in an amount of up to 20% by weight, suitably from 1 to 20% by weight, and preferably from 3 to 10% by weight. The presence of a weak acid allows the buffering capacity of the alkaline solution for the treatment of textiles in the high pH range of interest to be further increased. The optional adjuvant ingredients used include, for example, biocides, antifoaming agents, wetting agents, humectants, chelating agents, and suspending aids. The borate used in accordance with the invention is preferably borax pentahydrate. 10 Suitable aqueous alkaline solution contains a dissolved solids content of 35 to 55 wt%. The pH of the treatment liquid is suitably controlled in the range of 10.5 to 12.5, preferably 11.0 to 12.5. Fabrics which can be treated in accordance with the present invention include cellulosic fabrics and cotton fabrics. Cellulosic fabrics include fabrics made from cellulosic fibers, including slime fibers, lyocells, and high wet modulus high breaking strength modal fibers. Cellulosic fabrics and cotton fabrics include fabrics made from such materials as blends of synthetic fibers such as polyester, polyamide, and polyacrylonitrile. Typical blends include cotton/cellulose blends rich (eg, 85:15 or 20 60:40), synthetic fiber rich blends such as polyethylene terephthalate ethyl ester/cotton blends such as 67. : 33 blend and 50:50 blend. Fabrics treated in accordance with the present invention also contain elastane, including, for example, cotton/elastane blends. The method according to the invention can also be applied to other kinds of fabrics which may be subjected to treatment under alkaline conditions, such as 10, 0,046,445, a reduction-and-dispersion treatment applied to polyesters and polyester/cellulose blends, such as such fabrics, for example It can be treated by a fabric surface dye. 9 according to the present invention, a method for scouring a fiber fabric is provided, the method comprising a scouring pad containing water and a scoured fabric, added according to the invention and: a solution and heat treatment . Aqueous base for use «Another embodiment of the present invention provides a cellulosic fabric or

A method of mercerizing the cotton fabric is added to the bath, which comprises mercerizing the aqueous alkaline solution used in accordance with the present invention. According to another preferred embodiment of the present invention, there is provided a method of fixing a dye, typically a reactive dye, to a cotton or cellulosic fabric, the method comprising: in a dyeing treatment bath for applying a cellulosic or cotton fabric: An aqueous alkaline solution used in accordance with the present invention is added. [Bag: ^Γ The dyeing program can be batch, semi-continuous, continuous, or print processing. Unexpectedly, in view of the previous observation of the use of borate, the solution used in accordance with the present invention can be used to impart reactivity when added to a cold at a low concentration together with a suitable amount of a salt and a reactive dye. The dye is dyed 20 to the optimum range on the textile to help achieve excellent dyeing results. In particular, the resulting dyeing results are characterized by a bismuth coloring yield which is at least matched to the coloring yield obtained when soda ash is used as an alkaline buffer at a concentration of two more concentrations. For the two-color combination of dyes' use of the solution used according to the invention compared to the use of soda 11 200804645 ash in terms of total color (brightness and hue), can only be obtained in small and often not obvious (the Chiyou instrument and visually In terms of) differences. When the composition of the present invention is used as a bath buffer and an alkaline agent, the reactive dyes on cotton fibers or cellulose fibers can be successfully dyed, including all major and commercially important reactive dyes. category. These classes include monofunctional reactive dyes and difunctional reactive dyes. Examples of monofunctional dyes include, but are not limited to, dyes containing the following reactive groups: trichlorotrit, amine chlorotrim, amide sulfonium tris, trichloropyrimidine, chlorofluoro, 11, and Chloroquine ° such as Lin, the acid acid ethyl barrier, and the acid group 10 ethyl sulfonamide. Bifunctional dyes include, but are not limited to, dyes containing a combination of the following functional groups: home (amino chloride, chlorine) - "bisMCT", martial acid (lithic acid ethyl stone) - "bisSES", hydrazine (amine based test Acidic trimorphine), aminyl chloromorphine monosulfonate ethyl hydrazine - "MCT/SES", and amine fluorotrisole - tartaric acid ethyl hydrazine. Practical examples of bifunctional reactive dyes include CX Reactive Black No. 5 15 (Everzol/Remazol Black b), CL Reactive Yellow No. 176 (Ivan Left/Rima Left Yellow) 3RS), CI·Reactive Red No. 239 (Yi Zuo/Rima Zuo Β·Red 3BS), CI Reactive Yellow No. 84 (Evercion/proci〇n yellow H-E4R) , CX Reactive Red No. 141 (Efxin / Puxin Red H-E7B), and CI · Reactive Blue No. 171 (Aifu 20 Xin / Puxin Navy H_ER) ° These categories include so-called thermal dyeing Reactive dyes and temperature-sensitive reactive dyes. Thermal dyeing is typically carried out at about 8 (rc, while warm dyeing is typically carried out at temperatures ranging from 40 ° C to 60 ° C. The degree of dyeing on the fabric (the depth of shade to which the dyeing is applied) is based on fabric weight. In the range of 〇 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到 到A negative charge is developed, so these groups are ionized in the corresponding pH range (10-12). The cellulose in the cotton is also ionized under these conditions (OH groups lose protons), which are dyes and fabrics. The final chemical reaction 5 should be required ("fixed"). Therefore, there is electrostatic repulsion between the dye molecules and the fabric. In order for the dye to be depleted onto the fabric/adsorbed onto the fabric, the charge must be blocked or screened. Typically, the addition of a salt is carried out. The liquid alkali solution of the formulation used according to the invention comprises a source of borate selected from the group consisting of alkali metal borate or ammonium borate or boric acid. The alkali metal is preferably sodium 10 or potassium. Better because the sodium borate is formed The product is low and easy to obtain. The tetraborate pentahydrate pentahydrate (borax pentahydrate) is the best test metal borate, but like potassium pentaborate and potassium tetraborate, disodium tetraborate decahydrate can also be used. Sodium diborate pentaborate and sodium metaborate. Ammonium pentaborate which is an example of a non-metal borate can also be used. 15 The other main components of the liquid alkali composition are alkali metal hydroxide, hydrogen emulsified ammonium or organic hydroxide Tetraammonium. Preferred hydroxides are sodium hydroxide or potassium hydroxide, but also include tetraalkylammonium hydroxides such as tetramethylphosphonium hydroxide. Examples of the combination of the acid salt and the metal hydroxide Including but not limited to boron 20 夂 / 虱々 虱々 、 、 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删 删The percentage of the total weight of the liquid composition of the knife or gas emulsion component is listed in Table 1. The data in parentheses defines the composition limits of the narrower limits. 13 200804645 Table i Borate/Hydroxide Composition Minimum ( Wt%) maximum (wt%) Boric acid / potassium hydroxide boric acid 10 (15) 27 (22) potassium hydroxide (100%) 18 (24) 35 (35) boric acid / sodium hydroxide boric acid 10 (18) 27 (23) sodium hydroxide 14 (18) 32(28) Borax Pentahydrate / Hydroxide Hydroxide Pentahydrate 9(16) 36(28) Potassium Hydroxide 8(15) 30(26) In addition to borate and hydroxide, it may include pKa as needed a weak acid in the range of 10 to 11.8, which may be an inorganic weak acid or an organic weak acid. When a weak acid is included, the weak acid is at most 20% by weight of the liquid base composition, suitably 1 to 5 20 wt/min, and preferably lower than L〇wt% is, for example, 3 to 10% by weight. Although not limiting, examples of suitable weak acids include guanidine-aminobutyric acid, methylaminobutyric acid, and ascorbic acid. When included, a weak acid increases the buffering ability of the composition in the pH range of interest, but the use of a weak acid is not necessary. In general, a weak acid is only required when the side acid salt content is less than 10% by weight, and when the borate content is less than about 15 plus 0/〇 10, it is advantageous to include a weak acid. A weak acid is usually not required when it is above 15% borate. Additional formula additives (auxiliary ingredients) may be included in the liquid base composition used in accordance with the present invention. The auxiliary agent may be a defoaming agent based on poly-wei chemical, a low-foaming surfactant based on ρ()/Ε〇 block copolymer; wet_such as glutamic acid glycolate, scaly 15 alcohol glycolate , ethoxylated linear alcohols, alkyl benzoate, sodium succinate and contiguous 2-ethylhexanoic acid; biocides such as dithiofee And anti-settling agents such as alginate 14 200804645 and humectants such as urea and chelating agents such as edta and tripolyphosphonic acid. The difference in formula includes demineralized water. The liquid base composition used in accordance with the present invention is further characterized by a true solution which is dissolved in the worst case when stored in a temperature range of up to 5, even after storage for several months in a thoroughly sealed container. The composition is rarely inclined to crystallize. The liquid alkali composition is free-flowing, has low viscosity, and is colorless. It usually has a total dissolved solids content ranging from 35 to 55 to %. The liquid composition used in accordance with the present invention may be added to the dye liquor in an amount of from 1 to gram per liter, depending on the amount of dye applied to the fabric during the dyeing procedure. The amount applied is referred to as the depth of color, and the amount applied indicates the amount of the dye present in the dyebath, expressed as a percentage by weight of the fabric to be dyed. Table 2 provides guidelines for the use of the liquid base compositions of the present invention in a variety of different shade depths, from mild to moderate to severe. 15 Table 2 Hue depth (%) Liquid sorrow - Recommended dose range (g / liter dye bath) 0.5 1.5-4 1.5 3-5 3.0 3.5-6 6.0 4.5-7 ~ 9.0 5.5-9 Liquid used in accordance with the present invention The alkali composition is particularly suitable for depleted batch dyeing of cotton textiles and cellulosic textiles (involving the textile to be dyed completely in the dye solution), but it can also be used at higher concentrations for continuous pressurization 15 200804645 And semi-continuous pressure dyeing applications. For depletion dyeing, liquid to fabric ratio of 1:1 to 2〇1, preferably in the range of 5:1 to 15:1, more preferably in the range of 8:1 to 12:1, and most A typical depletion staining procedure of 10:1 〇' 5 # and the liquid test and temperature-sensitive reactive dye of the present invention (alone or 'i three-color combination) comprises the following general procedure. To dye the fabric into the dye bath, the dye bath liquid contains the required amount of dye and the amount of salt • (chlorinated sodium) or hydrated contact (GlaUber, s) salt to pre-dissolve the two-ion water, typically 30-80 The range of grams / liters. The temperature rises to thief to 6 〇 C 疋 although good salt (sodium chloride) or sodium hydrate hydrate (Gibo's salt) is added to the dye bath, typically in the range of 30·80 g/l. The dye bath is maintained for typically 60 minutes to perform. The dye is "depleted" onto the fabric. Subsequently, the required amount of liquid alkali is added, and the dyeing/kneading is maintained at the set temperature for another 6 minutes to perform dye chemical fixation to the fabric. At the end of this period, the fabric is washed to remove any salt, neutralized with dilute <15 acetic acid, and then washed again in cold and boiling water to remove any unfixed φ dye. The procedure for dyeing with hot dyes is similar, but the bath temperature is typically 8 ° C. The salt concentration added to perform depletion staining is typically in the range of 45-90 g/l. Typically, after scouring or mercerizing In this case, a much larger number of assay solutions according to the invention are used. These amounts are up to 100 g/l or even up to 200 g/l. The invention will be further illustrated by reference to the following examples of the following aqueous alkaline solutions. 16 200804645 • 5 • Formulation A 515.91 g of sodium hydroxide (82% active ingredient) was dissolved in 8 〇 185 g of demineralized water with stirring. Then, 377.83 g of borax pentahydrate (Neobor®, ex B〇rax Europe Limited) was added to the solution and stirred until dissolved. Thus obtained about 1.2 liters of aqueous alkaline solution containing 22.3 wt% borax pentahydrate and 30.4 wt% potassium hydroxide (82%) having a dry solids content of 52.6 wt% 〇 Formulation B 10 396·79 g of hydration Sodium (82% active ingredient) was dissolved in 821.65 grams of demineralized water with stirring. Then, 387.16 g of borax pentahydrate (Nepo, Borax Europe Ltd.) was added to the solution and stirred until dissolved. Thus, about 1.2 liters of an aqueous test solution containing 24.1% by weight of Cinnabar pentahydrate and 24.7 wt% of potassium hydroxide (82%) having a dry solid content measurement of _ 15 47.2% by weight was obtained. • For comparison purposes, use the following as base (C) soda ash (D) Cibatex SA-200 (ex Ciba Speciality Chemicals), a commercially available inorganic test and salt composition 20 contains 10 to 15 wt% potassium hydroxide, 5 to 8 wt% sodium hydroxide and 5 to 10 wt% sodium citrate having a dry solids content of 38.4 wt%. In the case of dyeing experiments using individual dyes, the dye yields indicating the dye is fixed on the fabric to the dye amount after the depletion, fixing, and cleaning steps, using a reflectance spectrophotometer at visible wavelengths 17 200804645 Range measurement. The reflectance measured at the minimum reflectance wavelength is measured relative to the reflectance percentage of the perfect white diffuser to calculate the so-called Kubelka-Munk value K/S using the following equation: K/ S = (100-R) 2 / 200R 5 K / S defines the color yield on the fabric. In the case of a dyeing experiment using a combination of trichromatic dyes, spectrophotometric measurement, based on the CiE color space, yields yield values of Δ£ (total color difference), (light difference), and the difference in hue between the paired results. Example 1 10 Dye·CL Reactive Black No. 5 (Rima Left Black B) A piece of 5 g of scoured and bleached knit cotton fabric was dyed with color index reactive black No. 5 at a liquid ratio of 10:1 to 1· 5% of the tonal depth, using the formula 固定 to fix as follows: In the polypropylene tube of the Rotadyer machine in Roaches, add CI·Reactive Black No. 5 solution (7.5 ml 1 gram) / liter of the backup solution 'equivalent to 1.5% tone depth), gasified sodium solution (12.5 ml 200 g / liter of standby solution, ie 50 g / liter) and water (27 · 0 ml), followed by a piece of 5 grams of scouring And bleached knit cotton fabric. The tube was placed in a Rota Dell machine crying for about 15 minutes and the temperature was raised from room temperature. During the dyeing operation 20, the tube is rotated inside the machine to ensure that the fabric is evenly impregnated by the dye liquor. After 60 minutes at 60 ° C, the machine was stopped to add Formulation A (3 〇 mL 5 克 / liter Formula A stock solution). At this time, the total amount is 5 〇 ml (Lr 1〇: 1). The fixing of the dye was again carried out at 6 (TC for 60 minutes. At the end of this procedure, the dyed fabric was taken out from the dyeing tube 18 200804645 and thoroughly washed in cold tap water for 5 minutes to reduce the salt concentration. The fabric was thoroughly diluted with acetic acid in water. Neutralize, once again wash in cold water (2 minutes), boil in 100 ml of water to remove the loose dye. Finally, rinse in cold water until no more dye is removed. The fabric is about 5 〇. 〇 dry 5 dry ' Datacolor International Spectraflash SF600 spectrophotometer for visual inspection of visible color yield (K/S) 不同 for different concentrations of Formula A, Formula B and for comparison with soda ash and steam Barthes SA-200 repeats this example. Multiple staining experiments were conducted to study the accumulation of reactive black No. 5 on cotton (color yield versus percent tone depth) listed in the table below: ---^ Salt concentration (g/L) %% deep liquid pH K/S ------- Concentration (g/L) Formulation A ------ 2 30 0.5 12.4 6.04 3 50 1.5 12.51 15.60 4 50 3.0 12.55 24.77 5 80 6.0 12.25 34.19 7 80 9.0 12.28 35.27 Square B 3.5 30 0.5 11.69 5.66 5 50 1.5 11.93 14.15 5.5 50 3.0 11.65 24.81 7.5 80 6.0 12.25 33.61 8.5 80 9.0 11.80 34.76 Soda ash (than car) 10 30 0.5 11.34 6.19 15 50 1.5 11.25 16.40 19 200804645

20 50 3.0 11.21 25.46 20 80 6.0 10.88 33.49 20 80 9.0 10.76 35.19 Cibatec SA-200 (Comparative) 2.75 30 0.5 12.01 6.06 3.5 50 1.5 12.05 15.95 4.5 50 3.0 12.07 24.72 6.5 80 6.0 11.97 33.86 6.5 80 9.0 11.45 35.11 The results can be attributed to the fact that the two borate-based liquid base solutions used according to the invention achieve a color yield closely matched to the color yield obtained using soda ash, but at a concentration of only a partial component thereof. The performance is also closely matched to the performance of the Cibatis SA-200, which is supplied by the company. Example 2

Dye: CL Reactive Yellow No. 176 (Rima Left Yellow 3RS) The procedure of Example 1 was repeated to obtain the following results: Salt concentration (g/L) % Hue depth Liquid pH K/S Concentration (g/L) Formulation A 2 30 0.5 11.40 2.32 3.5 50 L5 11.50 7.22 4 50 3.0 12.40 12.78 5 80 6.0 12.45 21.46 6 80 9.0 12.50 24.63 Formulation B 3.5 30 0.5 11.40 2.42 20 200804645 4.5 50 1.5 11.40 7.08 5.5 50 3.0 12.35 12.87 6.5 80 6.0 12.30 21.17 8.5 80 9.0 12.45 24.86 soda ash (comparative) 10 30 0.5 10.80 2.39 15 50 1.5 10.80 6.89 20 50 3.0 11.55 12.48 20 80 6.0 11.45 20.44 20 80 9.0 11.45 23.25 Cibates SA-200 (comparative) 2.75 30 0.5 11.40 2.47 3.5 50 1.5 11.50 7.31 4.5 50 3.0 12.40 13.30 6.5 80 6.0 12.50 22.18 6.5 80 9.0 12.50 25.29

The conclusions obtained using this dye are similar to those obtained in Example 1. The liquid base formula clearly gives a slightly superior color compared to the use of soda ash, and the hue depth is heavier. 5 Example 3 Dyes: C.I. Reactive Red No. 239 (Ivan Left/Rima Left Br. Red 3BS) The procedure of Example 1 was repeated and the following results were obtained: 21 200804645

Salt concentration (g/L) % tone depth liquid pH K/S concentration (dragon/liter) Formulation A 2 30 0.5 12.00 2.79 3.5 50 1.5 12.25 8.84 4 50 3.0 12.25 15.23 5 80 6.0 11.40 26.06 6 80 9.0 11.40 29.73 Formulation B 3.5 30 0.5 12.10 2.95 4.5 50 1.5 12.15 8.67 5.5 50 3.0 12.20 15.06 6.5 80 6.0 11.30 26.10 8.5 80 9.0 11.30 29.28 Soda ash (comparative) 10 30 0.5 11.60 3.01 15 50 1.5 11.50 8.93 20 50 3.0 11.50 16.26 20 80 6.0 10.50 25.30 20 80 9.0 10.40 28.37 Cababats SA-200 (ratio to i) 2.75 30 0.5 12.25 2.90 3.5 50 1.5 12.25 9.70 4.5 50 3.0 12.30 15.55 6.5 80 6.0 11.60 26.30 6.5 80 9.0 1L50 29.96 The conclusions drawn from the use of this dye are similar examples. 1 conclusions obtained. The liquid base formulation clearly gives a slightly superior color compared to the use of soda ash, and the hue 5 is heavier. 22 200804645 Example 4 Dyes: CI·Reactive Yellow No. 84 (Efxin/Pusin Yellow H-E4R) The procedure of Example 1 was repeated, but the temperature used in the depletion and fixation steps was 80 ° C instead of 60. . Get the following results:

Salt concentration (g/L) % tone depth liquid pH K/S concentration (g/l) Formulation A 2 45 0.5 11.25 3.08 3.5 60 1.5 11.50 9.41 4 70 3.0 11.50 16.88 5 90 6.0 11.45 25.61 6 90 9.0 11.45 28.74 Formulation B 3.5 45 0.5 11,35 3.00 4.5 60 1.5 11.40 9.23 5.5 70 3.0 11.40 16.78 6.5 90 6.0 11.20 24.56 8.5 90 9.0 11.50 28.57 soda ash (comparative) 10 45 0.5 10.80 3.21 15 60 L5 10.80 9.59 20 70 3.0 10.75 17.60 20 90 6.0 10.50 26.41 20 90 9.0 10.50 28.71 Cibatec SA-200 (comparative) 2.75 45 0.5 11.40 3.18 3.5 60 1.5 11.50 9.38 4.5 70 3.0 1L55 17.00 6.5 90 6.0 11.60 25.94 6.5 90 9.0 11.50 28.49 23 200804645 The two borate-based liquid bases of the present invention achieve a color yield matching color yield obtained using soda ash but only a partial component of the concentration. The potency closely matches the performance of the commercially available liquid base product Cababates SA-200. • 5 Example 5 - Dye · · CI · Reactive Red No. 141 (Efxin / Pusin Red H-E7B) Repeat the procedure of Example 1, but the temperature used in the depletion and fixation steps is 80 ° C instead of 60 ° C. The following results were obtained: Salt concentration (g/L) % Hue depth Liquid pH K/S Concentration (g/L) Formulation A 2 45 0.5 11.20 3.30 3.5 60 1.5 11.50 10.21 4 70 3.0 11.25 17.87 5 90 6.0 11.20 27.12 6 90 9.0 11.20 30.25 Formulation B 3.5 45 0.5 11.30 3.43 4.5 60 1.5 11.30 10.17 5.5 70 3.0 11.20 17.62 6.5 90 6.0 11.20 27.57 8.5 90 9.0 11.15 31.18 Soda ash (comparative) 10 45 0.5 10.70 3.36 15 60 1.5 10.70 10.25 20 70 3.0 10.70 18.58 20 90 6.0 10.50 28.38 20 90 9.0 10.45 30.92 • _______

24 200804645 Cibatec SA-200 (comparative) 2.75 45 0.5 11.40 3.40 3.5 60 L5 11.40 10.03 4.5 70 3.0 11.35 17.86 6.5 90 6.0 11.40 25.84 6.5 90 9.0 11.30 30.47 From this result, it is concluded that the two types of boric acid based in the present invention The liquid base of the salt can be obtained in a color yield matching the color yield obtained using soda ash but the concentration is only a partial component thereof. When a strong base is added, this type of thermally dyed reactive red dye is easily desorbed, resulting in waste of hydrolysis, reduced degree of fixation, or uneven coloration. For example, if caustic soda is used as the base, it is known that this may occur. This effect was not observed using the liquid alkaline formulation of the present invention. The efficacy of the rotten acid liquid base formulation also closely matches the performance of the commercially available liquid base product Cibatis SA-200. Example 6 10 Dye··Temperature dyeing three-color combination _20% CI Reactive Black No. 5 (Ivan Left/Rima Left Black B), 60% CI·Reactive Yellow No. 176 (Iven Left/Rimalu Yellow) 3RS), 20% CI·Reactive Red No. 239 (Ivan Left/Rima Left Red 3BS) The same salt concentration and alkali concentration are used for various tonal depths, and the procedure of Example i 15 is repeated, but K/s is not calculated. The comparison was made between various liquid alkali product color cloth samples and a soda gray dyeing cloth sample as a control group, and the results were expressed by total color difference ΔΕ, brightness difference AL, and hue difference Ah. Get ^下^结25 200804645 %色配戈"A pair of Su Temple Ding gray formula B to soda ash batbates SA-200 to Su _ Ding ash / Wo △ E △h △L △E △h △L △E Ah △L 0.5 1.08 0.24 1.05 1.25 0.04 1.23 0.99 -0.08 0.86 1.5 0.37 -0.01 0.19 0.44 -0.03 -0.41 0.39 -0.08 0.10 3.0 0.66 -0.07 0.09 0.48 -0.08 0.11 0.87 -0.09 0.38 6.0 0.53 -0.31 -0.34 0.73 -0.06 -0.69 0.88 -0.29 -0.75 9.0 0.86 -0.49 -0.65 1.00 -0.53 -0.82 0.67 -0.22 -0.36 φ All the difference is less than 1 unit, so it is acceptable, and it is not noticeable by visual inspection. The data shows that the liquid The color (hue and brightness) of the base product matched the color obtained with the soda ash control. ' 5 Example 7 Dye: Thermally Dyed Tricolor Dye - 60% CI Reactive Yellow No. 84 (Efsin / Pushin Yellow H -E4R), 25% CI·Reactive Red No. 141 (Efxin/Pusin Red Η·Ε7Β), and 15% CI Reactive Blue No. 171 (Efsin/Pussin, C-H-ER) 0 10 The procedure of Example 6 was repeated, but the depletion and fixation steps were carried out at a temperature of 80 ° C instead of 60 ° C. The following results were obtained. Deep formula Α for soda ash formula B for soda ash batartis SA-200 pair soda ash △E Ah △L △E △h △L ΔΕ △h △L 0.5 0.48 -0.06 0.45 0.73 -0.30 -0.54 0.38 -0.23 0.03 1.5 0.39 0.05 -0.32 0.35 0.07 -0.01 0.50 -0.17 0.20 3.0 0.65 0.12 0.52 0.42 0.05 0.19 0.58 0.20 0.49 6.0 1.20 1.01 0.47 1.46 0.91 1.14 1.14 1.03 031 9·0 2.15 1.99 0.62 1.93 1.82 0.57 1.81 1.71 0.39 26 200804645 The performance of the product is very similar to that of soda ash. The color (hue and brightness) can match the soda ash, but the depth of the hue is higher, and the value of ΛΕ and Ah exceeds 1 unit. I: Simple description of the figure] (none) 5 [Description of main component symbols] (no)

27

Claims (1)

200804645 X. Patent application scope: ! "Water-based secret_Additional domain for the purpose of controlling pH in fabric treatment, the aqueous alkaline solution contains 5 10 15 (1) 9 to 36 wt% selected from the group consisting of metal borates and ammonium salts, or boric acid; and (9) 8 to 35 swims at least - a metal hydroxide, ammonium hydroxide or organic gas oxidation fourth Ammonium. 2' The use of the first aspect of the patent application, wherein the test solution has the following composition, 19 to 36 wt% is selected from the group consisting of pure metal salt and ammonium salt, or acid; (η) 8 to 35 wt % at least one base is a gas, such as a halide, ammonium hydroxide or tetraammonium hydroxide; (iv) optionally a weak acid having a PKa in the range of from 10 to 118, preferably an organic weak acid; (iv) optionally, at most iwt〇/. Auxiliary ingredient; the difference is water. For example, the use of the second item of the patent scope includes the use of a biocide, a decontaminant, a wetting agent, a moisturizer, a chelating agent or a suspending aid as an auxiliary component. 4. The use according to any one of the preceding claims, wherein borax pentahydrate is used as the borate. The use according to any one of the preceding claims, wherein the aqueous test solution has a dissolved solids content of from 35 wt% to 55 wt%. 20 200804645 The use of the item, where the fabric is accepted. For the purpose of addition to reactive dyeing 6. The fabric of any of the foregoing claims is a cellulosic fabric or cotton. 7. The use of the treatment liquid in the application of the scope of claim 6 of the patent application. 'Tour' is used for cellulosic fabric or cotton. 8. The scouring of fabrics as claimed in claim 6 of the patent application. 9. For the purpose of patent application, No. 6 顼 、, a music, for the mercerizing treatment of cellulosic fabrics or cotton fabrics. 10. A method of treating a fabric under test conditions, the method comprising treating a fabric with a treatment liquid having an aqueous test solution added thereto, the aqueous test solution comprising (Ο9 to 36% by weight selected from alkali a borate of a metal borate and ammonium borate, or boric acid; and ((1) 8 to 35 wt% of at least one alkali metal hydroxide, barium hydroxide 15 or tetraammonium hydroxide. 11 · A treatment of cellulosic fabric or cotton fabric a method comprising treating a fabric with a treatment liquid in which an aqueous alkaline solution has been added, the aqueous alkaline solution comprising (1) 9 to 36 wt% of a bismuth citrate selected from the group consisting of alkali metal borate and ammonium borate, or boric acid; And (ii) 8 to 35 wt% of at least one metal hydroxide, hydroxide or tetraammonium hydroxide. 12. A method of fixing a dye to cotton fibers or cellulose fibers, the method comprising applying to cotton Adding 29 to the dyeing treatment liquid of the fabric or cellulose fabric 200804645 kinds of aqueous alkaline solution containing (i) 9 to 36% by weight of borate selected from alkali metal borate and ammonium borate, or boric acid; and (ii) 8 5% by weight of at least one metal hydroxide, ammonium hydroxide or organic ammonium hydroxide. The method of any one of claims 1 to 12, wherein the alkaline solution The following composition (i) 9 to 36 wt% is selected from the group consisting of alkali metal borate and borate ammonium borate, or boric acid; - (ii) 8 to 35 wt% of at least one alkali metal hydroxide, ammonium hydroxide or organic hydroxide a fourth ammonium; (lii) optionally, a weak acid having a pKa in the range of from 1 Torr to 11.8, preferably an organic weak acid; (iv) optionally, up to iwt% of the adjuvant component; the difference being water. The method of claim 13 wherein a biocide, a decontaminant, a wetting agent, a humectant, a chelating agent or a suspending aid is used as an auxiliary component. 15 as claimed in any of claims 10 to 14. The method of any of the preceding claims, wherein the method of any one of claims 10 to 15 wherein the aqueous alkaline solution has a dissolved solids content of from 35 wt% to 55 wt%. 17. If you apply for any of the patent scopes 10 to 16 The method wherein the pH of the treatment liquid is controlled within the range of ι 〇 5 to 12.5. 30 200804645 18. The method of claim 17, wherein the pH is controlled in the range of 11.0 to 12.5. The method of any one of claims 10 to 18, wherein the aqueous alkaline solution is added to the treatment liquid in an amount of from 1 g/liter to 10 g/liter. The method of any one of the items 19, wherein the cotton fabric or cellulosic fabric is dyed in a batch, semi-continuous, continuous or printing process, and the aqueous alkaline solution is added to the dye applied to the fabric Treatment fluid. 10. The method of claim 20, wherein the dye is a reactive dye. 22. A method for scouring a cellulosic fabric or a cotton fabric, the method comprising: in a scouring bath comprising water, a surfactant, and a fabric to be scoured, added as in any one of claims 1 to 5 of the patent application. The water-based alkaline solution 15 defined by the item, and heat treatment. 23. A method of mercerizing a cellulosic fabric or cotton fabric, the method comprising the step of adding an aqueous assay solution as defined in any one of claims 1 to 5 to a mercerizing bath. 31 200804645 VII. Designation of representative representatives: (1) The representative representative of the case is: (). (none) (2) A brief description of the symbol of the representative figure·· 8. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: