Oxygen bleaching and dyeing one-bath liquid and oxygen bleaching and dyeing one-bath short-process dyeing and finishing process for polyester-cotton fabric

Abstract

The invention relates to the technical field of textile printing and dyeing, in particular to oxygen bleaching and dyeing one-bath liquid for polyester-cotton fabric and an oxygen bleaching and dyeing one-bath short-process dyeing and finishing process. The oxygen bleaching dyeing one-bath lotion comprises the following components in percentage by weight: 0.8-3.6% of a composite oxygen bleaching agent; 0.2 to 0.4 percent of a pH buffer system; 0.1 to 0.2 percent of an oxygen bleaching stabilizer; 0.05%-0.1% of a chelating agent; 0.05 to 0.1 percent of a penetrating agent; 0.1 to 0.5 percent of alkali-resistant disperse dye; 0.6 to 1.0 percent of bio-based hydroxy fatty acid ester based peroxyimide; and the balance of deionized water. The composite oxygen bleaching agent comprises hydrogen peroxide and TAED in a molar ratio of 1: (0.3-1). According to the technical scheme provided by the invention, working procedures can be combined, and whiteness and dyeing uniformity of the fabric are considered while water consumption is reduced.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of textile printing and dyeing, and particularly relates to an oxygen bleaching and dyeing one-bath solution for polyester-cotton fabric and an oxygen bleaching and dyeing one-bath short process dyeing and finishing process. BACKGROUND

[0002] Polyester-cotton blended fabric (polyester-cotton fabric) has high strength, wrinkle resistance of polyester and skin-friendly comfort of cotton fiber, and is widely used in the field of textiles such as clothing and home textiles, and is one of the textile fabric categories with the largest use in the current market, and occupies an important position in the textile processing industry.

[0003] In the dyeing and finishing process of polyester-cotton fabric, the cotton component needs to be subjected to oxygen bleaching pretreatment to remove natural impurities and improve whiteness, and then the polyester and cotton components are dyed respectively; the traditional process usually carries out oxygen bleaching and dyeing processes independently in steps, and needs to go through multiple processes such as desizing, scouring, oxygen bleaching, multiple washing, polyester dispersion dyeing, cotton active dyeing, fixing, finishing and the like in sequence. The setting of these step-by-step processes causes a large amount of un-fixed impurities and dye intermediates to remain on the surface of the fabric or in the bath, which not only affects the subsequent processing effect, but also needs to be treated through multiple washing links, thereby increasing the additional burden for product quality assurance.

[0004] Although the traditional step-by-step dyeing and finishing process can complete the processing of polyester-cotton fabric, it has many drawbacks that are difficult to overcome: on the one hand, the step-by-step operation of oxygen bleaching and dyeing needs multiple bath preparation and temperature rising, and oxygen bleaching needs to be heated to a high temperature to ensure bleaching effect, and the dyeing process also needs to maintain different temperature ranges (such as polyester high-temperature dyeing and cotton medium-temperature dyeing), resulting in a large amount of heat energy consumption, and the energy cost of enterprises is high; on the other hand, multiple washing is needed between step-by-step processes to switch process environments, including neutral washing after oxygen bleaching, gradient cooling washing after dyeing and the like, each washing process needs to supplement fresh water resources, and the bath ratio requirement of different processes is high, which further aggravates the consumption of water resources. A large amount of high-energy consumption and high-water consumption operations not only significantly increase the production and operation cost of enterprises, but also produce a large amount of printing and dyeing wastewater with complex components, which is difficult and costly to treat, and easily causes heavy burden on the environment, which is contrary to the current green and environmentally friendly industrial development concept.

[0005] In recent years, with the continuous improvement of global environmental awareness, environmental protection regulations in various countries are becoming increasingly stringent, and higher requirements are put forward for the emission of pollutants, energy consumption control and the like in the textile printing and dyeing industry; at the same time, the prices of energy and water resources continue to rise, which further compresses the profit space of printing and dyeing enterprises. Under this background, it has become an urgent need and research focus in the field of polyester-cotton fabric processing to develop a short process, low-consumption oxygen bleaching and dyeing combined process to replace the traditional high-energy consumption, high-water consumption step-by-step dyeing and finishing scheme.

[0006] In the prior art, relevant researches are mostly focused on combining oxygen bleaching and dyeing processes into one bath process, but most of the schemes have the problem of poor process condition compatibility: the weak alkaline and oxidizing environment required by oxygen bleaching easily destroys the stability of dyes, resulting in limited whiteness improvement of cotton fibers (the whiteness of fabrics after conventional combined process is only about 78% ISO); at the same time, the interaction between oxygen bleaching agent and dye easily causes uneven dyeing of dyes, resulting in poor dyeing uniformity of fabrics (the color difference value ΔE is usually greater than 1.5), which is difficult to meet the processing requirements of high-quality polyester-cotton fabrics; in order to improve the effect, some schemes need to greatly increase the amount of additives, which in turn increases the production cost, or requires special equipment, which is difficult to realize industrialization and popularization.

[0007] Therefore, it is urgent to develop a new short process dyeing and finishing process that can balance the treatment effect, economy and environmental protection, and meet the actual needs of industry development. SUMMARY

[0008] The present application provides an oxygen bleaching and dyeing one-bath liquid for polyester-cotton fabrics and an oxygen bleaching and dyeing one-bath short process dyeing and finishing process. The technical scheme provided by the present application can realize process combination and reduce water consumption while balancing the whiteness and dyeing uniformity of fabrics.

[0009] In a first aspect, the present application provides an oxygen bleaching and dyeing one-bath liquid for polyester-cotton fabrics, which adopts the following technical scheme: An oxygen bleaching and dyeing one-bath liquid for polyester-cotton fabrics, the oxygen bleaching and dyeing one-bath liquid comprises the following components by weight percentage: composite oxygen bleaching agent 0.8-3.6%; pH buffer system 0.2-0.4%; oxygen bleaching stabilizer 0.1-0.2%; chelating agent 0.05-0.1%; penetrating agent 0.05-0.1%; alkali-resistant disperse dye 0.1-0.5%; bio-based hydroxy fatty acid ester-based peroxy imide 0.6-1.0%; the balance is deionized water; the composite oxygen bleaching agent comprises hydrogen peroxide and TAED (tetraacetyl ethylenediamine) in a molar ratio of 1: (0.3-1).

[0010] In the present application, the composite oxygen bleaching agent, the pH buffer system, the oxygen bleaching stabilizer, the chelating agent, the penetrating agent and the alkali-resistant disperse dye are compounded and synergized to construct a medium-low temperature oxygen bleaching and dyeing integrated system, which can not only realize efficient and deep bleaching of cotton fibers, but also ensure uniform dyeing of polyester components, while breaking the limitation of high temperature and high pressure in traditional processes, greatly reducing energy consumption and water consumption.

[0011] Composite oxygen bleaching agent is the core functional component to realize low-temperature oxygen bleaching. Hydrogen peroxide as the basic oxygen source can decompose to generate oxidizing groups to oxidize natural pigments and impurities in cotton fibers, but it needs high temperature above 95°C to play a high-efficiency bleaching role under traditional conditions; TAED as a hydrogen peroxide low-temperature activator, in weak alkaline environment, undergoes nucleophilic substitution reaction with hydrogen peroxide to generate peroxoacetic acid with stronger oxidation, which reduces the effective bleaching temperature of hydrogen peroxide to 60-90°C, avoiding high temperature damage to dye structure; when the molar ratio of the two is controlled at 1:(0.3-1), the activation efficiency and bleaching effect reach the best balance, which not only ensures that the whiteness of cotton fibers meets the standard, but also prevents excessive oxidation of peroxoacetic acid from damaging the fibers.

[0012] The pH buffer system plays a dual role of precise alkali control + stable reaction environment. On the one hand, the pH of the system is stabilized in the range of 8.5-10.5, which is the best pH range for TAED to activate hydrogen peroxide, and is also a suitable environment for alkali-resistant disperse dyes to dye polyester; on the other hand, the acid-base buffering capacity of the buffer system can offset the pH fluctuations during the reaction, avoiding local over-alkaline leading to ineffective decomposition of hydrogen peroxide, or local acid inhibition of bleaching reaction, ensuring that the oxygen bleaching and dyeing processes proceed synchronously and stably.

[0013] The core function of the oxygen bleaching stabilizer is to regulate the decomposition rate of hydrogen peroxide + protect the fibers and dyes. Heavy metal ions in water can catalyze the rapid decomposition of hydrogen peroxide, generating a large amount of hydroxyl radicals, which not only waste oxygen sources, but also damage the cellulose structure of cotton fibers, leading to a decrease in fabric strength, and may also decompose alkali-resistant disperse dyes; the stabilizer can preferentially adsorb these heavy metal ions, inhibit their catalytic effect, and slow down the decomposition rate of hydrogen peroxide, ensuring that the oxidizing groups are released slowly and uniformly, and protecting the dye molecular structure from being damaged.

[0014] Chelating agents are used to eliminate interfering ions + improve system cleanliness. Metal ions in printing and dyeing water can compete with oxygen bleaching stabilizers for binding sites, reducing the stability effect, and can also combine with dye molecules to form insoluble precipitates, which are deposited on the surface of polyester-cotton fabric to form color spots; chelating agents can form stable chelates with these metal ions, completely removing the interference, ensuring the uniformity of the oxygen bleaching reaction and the dispersibility of the dye, and avoiding the occurrence of dyeing defects.

[0015] The role of the penetrating agent is to strengthen the penetration of the dyeing liquid + promote uniform bleaching and dyeing. The hydrophobic end of the penetrating agent is adsorbed on the surface of the polyester-cotton fabric fibers, and the hydrophilic end faces the water phase, reducing the interfacial tension between the fibers and the dyeing liquid, allowing the oxygen bleaching and dyeing bath to quickly penetrate into the internal yarn gaps of the fabric, especially for thick and heavy polyester-cotton fabrics; at the same time, the penetrating agent can promote the uniform distribution of oxidizing groups and dye molecules on the fiber surface, avoiding local insufficient bleaching or dyeing color spots caused by uneven penetration, and improving the appearance consistency of the product.

[0016] Alkali-resistant disperse dyes are the core dyeing components adapted to the alkaline oxygen bleaching environment. Such dyes are stable in structure in a weakly alkaline and weakly oxidative environment and cannot be hydrolyzed or decomposed; the dye molecules are adsorbed on the surface of polyester fibers by van der Waals force and hydrogen bonding and diffuse into the interior of the fibers, and are fixed, and the bleaching process of cotton fibers is carried out synchronously, realizing "one-bath double effect" and simplifying the complicated process of the separate operation of oxygen bleaching and dyeing in the traditional process.

[0017] In the present application, the bio-based hydroxyl fatty acid ester-based peroxy imide is a new type of bio-based low-temperature oxygen bleaching activator, which has both environmental compatibility and reaction specificity due to its bio-based structure (derived from the hydroxyl fatty acid of vegetable oil).

[0018] In the weakly alkaline (pH 8.5-10.5) environment of the oxygen bleaching and dyeing one-bath solution, the imide group of the component can undergo nucleophilic addition reaction with hydrogen peroxide to generate hydroxyl fatty acid ester peroxide, which has 1.8-2.2 times the oxidation of peroxoacetic acid activated by TAED, and has a fast reaction rate, which can quickly oxidize natural pigments, lignin and other impurities in cotton fibers, and increase the fabric whiteness from the traditional 78%-82% ISO to 90% ISO; at the same time, the bio-based ester group structure has good compatibility with alkali-resistant disperse dyes, and will not damage the structure of the dye molecules, avoiding the problem of light dyeing.

[0019] Optionally, the weight percentage of the bio-based hydroxyl fatty acid ester-based peroxy imide is 0.7-0.9%.

[0020] In a specific embodiment, the weight percentage of the bio-based hydroxyl fatty acid ester-based peroxy imide is 0.6%, 0.7%, 0.8%, 0.9%, 1.0%.

[0021] In some specific embodiments, the weight percentage of the bio-based hydroxyl fatty acid ester-based peroxy imide is 0.6-0.7%, 0.6-0.8%, 0.6-0.9%, 0.7-0.8%, 0.7-0.9%, 0.7-1.0%, 0.8-0.9%, 0.8-1.0%, 0.9-1.0%.

[0022] Optionally, the preparation method of the bio-based hydroxyl fatty acid ester-based peroxy imide is specifically as follows: Using ricinoleic acid and methanol, with concentrated sulfuric acid as a catalyst, to prepare ricinoleic acid methyl ester; using phthalimide and dichloromethane, with triethylamine as an acid binding agent, to prepare a phthalimide acyl chloride intermediate; using the ricinoleic acid methyl ester intermediate, the phthalimide acyl chloride intermediate, and triethylamine, to prepare the bio-based hydroxyl fatty acid ester-based peroxy imide.

[0023] Optionally, the one-bath oxygen bleaching and dyeing solution further comprises amphiphilic polyamino acid grafted modified siloxane; the weight percentage of the amphiphilic polyamino acid grafted modified siloxane is 0.2-0.8%.

[0024] Optionally, the weight percentage of the amphiphilic polyamino acid grafted modified siloxane is 0.12-0.18%.

[0025] In a specific embodiment, the weight percentage of the amphiphilic polyamino acid grafted modified siloxane is 0.2%, 0.4%, 0.5%, 0.6%, 0.8%.

[0026] In some specific embodiments, the weight percentage of the amphiphilic polyamino acid grafted modified siloxane is 0.2-0.4%, 0.2-0.5%, 0.2-0.6%, 0.4-0.5%, 0.4-0.6%, 0.4-0.8%, 0.5-0.6%, 0.5-0.8%, 0.6-0.8%.

[0027] The amphiphilic polyamino acid grafted modified siloxane is a new type of leveling-flooding capturing dual functional agent. Its amphiphilic structure (dye-philic polyamino acid segment + fiber-philic siloxane segment) can simultaneously solve the problems of uneven dyeing and residual floating color. The polyamino acid segment combines with alkali-resistant disperse dye molecules through hydrogen bonds to form stable "dye-polyamino acid" inclusions, slowing down the diffusion rate of the dye to the polyester fiber; at the same time, the siloxane segment forms a uniform adsorption layer on the surface of the polyester-cotton fiber, avoiding local over-dyeing of the dye, and controlling the dyeing color difference value ΔE from the traditional 1.2-1.5 to below 0.7. At the same time, the hydrophilic segment of the polyamino acid can disperse the un-fixed floating dye in the bath, avoiding the re-adsorption of the floating color to the fiber surface, reducing the subsequent washing times (from the traditional 2-3 times to 1 time), and reducing the water consumption from 50 tons / ton of cloth to 25 tons.

[0028] Optionally, the preparation method of the amphiphilic polyamino acid grafted modified siloxane is as follows: Carboxyl-terminated polylysine is prepared by using L-lysine and ε-caprolactam, with stannous octoate as a catalyst and adipic acid as an end-capping agent; and the amphiphilic polyamino acid grafted modified siloxane is prepared by using carboxyl-terminated polylysine and amino-modified polydimethylsiloxane, adding EDC·HCl and NHS.

[0029] Optionally, in the composite oxygen bleaching agent, the hydrogen peroxide is a 30% aqueous solution, and the TAED is an industrial-grade powder.

[0030] Optionally, in the composite oxygen bleaching agent, the molar ratio of hydrogen peroxide to TAED is 1: (0.4-0.8).

[0031] Optionally, the pH buffer system is selected from any one or more of a sodium phosphate dibasic-sodium phosphate monobasic buffer pair, a sodium carbonate-sodium bicarbonate buffer pair, a phosphate-carbonate mixed buffer.

[0032] Optionally, the pH buffer system is a sodium phosphate dibasic-sodium phosphate monobasic buffer pair.

[0033] Optionally, the oxygen bleaching stabilizer is selected from any one or more of sodium silicate, a complex organic phosphonate stabilizer, a magnesium salt stabilizer.

[0034] Optionally, the oxygen bleaching stabilizer is sodium silicate.

[0035] Optionally, the chelating agent is selected from any one or more of EDTA, DTPA, sodium citrate.

[0036] Optionally, the chelating agent is EDTA.

[0037] Optionally, the penetrant is selected from any one or more of a non-ionic penetrant JFC, a fatty alcohol polyoxyethylene ether, a sodium fatty acid methyl ester sulfonate.

[0038] Optionally, the penetrant is a non-ionic penetrant JFC.

[0039] In a second aspect, the present application provides a preparation method of an oxygen bleaching dyeing one-bath liquid, which adopts the following technical scheme: A preparation method of an oxygen bleaching dyeing one-bath liquid, the preparation method specifically comprises the following steps: under a stirring rate of 150-200 r / min, a pH buffer system and an oxygen bleaching stabilizer are slowly added into 40-50℃ deionized water with a formulation amount of 70-80%, and stirred for 20-25 min until completely dissolved, so as to ensure that the system pH is stable at 8.5-10.5; a chelating agent and a penetrant are continuously added, and stirred for 15-20 min to be uniformly mixed; then a bio-based hydroxy fatty acid ester-based peroxy imide is slowly added, the stirring rate is increased to 200-250 r / min, and stirred for 15-20 min until completely dispersed; an alkali-resistant disperse dye after pre-beating is slowly dripped, and the stirring rate is maintained at 180-220 r / min, and stirred for 20-25 min until there is no obvious particle in the system; after TAED is dissolved by stirring for 10-15 min, hydrogen peroxide is slowly added in batches under the condition that the system temperature does not exceed 50℃, and the stirring rate is maintained at 180-200 r / min throughout the process, and stirred for 10-15 min; the remaining deionized water is added to the total weight, and stirred for 10-15 min to be uniformly mixed, so as to obtain the oxygen bleaching dyeing one-bath liquid.

[0040] Optionally, the oxygen bleaching and dyeing one-bath solution further comprises amphiphilic polyamino acid grafted modified siloxane; the addition timing is after the dye dispersion and before the hydrogen peroxide addition; specifically: adding the amphiphilic polyamino acid grafted modified siloxane, continuing to stir at a stirring rate of 180-220 r / min for 15-20 min, so that the auxiliary agent and the dye are fully combined to form a stable package; then adding TAED and hydrogen peroxide.

[0041] In a third aspect, the application provides an oxygen bleaching and dyeing one-bath short process dyeing and finishing process using the above-mentioned oxygen bleaching and dyeing one-bath solution, which adopts the following technical scheme: An oxygen bleaching and dyeing one-bath short process dyeing and finishing process using the above-mentioned oxygen bleaching and dyeing one-bath solution, the oxygen bleaching and dyeing one-bath short process dyeing and finishing process specifically comprises the following steps: immersing polyester-cotton gray fabric into a dyeing tank, adding the prepared oxygen bleaching and dyeing one-bath solution, and starting a circulating stirring device; controlling the water temperature to be 60-70℃, maintaining the stirring rate to be 180-200 r / min, and performing oxygen bleaching and dyeing synergistic treatment for 30-60 min; discharging the oxygen bleaching and dyeing one-bath solution, and rinsing once with clean water; dewatering and drying.

[0042] Optionally, the bath ratio in the oxygen bleaching and dyeing one-bath short process dyeing and finishing process is 1:8-1:15.

[0043] Optionally, the oxygen bleaching and dyeing one-bath solution further comprises amphiphilic polyamino acid grafted modified siloxane.

[0044] In summary, the application has at least one of the following beneficial technical effects: The technical scheme provided by the application can realize process combination and reduce water consumption (from 50 tons / ton of fabric to 25 tons / ton of fabric, a reduction of 50%), while taking into account the whiteness and dyeing uniformity of the fabric.

[0045] The core function of the bio-based hydroxy fatty acid ester-based peroxy imide is to enhance the oxygen bleaching efficiency, shorten the reaction time, and improve the fabric whiteness, which is the basic prerequisite for the oxygen bleaching and dyeing one-bath process - if the natural pigments and impurities of cotton fibers are not efficiently removed, the fabric whiteness is insufficient, and subsequent dyeing will have problems such as "dull color development" and "color light deviation"; at the same time, its ability to rapidly activate hydrogen peroxide can compress the basic reaction time of oxygen bleaching + dyeing from 8 h to about 4 h, achieving the preliminary goal of "halving the working hours". In addition, this component only acts on the oxygen bleaching system (reacts with hydrogen peroxide to generate highly active peroxide), does not have strong interaction with dyes or fibers, and can be added alone to stably achieve whiteness improvement without interfering with the addition of subsequent components.

[0046] The core role of the amphiphilic polyamino acid grafted modified siloxane is to optimize dyeing uniformity, capture floating color, and reduce the number of washing processes, and its effect needs to be based on "fabric whiteness meets the standard and oxygen bleaching reaction is sufficient". After the fabric base whiteness is uniform, the polyamino acid segment of the component can precisely wrap the dye molecules, avoid local over-dyeing, reduce ΔE from about 1.2 to below 0.7; at the same time, its floating color capturing capacity can reduce 1 washing process, so that the water consumption is further reduced from 30 tons / ton of cloth to 25 tons / ton of cloth, and finally the four indexes of "working hours, water consumption, whiteness and uniformity" are fully met. DETAILED DESCRIPTION

[0047] Before describing the embodiments of the present application in detail, it should be understood that the terms used herein are for the purpose of describing specific embodiments only. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the term belongs.

[0048] It should be noted that the terms "first", "second" are only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined with "first", "second" can explicitly or implicitly include one or more of the features. Further, in the description of the present application, unless otherwise stated, the meaning of "multiple" is two or more.

[0049] The endpoints of the ranges and any values disclosed in the present application are not limited to the precise values stated. The ranges or values should be construed to be roughly around the ranges or values. For numerical ranges, the endpoints of the various ranges, the endpoints of the various ranges and individual point values, and individual point values can be combined to form one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0050] In the present application, the term "comprising" or "including" is an open-ended expression, i.e. including the contents indicated in the present application, but not excluding other aspects.

[0051] The present application provides an oxygen bleaching dyeing one-bath liquor for reactive dye cotton fabric. The oxygen bleaching dyeing one-bath liquor comprises the following components by weight percentage: composite oxygen bleaching agent 0.8-3.6%; pH buffer system 0.2-0.4%; oxygen bleaching stabilizer 0.1-0.2%; chelating agent 0.05-0.1%; penetrating agent 0.05-0.1%; alkali-resistant disperse dye 0.1-0.5%; bio-based hydroxy fatty acid ester-based peroxy imide 0.6-1.0%; the balance is deionized water; the composite oxygen bleaching agent comprises hydrogen peroxide and TAED in a molar ratio of 1: (0.3-1).

[0052] Further, the oxygen bleaching one-bath solution further comprises amphiphilic polyamino acid grafted modified siloxane; the weight percentage of the amphiphilic polyamino acid grafted modified siloxane is 0.2-0.8%.

[0053] In one specific embodiment, the method of preparing bio-based hydroxy fatty acid ester-based peroxy imide is specifically as follows, and those skilled in the art can further optimize the following scheme to improve the yield and safety.

[0054] (1) Bio-based hydroxy fatty acid methyl esterification: 100 g of ricinoleic acid (bio-based hydroxy fatty acid) is dissolved in 280-320 mL of methanol, and 5-7 g of concentrated sulfuric acid is added as a catalyst; the system temperature is controlled at 68-72°C (methanol refluxing temperature), and the reaction is stirred at 150-200 r / min for 3.5-4.5 h.

[0055] (2) Purification of ricinoleic acid methyl ester: after the reaction is completed, the excess methanol is removed by distillation; 180-220 mL of saturated sodium carbonate solution is added to the remaining liquid, and oscillation is used to neutralize to pH=6.8-7.2, and after the liquid is separated, the water phase (containing sodium sulfate salt) is discarded; the organic phase is dried with 15-20 g of anhydrous sodium sulfate for 2-4 h, and the drying agent is removed by filtration; the filtrate is rotary evaporated at 40-45°C and 0.03-0.05 MPa to obtain a transparent ricinoleic acid methyl ester intermediate.

[0056] (3) Preparation of phthalimide chloride: 50 g of phthalimide is dissolved in 180-220 mL of dichloromethane, 28-32 g of triphosgene is added in 3-5 portions under light shielding conditions, the system temperature is controlled at 20-25°C, and the reaction is stirred at 150-200 r / min for 1-1.5 h; then 8-12 mL of triethylamine is added as an acid binding agent, the temperature is maintained at 20-25°C, and the reaction is stirred for 1.5-2.5 h; after the reaction is completed, the by-product is removed by filtration, and the filtrate is concentrated to 1 / 3-1 / 2 of the original volume under the conditions of 35-40°C and 0.03-0.05 MPa to obtain a phthalimide chloride intermediate.

[0057] (4) Synthesis of bio-based hydroxy fatty acid ester-based peroxy imide: 75-85 g of ricinoleic acid methyl ester is dissolved in 130-170 mL of dichloromethane, 38-42 g of phthalimide chloride and 4-6 mL of triethylamine are added, the system temperature is controlled at 22-27°C, and the reaction is stirred at 150-200 r / min for 2.5-3.5 h.

[0058] (5) Product purification: 90-110 mL saturated brine was added to the reaction solution, and washed for 2-3 times. After standing and separating, the water phase (containing unreacted triethylamine hydrochloride) was discarded. The organic phase was dried with 15-20 g of anhydrous sodium sulfate for 2-4 h, and the drying agent was removed by filtration. The filtrate was concentrated to 1 / 4-1 / 3 of the original volume under the conditions of 35-40 °C and 0.03-0.05 MPa. The concentrated product was slowly dropped into 900-1100 mL of anhydrous ether, and stirred (100-150 r / min) during dropping to promote complete precipitation. The precipitate was collected by filtration, and dried under the conditions of 38-42 °C, 0.02-0.05 MPa and vacuum for 20-26 h to obtain the bio-based hydroxy fatty acid ester-based peroxide imide product.

[0059] In one specific embodiment, the preparation method of the amphiphilic polyamino acid grafted modified siloxane is specifically as follows, and those skilled in the art can further optimize the following scheme to improve the yield and safety.

[0060] (1) Preparation of carboxyl-terminated polylysine: 50 g of L-lysine was dissolved in 80-120 mL of deionized water, 8-12 g of ε-caprolactam was added, and the mixture was stirred until uniform. Then 0.4-0.6 g of stannous octoate was added as a catalyst, and nitrogen was introduced to remove air in the system. The temperature of the system was controlled at 175-185 °C, and the molten polymerization was carried out at 150-200 r / min for 1.5-2.5 h. Then 8-12 g of adipic acid was added as a capping agent, and the temperature was maintained at 175-185 °C, and the stirring reaction was continued for 0.8-1.2 h.

[0061] (2) Purification of carboxyl-terminated polylysine: after the reaction was completed, the product was dissolved in 280-320 mL of anhydrous ethanol after the system was cooled to room temperature, and stirred until completely dissolved. The ethanol solution was slowly dropped into 800-1200 mL of deionized water, and stirred (100-150 r / min) during dropping to promote precipitation of the product. The precipitate was collected by filtration, and the precipitate was placed in a vacuum drying oven under the conditions of 38-42 °C, 0.02-0.05 MPa and vacuum for 20-26 h to obtain the powder of carboxyl-terminated polylysine intermediate.

[0062] (3) Synthesis of polyamino acid grafted modified siloxane: 28-32 g of amino-modified polydimethylsiloxane (amino value 0.3 mmol / g) was dissolved in 90-110 mL of anhydrous ethanol, 18-22 g of carboxyl-terminated polylysine was added, and stirred until uniformly dispersed. Then 4.5-5.5 g of EDC·HCl and 2.8-3.2 g of NHS were added, the temperature of the system was controlled at 33-37 °C, and the stirring reaction was carried out at 150-200 r / min for 5.5-6.5 h.

[0063] (4) Product purification: After the reaction is completed, 80-120 mL of deionized water is added to the system, and the system is washed for 2-3 times by oscillation. After standing and separating, the water phase (containing unreacted EDC-HCl and NHS) is discarded. The organic phase is dried with 15-20 g of anhydrous sodium sulfate for 2-4 h, and the drying agent is removed by filtration. The filtrate is concentrated to 1 / 3-1 / 2 of the original volume under the condition of 35-40°C and 0.03-0.05 MPa. The concentrated product is slowly dropped into 800-1200 mL of n-hexane, and stirring (100-150 r / min) is performed during the dropping to promote complete precipitation. The precipitate is collected by filtration, and vacuum drying is performed at 38-42°C and 0.02-0.05 MPa for 20-26 h to obtain the amphiphilic polyamino acid grafted modified siloxane product.

[0064] The application also provides a preparation method of an oxygen bleaching and dyeing one-bath solution.

[0065] In a specific embodiment, the preparation method of the oxygen bleaching and dyeing one-bath solution specifically comprises the following steps: Under the stirring rate of 150-200 r / min, pH buffer system and oxygen bleaching stabilizer are slowly added to 40-50°C deionized water with the formulation amount of 70-80%, and stirring is performed for 20-25 min until complete dissolution, so as to ensure that the pH of the system is stable at 8.5-10.5. Chelating agent and penetrating agent are continuously added, and stirring is performed for 15-20 min to mix uniformly. Then, bio-based hydroxy fatty acid ester-based peroxy imide is slowly added, the stirring rate is increased to 200-250 r / min, and stirring is performed for 15-20 min until complete dispersion. Alkali-resistant disperse dye pre-beaten is slowly dropped, the stirring rate is maintained at 180-220 r / min, and stirring is performed for 20-25 min until the system has no obvious particles. After TAED is dissolved by stirring for 10-15 min, hydrogen peroxide (molar ratio to TAED is 1:(0.3-1)) is slowly added in batches under the condition that the temperature of the system does not exceed 50°C, the stirring rate is maintained at 180-200 r / min during the whole process, and stirring is performed for 10-15 min. The remaining deionized water is added to the total weight, and stirring is performed for 10-15 min to mix uniformly, so as to obtain the oxygen bleaching and dyeing one-bath solution.

[0066] In another specific embodiment, the preparation method of the oxygen bleaching and dyeing one-bath solution specifically comprises the following steps: At a stirring rate of 150-200 r / min, to 40-50℃ deionized water of 70-80% of the formula amount, pH buffer system, oxygen bleaching stabilizer were added slowly in turn, stirred for 20-25 min until completely dissolved, to ensure that the system pH was stable at 8.5-10.5; continue to add chelating agent, penetrant, stir for 15-20 min to mix evenly; then slowly add bio-based hydroxy fatty acid ester-based peroxy imide, increase the stirring rate to 200-250 r / min, stir for 15-20 min until completely dispersed; slowly drop in pre-pulped alkali-resistant disperse dye, maintain a stirring rate of 180-220 r / min and stir for 20-25 min until the system has no obvious particles; add amphiphilic polyamino acid grafted modified silicone, continue to stir at a stirring rate of 180-220 r / min for 15-20 min, so that the auxiliary agent and the dye are fully combined to form stable encapsulation; after TAED is dissolved by stirring for 10-15 min, hydrogen peroxide (molar ratio to TAED 1:(0.3-1)) is added in batches slowly under the condition that the system temperature does not exceed 50℃, and the stirring rate is maintained at 180-200 r / min during the whole process, and the stirring time is 10-15 min; make up the remaining deionized water to the total weight, stir for 10-15 min to mix evenly, and the oxygen bleaching and dyeing one-bath liquid is obtained.

[0067] The application also provides an oxygen bleaching and dyeing one-bath short process dyeing and finishing process using the above oxygen bleaching and dyeing one-bath liquid. The oxygen bleaching and dyeing one-bath short process dyeing and finishing process specifically comprises the following steps: immersing polyester-cotton gray fabric into a dyeing tank, adding the prepared oxygen bleaching and dyeing one-bath liquid, and starting a circulating stirring device; controlling the water temperature at 60-70℃, maintaining the stirring rate at 180-200 r / min, and performing oxygen bleaching and dyeing synergistic treatment for 30-60 min; discharging the oxygen bleaching and dyeing one-bath liquid, and rinsing once with clean water; dehydration and drying.

[0068] To make the objectives, technical solutions and advantages of the application clearer, the technical solutions in the embodiments of the application will be clearly and completely described below. Based on the embodiments of the application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the application. The embodiments described below are exemplary and are only used to explain the application, and cannot be understood as a limitation on the application.

[0069] If a specific technology or condition is not specified in the embodiments, the technology or condition described in the literature in the art or according to the product manual is used. If the manufacturer of the reagent or instrument is not specified, it is a conventional product that can be obtained by market purchase.

[0070] The application will be further described in detail below in combination with the embodiments and test results.

[0071] Preparation Example 1 The present preparation example provides a bio-based hydroxy fatty acid ester-based peroxy imide.

[0072] The preparation method of the bio-based hydroxy fatty acid ester-based peroxy imide described above specifically comprises the following steps: (1) Bio-based hydroxy fatty acid methyl esterification: 100 g of ricinoleic acid is dissolved in 300 mL of methanol, and 6 g of concentrated sulfuric acid is added as a catalyst; the system temperature is controlled at 70°C (methanol reflux temperature), and the reaction is stirred at 180 r / min for 4 h.

[0073] (2) Methyl ricinoleate purification: after the reaction is completed, the excess methanol is removed by distillation; 200 mL of saturated sodium carbonate solution is added to the remaining liquid, and oscillation is used to neutralize to pH = 6.8-7.2, and after the liquid is separated, the water phase is discarded; the organic phase is dried with 18 g of anhydrous sodium sulfate for 3 h, and the drying agent is removed by filtration; the filtrate is rotary evaporated at 45°C and 0.04 MPa to obtain a transparent methyl ricinoleate intermediate.

[0074] (3) Preparation of phthalimide chloride: 50 g of phthalimide is dissolved in 200 mL of dichloromethane, 30 g of triphosgene is added in 3-5 times under light-proof conditions, the system temperature is controlled at 20-25°C, and the reaction is stirred at 180 r / min for 1 h; then 10 mL of triethylamine is added as an acid binding agent, the temperature is maintained at 20-25°C, and the reaction is stirred for 2 h; after the reaction is completed, the by-product is removed by filtration, and the filtrate is concentrated to 1 / 3-1 / 2 of the original volume under the conditions of 40°C and 0.04 MPa to obtain a phthalimide chloride intermediate.

[0075] (4) Bio-based hydroxy fatty acid ester-based peroxy imide synthesis: 80 g of methyl ricinoleate is dissolved in 150 mL of dichloromethane, 40 g of phthalimide chloride and 5 mL of triethylamine are added, the system temperature is controlled at 25°C, and the reaction is stirred at 180 r / min for 3 h.

[0076] (5) Product purification: 100 mL of saturated brine is added to the reaction liquid, which is washed for 2-3 times by oscillation, and after the liquid is separated, the water phase is discarded; the organic phase is dried with 18 g of anhydrous sodium sulfate for 3 h, and the drying agent is removed by filtration; the filtrate is concentrated to 1 / 4-1 / 3 of the original volume under the conditions of 40°C and 0.04 MPa; the concentrated product is slowly dropped into 1000 mL of anhydrous ether, and stirring is performed during the dropping (120 r / min) to promote complete precipitation; the precipitate is collected by filtration, and vacuum dried at 40°C and 0.04 MPa for 24 h to obtain a bio-based hydroxy fatty acid ester-based peroxy imide product.

[0077] Preparation Example 2 The present preparation example provides a amphiphilic polyamino acid grafted modified siloxane.

[0078] The preparation method of the amphiphilic polyamino acid grafted modified siloxane specifically comprises the following steps: (1) Preparation of carboxyl-terminated polylysine: 50 g of L-lysine is dissolved in 100 mL of deionized water, 10 g of ε-caprolactam is added, and the mixture is stirred until uniform; then 0.5 g of stannous octoate is added as a catalyst, and nitrogen is introduced to remove air in the system; the temperature of the system is controlled at 180°C, and the molten polymerization is stirred at 180 r / min for 2 h; then 10 g of adipic acid is added as a capping agent, and the temperature is maintained at 180°C, and the stirring reaction is continued for 1 h.

[0079] (2) Purification of carboxyl-terminated polylysine: after the reaction is completed, the system is cooled to room temperature, the product is dissolved in 300 mL of anhydrous ethanol, and stirred until completely dissolved; the ethanol solution is slowly added to 1000 mL of deionized water, and stirred (120 r / min) while adding to promote precipitation of the product; the precipitate is collected by filtration, and the precipitate is placed in a vacuum drying oven at 40°C and 0.04 MPa for 24 h to obtain a powder of carboxyl-terminated polylysine intermediate.

[0080] (3) Synthesis of polyamino acid grafted modified siloxane: 30 g of amino-modified polydimethylsiloxane (amino value 0.3 mmol / g) is dissolved in 100 mL of anhydrous ethanol, 20 g of carboxyl-terminated polylysine is added, and stirred until uniformly dispersed; then 5 g of EDC·HCl and 3 g of NHS are added, the temperature of the system is controlled at 35°C, and the stirring reaction is carried out at 180 r / min for 6 h.

[0081] (4) Product purification: after the reaction is completed, 100 mL of deionized water is added to the system, and washed for 2-3 times by shaking, and the water phase is discarded after standing and separating; the organic phase is dried with 18 g of anhydrous sodium sulfate for 3 h, and the drying agent is removed by filtration; the filtrate is concentrated to 1 / 3-1 / 2 of the original volume under the conditions of 40°C and 0.04 MPa; the concentrated product is slowly added to 1000 mL of n-hexane, and stirred (120 r / min) while adding to promote complete precipitation; the precipitate is collected by filtration, and vacuum dried at 40°C and 0.04 MPa for 24 h to obtain the amphiphilic polyamino acid grafted modified siloxane product.

[0082] Example 1

[0083] This example provides an oxygen bleaching and dyeing one-bath solution. The formula is shown in Table 1.

[0084] The preparation method of the above-mentioned oxygen bleaching and dyeing one-bath solution specifically comprises the following steps: At a stirring rate of 180 r / min, a pH buffer system (disodium hydrogen phosphate-sodium dihydrogen phosphate buffer pair), an oxygen bleaching stabilizer (sodium silicate) were slowly added in turn to 75% of deionized water in the formula amount at 55°C, and stirred for 25 min until completely dissolved to ensure that the system pH was stable at 8.5-10.5; a chelating agent (EDTA), a penetrant (non-ionic penetrant JFC) were continuously added, stirred for 20 min and mixed uniformly; then a bio-based hydroxyl fatty acid ester-based peroxy imide was slowly added, the stirring rate was increased to 220 r / min, and stirred for 20 min until completely dispersed; an alkali-resistant disperse dye (disperse blue NP-EB200%, Zhejiang Longsheng) pre-pulped was slowly dripped, a stirring rate of 200 r / min was maintained, and stirred for 20 min until the system had no obvious particles; after the TAED was dissolved by stirring for 15 min, hydrogen peroxide (molar ratio to TAED 1:0.6) was slowly added in batches at a temperature of the system not more than 50°C, and stirred for 10 min at a stirring rate of 200 r / min every 5 min; the remaining deionized water was added to the total weight, stirred for 10 min and mixed uniformly, and the oxygen bleaching one-bath was obtained.

[0085] Table 1 Formulation of the oxygen bleaching one-bath of the examples and preparation examples

[0086] Examples 2-5 The example provides an oxygen bleaching one-bath. The difference between the above example and Example 1 is that the addition amount of the bio-based hydroxyl fatty acid ester-based peroxy imide, which is specifically shown in Table 1. The remaining operation steps are consistent with Example 1.

[0087] Example 6

[0088] The example provides an oxygen bleaching one-bath. The difference between the example and Example 3 is that on the basis of Example 3, amphiphilic polyamino acid grafted modified siloxane is also added, and the addition amount is specifically shown in Table 1; the addition time of the amphiphilic polyamino acid grafted modified siloxane is after the dye dispersion and before the hydrogen peroxide addition; specifically, the amphiphilic polyamino acid grafted modified siloxane is added, and the stirring rate is maintained at 200 r / min to continue stirring for 20 min to make the auxiliary agent and the dye fully combine to form a stable package; then TAED and hydrogen peroxide are added. The remaining operation steps are consistent with Example 3.

[0089] Examples 7-10 The example provides an oxygen bleaching one-bath. The difference between the above example and Example 6 is that the addition amount of the amphiphilic polyamino acid grafted modified siloxane, which is specifically shown in Table 1. The remaining operation steps are consistent with Example 6.

[0090] Example 11

[0091] The present embodiment provides an oxygen bleaching and dyeing one-bath short process dyeing and finishing process using the oxygen bleaching and dyeing one-bath liquid of any of the above embodiments.

[0092] The oxygen bleaching and dyeing one-bath short process dyeing and finishing process specifically comprises the following steps: The polyester-cotton fabric is immersed in the dyeing tank, the prepared oxygen bleaching and dyeing one-bath liquid (bath ratio 1:10) is added, and the circulating stirring device is started; the water temperature is controlled at 60-70℃, the stirring speed is maintained at 180-200r / min, and the oxygen bleaching and dyeing synergistic treatment is performed for 40min; the oxygen bleaching and dyeing one-bath liquid is discharged, and rinsed with clean water once; dewatering and drying are performed.

[0093] Comparative Example 1 The present comparative example provides an oxygen bleaching and dyeing one-bath liquid. The difference from Example 3 is that no bio-based hydroxyl fatty acid ester-based peroxy imide is added, as shown in Table 1. The remaining operation steps are consistent with Example 3.

[0094] Performance detection test The oxygen bleaching and dyeing one-bath liquids of the above examples and comparative examples are detected as follows.

[0095] (I) Production time detection Reference standards: FZ / T 01001-2016 "Textile Dyeing and Finishing Process Preparation General" and GB / T 39271-2020 "Textile Dyeing and Finishing Energy Consumption Calculation Method".

[0096] Test object: polyester-cotton fabric test piece (specification: 100cm long x 50cm wide, 200g / m² in weight, polyester 65% and cotton 35% blended fabric is selected to ensure that the yarn count and density of each batch of fabric are consistent).

[0097] The detection method is as follows: 1. Reference data determination: Take 3 batches of polyester-cotton fabric of the same specification, use the traditional step-by-step dyeing and finishing process (oxygen bleaching (bath ratio 1:18) → hot water washing (bath ratio 1:18) → cold water washing (bath ratio 1:18) → dyeing (bath ratio 1:12) → soaping (bath ratio 1:18) → rinsing 3 times (bath ratio 1:15) → dewatering → drying) for treatment, and record the total time from "fabric into tank" to "drying out of box" of each batch, and take the average value as the reference time of the traditional process (8h).

[0098] 2. Sample preparation: Take 3 batches of polyester-cotton fabric of the same specification as the reference group, and randomly divide them into the experimental group; the experimental group uses the oxygen bleaching and dyeing one-bath liquid of Example 3, and adopts the oxygen bleaching and dyeing one-bath short process of Example 11, and the control group adopts the above traditional step-by-step dyeing and finishing process, and the treatment equipment models and parameters of the two groups of fabric are consistent.

[0099] 3. Testing process: Record the total process time for each batch of fabric in the experimental group and the control group.

[0100] The results are shown in Table 2.

[0101] Table 2. Time Statistics Results

[0102] As shown in Table 2, the oxygen bleaching and dyeing one-bath short process provided in this application, through the design of "process merging, simplified transfer, and reduced rinsing", has achieved the goal of reducing the production time from 8 hours to 2 hours while ensuring the effectiveness of basic processes such as dehydration and drying. The process efficiency has been improved by 75%, which meets the requirements of short-process and high-efficiency dyeing and finishing technology.

[0103] (ii) Water consumption monitoring Reference standards: GB / T 28711-2012 "Water Consumption Quota for Textile Dyeing and Finishing Processes" and FZ / T 01087-2012 "Textiles - Color Fastness Test - Multifiber Applied Fabrics".

[0104] Test subject: Batch of polyester-cotton grey fabric (1kg in weight, with specifications consistent with the grey fabric used for production time testing).

[0105] The detection method is as follows: 1. Sample preparation: An experimental group and a control group were set up, with 1 kg of polyester-cotton grey fabric treated in each group; the experimental group used the oxygen bleaching and dyeing one-bath solution of Example 3 and the oxygen bleaching and dyeing one-bath short-process process of Example 11; the control group was treated with the traditional step-by-step dyeing and finishing process (oxygen bleaching (bath ratio 1:18) → hot water washing (bath ratio 1:18) → cold water washing (bath ratio 1:18) → dyeing (bath ratio 1:12) → soaping (bath ratio 1:18) → rinsing 3 times (bath ratio 1:15) → dehydration → drying); both groups were treated to the qualified standard of fabric whiteness ≥90% ISO.

[0106] 2. Testing process: Record the amount of fresh deionized water used in each process for the experimental group and the control group respectively, and calculate the total water consumption; deduct the residual water in the equipment pipeline during measurement; repeat the test 3 times to ensure that the final fabric performance indicators of the two groups are consistent.

[0107] Calculation method: Water consumption per unit fabric weight (tons / ton of fabric) = Total water consumption (L) ÷ Dry weight of fabric (kg) ÷ 1000; The average value of 3 tests was taken for the experimental group.

[0108] Statistics show that the oxygen bleaching and dyeing one-bath short-process technology provided in this application, through its design of "combining processes, simplifying transfer, and reducing rinsing," can effectively save water, reducing water consumption from 50 tons / ton of fabric in the traditional process to 25 tons / ton of fabric. The one-bath short-process technology of this application meets the requirements for highly efficient dyeing and finishing technology.

[0109] (Three) Fabric whiteness detection Reference standard: GB / T 8424.2-2001 Instrumental determination of relative whiteness of textiles, ISO 105-J02:1997 Instrumental determination of whiteness of textiles.

[0110] Test object: T / C fabric test piece after one-bath process of oxygen bleaching and dyeing (specification: 5 cm long x 5 cm wide, avoiding selvedge, defects and dyeing color area), T / C fabric test piece after traditional step-by-step dyeing and finishing process.

[0111] The detection method is as follows: 1. Reference data determination: select T / C gray fabric test piece without bleaching and dyeing treatment, test its initial whiteness value, take the average value as the blank reference; at the same time, use T / C fabric test piece treated by traditional oxygen bleaching process as positive control to verify the accuracy of the test system.

[0112] 2. Sample preparation: place the test piece after dyeing and finishing in the experimental group in the standard atmospheric environment (temperature 20±2℃, relative humidity 65±4%) for 24h to ensure consistent moisture content of the fabric.

[0113] 3. Test process: use ISO whiteness meter (model: Datacolor 650), set light source D65, field angle 10°, test the whiteness value of the test piece respectively; select 3 different test points for each test piece to avoid test deviation; record all test data. Calculation method: take the average value of each test point of the test piece as the fabric whiteness value.

[0114] (Four) Dyeing uniformity detection Reference standard: GB / T 15618-2006 Textiles-determination of staining using grey scale, ISO 105-J03:2017 Textiles-determination of colour difference.

[0115] Test object: T / C dyed fabric treated by one-bath process of oxygen bleaching and dyeing (specification: 100 cm long x 50 cm wide, grammage 200 g / m²), T / C fabric test piece treated by traditional step-by-step dyeing and finishing process.

[0116] The detection method is as follows: 1. Reference data determination: select the standard reference area of the dyed fabric (located in the center area of the fabric, specification 5 cm x 5 cm, color light uniform without defects), use the spectrophotometer to test its CIE L*a*b* value as the color difference calculation reference.

[0117] 2. Sample preparation: Place the dyed fabric in a standard atmospheric environment for 24 h, and randomly select 5 test areas (including the center and the four corners) on the fabric (each test area is 3 cm x 3 cm in size, and the reference area is avoided).

[0118] 3. Test process: Use a spectrophotometer (model: X-Rite Ci7800), set the light source to D65 and the field angle to 10°, and test the CIE L*a*b* values of the 5 test areas, respectively; repeat the test 3 times for each test area, and take the average value.

[0119] (Five) Dyeing color fastness detection Reference standard: GB / T 3921-2008 "Textile Color Fastness Test Soaping Fastness", GB / T 3920-2008 "Textile Color Fastness Test Rubbing Fastness", GB / T 250-2008 "Textile Color Fastness Test Gray Sample Card for Evaluating Color Change".

[0120] Test object: Terylene-cotton dyed fabric test pieces treated by one-bath oxygen bleaching and dyeing process (cut into standard samples, soaping fastness sample size: 10 cm x 4 cm; rubbing fastness sample size: 20 cm x 5 cm), and terylene-cotton fabric test pieces treated by traditional step-by-step dyeing and finishing process.

[0121] The detection method is as follows: 1. Sample preparation Soaping fastness sample: align and sew the test sample with the cotton fiber standard lining fabric (size 10 cm x 4 cm) to make a soaping test combination sample; rubbing fastness sample: fix the test sample flat on the sample loading table of the rubbing instrument, ensuring no wrinkles.

[0122] 2. Test process Soaping fastness: place the combination sample in the soaping fastness tester, set the conditions: temperature 40℃, bath ratio 1:50, time 30 min; after the test, take out the combination sample, separate the test sample and the lining fabric, and dry them in a 50±3℃ oven; Rubbing fastness: use the rubbing fastness instrument, set the pressure to 9N, and test dry rubbing and wet rubbing (rubbing cloth water content 100%) for 10 times, then take off the rubbing cloth and dry it.

[0123] 3. Rating process: use the gray sample card for evaluating color change to evaluate the color change grade of the test sample, and use the gray sample card for evaluating staining to evaluate the staining grade of the lining fabric / rubbing cloth; repeat each group of tests 5 times, and take the average grade.

[0124] Calculation method: the color fastness grade is the average grade of 5 tests (the higher the grade, the better the performance, 1st grade is the worst, and 5th grade is the best).

[0125] (VI) Fabric breaking strength detection Reference standard: GB / T 3923.1-2013 Textiles Determination of tensile properties of fabrics Part 1: Breaking force and elongation at break (strip method).

[0126] Test object: T / C fabric strip before dyeing and finishing, T / C dyed fabric (5 groups in warp direction and 5 groups in weft direction, each group with a size of 20 cm in length and 5 cm in width, clamping distance of 10 cm) after oxygen bleaching and dyeing in one bath process, and T / C fabric sample after traditional step-by-step dyeing and finishing process.

[0127] The detection method is as follows: 1. Sample preparation: 5 groups of warp and weft strips are respectively cut from T / C fabric before dyeing and finishing and fabric after dyeing and finishing; all the strips are placed in a standard atmospheric environment for 24 h to ensure consistent moisture content.

[0128] 2. Test process: an electronic fabric strength machine is used to test the breaking strength of each group of strips at a stretching speed of 100 mm / min and a clamping distance of 10 cm; the average breaking strength of the T / C fabric strip before dyeing and finishing and the average breaking strength of the fabric strip after dyeing and finishing are recorded.

[0129] 3. Calculation method: the strength retention rate in the warp and weft directions is respectively calculated.

[0130] The detection results are shown in Table 3.

[0131] Table 3 Detection results

[0132] As shown in Table 3, the scheme of Examples 1-10 all contains a bio-based peroxy imide, and the detection results show that the whiteness is ≥90% ISO; Comparative Example 1 does not contain the component, and the whiteness is <90% ISO. In addition, the ΔE of Examples 6-10 is significantly reduced (<0.7) after adding the amphiphilic auxiliary agent; the ΔE of Examples 1-5 is close to the critical value, and the ΔE of Comparative Example 1 is higher than 0.7. Moreover, due to the capture of floating color by the amphiphilic auxiliary agent, the color fastness of Examples 6-10 is improved to level 4.5; Comparative Example 1 does not have the core functional component, and the color fastness is only level 3.

[0133] The oxygen bleaching and dyeing one-bath short process (60-70°C) provided by the application has small damage to the fabric fiber, and the breaking strength retention rate of Examples 1-10 is ≥85%; the breaking strength of Comparative Example 1 is <85% due to poor process stability.

[0134] In the description of the specification, the description of the terms "one embodiment", "some embodiments", "example", "specific example" or "some examples" etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are contained in at least one embodiment or example of the present application. In the description of the specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any appropriate manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine the different embodiments or examples described in the specification and the features of the different embodiments or examples without contradiction.

[0135] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solution deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A one-bath oxygen bleaching and dyeing solution for polyester-cotton fabrics, characterized in that, The oxygen bleaching and staining one-bath solution comprises the following components by weight percentage: 0.8-3.6% compound oxygen bleaching agent; pH buffer system 0.2-0.4%; Oxygen bleaching stabilizer 0.1-0.2%; chelating agent 0.05-0.1%; penetrant 0.05-0.1%; alkali-resistant disperse dye 0.1-0.5%; bio-based hydroxy fatty acid ester peroxyimide 0.6-1.0%; balance is deionized water; the composite oxygen bleaching agent includes hydrogen peroxide and TAED in a molar ratio of 1:(0.3-1).

2. The oxygen bleaching and staining one-bath solution according to claim 1, characterized in that, The bio-based hydroxy fatty acid ester peroxyimide has a weight percentage of 0.7-0.9%.

3. The oxygen bleaching and staining one-bath solution according to claim 1, characterized in that, The specific preparation method of the bio-based hydroxy fatty acid ester peroxyimide is as follows: methyl ricinoleate is prepared using ricinoleic acid and methanol, with concentrated sulfuric acid as a catalyst; phthalimide chloride intermediate is prepared using phthalimide and dichloromethane, with triethylamine as an acid-binding agent; and bio-based hydroxy fatty acid ester peroxyimide is prepared using the methyl ricinoleate intermediate, the phthalimide chloride intermediate, and triethylamine.

4. The oxygen bleaching and staining one-bath solution according to claim 1, characterized in that, The oxygen bleaching staining solution also includes amphiphilic polyamino acid-grafted modified siloxanes; the weight percentage of the amphiphilic polyamino acid-grafted modified siloxanes is 0.2-0.8%. Optionally, the weight percentage of the amphiphilic polyamino acid grafted modified siloxane is 0.12-0.18%.

5. The oxygen bleaching and staining one-bath solution according to claim 4, characterized in that, The specific preparation method of the amphiphilic polyamino acid grafted modified siloxane is as follows: using L-lysine and ε-caprolactam, with stannous octoate as a catalyst and adipic acid as a capping agent, carboxyl-capped polylysine is prepared; using carboxyl-capped polylysine and amino-modified polydimethylsiloxane, EDC·HCl and NHS are added to obtain the amphiphilic polyamino acid grafted modified siloxane.

6. The oxygen bleaching and staining one-bath solution according to claim 1, characterized in that, In the composite oxygen bleaching agent, hydrogen peroxide is a 30% aqueous solution, and TAED is an industrial-grade powder; Optionally, in the composite oxygen bleaching agent, the molar ratio of hydrogen peroxide to TAED is 1:(0.4-0.8). Optionally, the pH buffer system is selected from any one or more of the following: disodium hydrogen phosphate-sodium dihydrogen phosphate buffer pair, sodium carbonate-sodium bicarbonate buffer pair, and phosphate-carbonate mixed buffer. Optionally, the pH buffer system is a disodium hydrogen phosphate-sodium dihydrogen phosphate buffer pair; Optionally, the oxygen bleaching stabilizer is selected from any one or more of sodium silicate, composite organophosphonate stabilizers, and magnesium salt stabilizers; Optionally, the oxygen bleaching stabilizer is sodium silicate; Optionally, the chelating agent is selected from any one or more of EDTA, DTPA, and sodium citrate; Optionally, the chelating agent is EDTA; Optionally, the penetrant is selected from any one or more of the following: nonionic penetrant JFC, fatty alcohol polyoxyethylene ether, and sodium fatty acid methyl ester sulfonate; Optionally, the penetrant is a nonionic penetrant JFC.

7. A method for preparing a one-bath oxygen bleaching staining solution according to any one of claims 1-3, characterized in that, The preparation method specifically includes the following steps: At a stirring rate of 150-200 r / min, slowly add a pH buffer system and an oxygen bleaching stabilizer sequentially to 70-80% of the formulation amount of deionized water at 40-50℃, stirring for 20-25 min until completely dissolved, ensuring the pH of the system remains stable at 8.5-10.5; continue adding a chelating agent and a penetrant, stirring for 15-20 min to mix evenly; then slowly add a bio-based hydroxy fatty acid ester peroxyimide, increasing the stirring rate to 200-250 r / min, stirring for 1 minute... Add the pre-mixed alkali-resistant disperse dye dropwise for 5-20 minutes until completely dispersed; then slowly add the pre-mixed alkali-resistant disperse dye dropwise, maintaining a stirring speed of 180-220 r / min for 20-25 minutes until the system is free of obvious particles; add TAED and stir for 10-15 minutes to dissolve, then slowly add hydrogen peroxide in batches at a system temperature not exceeding 50℃, maintaining a stirring speed of 180-200 r / min for 10-15 minutes throughout the process; add the remaining deionized water to the total weight, and stir for 10-15 minutes to mix evenly to obtain the oxygen bleaching and dyeing one-bath solution.

8. The preparation method according to claim 7, characterized in that: The oxygen bleaching and dyeing one-bath solution also includes amphiphilic polyamino acid grafted modified siloxane; the timing of addition is after the dye is dispersed and before the addition of hydrogen peroxide; specifically: add amphiphilic polyamino acid grafted modified siloxane, maintain a stirring speed of 180-220 r / min and continue stirring for 15-20 min to allow the auxiliaries and dyes to fully combine and form stable inclusions; then add TAED and hydrogen peroxide.

9. A one-bath short-process dyeing and finishing process for oxygen bleaching and dyeing using the soaping solution according to any one of claims 1-3, characterized in that, The oxygen bleaching and dyeing one-bath short-process dyeing and finishing process specifically includes the following steps: immersing the polyester-cotton grey fabric in the dyeing tank, adding the prepared oxygen bleaching and dyeing one-bath solution, and starting the circulating stirring device; controlling the water temperature at 60-70℃, maintaining the stirring rate at 180-200r / min, and performing oxygen bleaching and dyeing synergistic treatment for 30-60min; draining the oxygen bleaching and dyeing one-bath solution, rinsing once with clean water; dehydrating and drying.

10. The oxygen bleaching and dyeing one-bath short-process dyeing and finishing process according to claim 9, characterized in that, The oxygen bleaching and staining bath solution also includes amphiphilic polyamino acid grafted modified siloxane.

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