Normal-temperature disperse dye low-bath-ratio dyeing auxiliary composition and application process thereof

Abstract

The invention relates to the field of dyeing auxiliaries, and provides a normal-temperature disperse dye low-bath-ratio dyeing auxiliary composition and a process thereof. The auxiliary agent is composed of a multi-block polyether nonionic surfactant, an alkyl amido betaine ampholytic surfactant, a composite organic solvent phase composed of N-acetylmorpholine / propylene glycol phenyl ether / C2-C4 alkyl benzoate, C8-C12 fatty alcohol phosphate, an organosiloxane emulsion and a pH adjusting component, and all the components and the ratio are synergistically optimized. By adopting the auxiliary agent, under a two-stage normal temperature-micro heating dyeing process with the bath ratio of 1: (2-3.5) and the highest temperature not higher than 42 DEG C, the dye uptake and dry and wet rubbing fastness close to those of a conventional high-temperature and high-pressure process can be obtained, the dispersion stability and leveling property of a dye bath are remarkably improved, and foaming, water consumption and energy consumption are reduced.

Description

Technical Field

[0001] This invention relates to the technical field of dyeing and printing auxiliaries, and in particular to a low-liquor-ratio dyeing auxiliary composition for room-temperature disperse dyes and its application process. Background Technology

[0002] Conventional dyeing of polyester fibers with disperse dyes typically employs high-temperature, high-pressure processes, generally requiring temperatures above 120°C to ensure that dye molecules overcome the glass transition temperature of the polyester and diffuse smoothly into the fiber interior. While this type of process achieves high dye uptake, it generally suffers from high energy consumption, demanding equipment requirements, high water and steam consumption, and long process cycles, hindering energy conservation, emission reduction, cost reduction, and efficiency improvement. Furthermore, to enhance the affinity of disperse dyes for polyester at lower temperatures, existing technologies often incorporate large amounts of aromatic carrier solvents or high-boiling-point polar solvents. These carriers typically have strong odors and poor biodegradability, easily leading to harsh operating environments and increased wastewater treatment burdens.

[0003] To meet the production demands of low liquor ratios, rapid dyeing, and energy conservation, the industry has proposed disperse dyeing schemes under normal or medium temperature conditions in recent years. These schemes attempt to achieve polyester dyeing below 40°C by increasing surfactant content, introducing composite solvents, or using special auxiliary agent systems. However, these normal or medium temperature dyeing systems still have many shortcomings under low liquor ratio conditions: on the one hand, high-concentration disperse dyes are prone to particle flocculation and sedimentation in the 20–40°C range, leading to unstable dye baths, noticeable color variations, and localized color spots; on the other hand, the ratios of traditional dispersants and leveling agents are mostly empirical combinations, and the proportions of nonionic, anionic, and amphoteric surfactants have not been systematically optimized for low liquor ratios and high shear cycle conditions, easily resulting in problems such as excessive foaming, significant re-adhesion, dull color, or poor batch reproducibility.

[0004] Therefore, there is an urgent need for a disperse dyeing auxiliary composition and a matching dyeing process that can maintain high dispersion stability, high dyeing rate, low foaming, good leveling properties and low odor burden under normal or near-normal temperature conditions, especially under low liquor ratio conditions. Summary of the Invention

[0005] The purpose of this invention is to overcome the above-mentioned problems existing in the prior art and provide a low-liquor-ratio dyeing auxiliary composition for room temperature disperse dyes and its application process. This composition enables disperse dyes to maintain high dispersion stability and high dyeing efficiency in the low temperature range of 20-40℃ and under low liquor ratio conditions of 1:2-3.5. At the same time, it significantly reduces the risk of dye bath bubbling, color unevenness and back-staining, improves dyeing reproducibility, and achieves dyeing depth and color fastness close to that of conventional high temperature dyeing without relying on high temperature and high pressure equipment and high carrier usage.

[0006] To achieve the above objectives, a first aspect of the present invention provides a room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition, comprising the following components by weight: 15–35 parts of multi-block polyether nonionic surfactant; 5–12 parts of alkylamide betaine amphoteric surfactants; 20–35 parts of composite organic solvent phase; 2 to 6 parts of phosphate ester compounds; 0.3–1.5 parts organosiloxane emulsion; 0.5–3 parts pH adjustment component; The remainder is water; The multi-block polyether nonionic surfactant is a polyether with alternating propoxy and ethoxy units, a total number of alkyl oxy units of 10 to 40, a mass fraction of ethoxy units of 45 to 65 wt%, a number average molecular weight of 1500 to 4500, an HLB value of 11 to 14 in a 1 wt% aqueous solution, and a cloud point of 38 to 50 °C. The alkyl group of the alkylamide betaine amphoteric surfactant is a C12-C18 straight-chain or branched alkyl group. The composite organic solvent phase is composed of N-acetylmorpholine, propylene glycol phenyl ether and C2-C4 alkyl benzoate, with a mass ratio of 1:(0.7-1.3):(0.7-1.3). When the composite organic solvent phase is mixed with water at a volume ratio of 1:4 at 25°C, it forms a single-phase water-soluble system with a turbidity value not higher than 50 NTU.

[0007] As a further improvement of the present invention, the mass ratio of the multi-block polyether nonionic surfactant to the alkylamide betaine amphoteric surfactant is 2:(0.5-1.2).

[0008] Nonionic polyether provides the main dispersion and dissolution, while amphoteric betaine supplements the interfacial activity and provides antistatic and anti-reflocculation functions. The two form a composite micelle that can stably encapsulate dispersed dye particles under low liquor ratio and high shear cycling conditions, while maintaining low foaming and easy washing of the system. If the proportion of amphoteric surfactant is too low, it cannot sufficiently suppress the electrostatic attraction and hydrophobic aggregation between dye particles; if the proportion is too high, it will enhance the foaming of the system and the hydrophilicity of the fibers, resulting in increased re-staining and darkening of the color.

[0009] Therefore, within this ratio range, multi-block polyether nonionic surfactants and alkylamide betaine amphoteric surfactants solve the problems of excessive foaming, insufficient dispersion power, and unstable leveling properties when using traditional surfactants.

[0010] As a further improvement of the present invention, the phosphate ester compound is one or more of the phosphate monoesters and / or diesters of C8-C12 fatty alcohols and / or their polyoxyethylene ethers and their neutral salts.

[0011] C8-C12 aliphatic chain phosphate esters possess sufficient hydrophobicity to be compatible with polyester fiber surfaces, while also providing strong wetting and penetration capabilities through their phosphate groups. This allows them to rapidly reduce the interfacial tension between the fiber and dye liquor at lower temperatures, promoting uniform spreading and penetration of the dye bath into the fiber under low liquor ratio conditions. Their polyoxyethylene ether structure synergizes with multi-block polyethers, enhancing the charge and steric stability of the dispersed particles. Compared to traditional alkylbenzene sulfonates, phosphate esters exhibit lower foaming, better resistance to electrolytes and high-concentration dyes, and are less prone to severe precipitation or turbidity with amphoteric surfactants. Therefore, they can maintain a stable, transparent or semi-transparent dye bath even under high-concentration disperse dyes and low liquor ratio conditions, reducing color variations and deposition spots.

[0012] Therefore, the limitation of this specific type of phosphate ester and its chain length range enables the auxiliary agent to take into account the properties of penetration, leveling and low foaming when dyeing at room temperature and low liquor ratio, and specifically solves the technical contradictions of insufficient wetting and difficult foam control in the existing system.

[0013] As a further improvement of the present invention, the organosiloxane emulsion is an aqueous emulsion of polydimethylsiloxane or polyether-modified polydimethylsiloxane.

[0014] Polydimethylsiloxane has extremely low surface tension and excellent lubricity. Under dyeing conditions with low liquor ratio and high circulation speed, it can significantly reduce the coefficient of friction between fibers and between fibers and the inner wall of the dyeing vat, reduce creases, fuzz and mechanical damage, and improve the smoothness and abrasion resistance of dyed fabrics. At the same time, its low foaming and defoaming properties help to suppress the foaming tendency of the system caused by amphoteric surfactants and dispersants.

[0015] Polyether-modified polydimethylsiloxane, while maintaining the lubricity of siloxane, improves the compatibility of emulsions in aqueous phases and surfactant systems by introducing hydrophilic polyether segments, avoiding the problems of easy oil floating and sticking to rollers that occur with traditional silicone oils during dyeing, and suppressing defects such as silicone spots and oil spots.

[0016] By limiting the siloxane structure to the two types mentioned above, the operation window of the low liquor ratio room temperature dyeing process and the appearance and feel quality of the finished product are further improved while ensuring the stability of the dye bath system and the absence of surface defects. This makes up for the shortcomings of the existing auxiliary agent system, which relies only on organic solvents and ordinary wetting agents and ignores the synergistic effect of lubrication and anti-foaming.

[0017] As a further improvement of the present invention, the pH adjusting component is selected from one or more of sodium acetate, ammonium acetate, sodium formate, 2-hydroxy-2-methylpropanesulfonic acid and its sodium salt.

[0018] As a further improvement of the present invention, the mass ratio of the multi-block polyether nonionic surfactant, the alkylamide betaine amphoteric surfactant and the composite organic solvent phase is 1:0.25-0.5:0.8-1.6.

[0019] Within this ratio range, nonionic polyether serves as the skeleton to provide the micelle core, and the composite organic solvent phase forms a microemulsion-like solvation core with it. Alkyl amide betaine is mainly distributed in the interface layer. The three work together to form a stable dye carrier structure, so that high-concentration disperse dyes can still maintain fine particle size and good dispersion under low bath ratio and room temperature conditions, without significant sedimentation or adhesion to the tank wall.

[0020] If the amount of composite organic solvent is too low, it will be difficult to fully dissolve and swell the dispersed dye microcrystals at room temperature, resulting in insufficient driving force for dyeing. If the amount is too high, it will lead to excessive solvation of the system, increasing costs and odor burden, and may even cause excessive swelling of the polyester, resulting in decreased strength or dimensional instability. This range was determined under the multi-objective balance of dyeing depth, levelness, environment, and cost, resolving the contradiction in traditional systems where pursuing dyeing depth results in the use of excessive carriers, leading to a decrease in environmental friendliness, while pursuing environmental friendliness results in insufficient dyeing depth.

[0021] As a further improvement of the present invention, in the composite organic solvent phase, N-acetylmorpholine, propylene glycol phenyl ether and C2-C4 alkyl benzoate each account for 20-45 wt% of the total mass of the composite organic solvent phase, and the mass fraction of N-acetylmorpholine is greater than or equal to the mass fraction of propylene glycol phenyl ether.

[0022] By limiting the content of N-acetylmorpholine, propylene glycol phenyl ether, and C2-C4 alkylbenzoate in the composite organic solvent phase to 20-45 wt%, and ensuring that the mass fraction of N-acetylmorpholine is not less than that of propylene glycol phenyl ether, a stable single-phase structure can be formed in the ternary solvent system at room temperature. This avoids microphase separation caused by component imbalance, thereby maintaining the dissolution-dispersion state of disperse dyes at the molecular level. This window significantly improves the dye retention ability of the composition under low liquor ratio conditions, improves the dyeing rate and color unevenness, and allows the composition to maintain excellent room temperature dispersion and leveling properties within the temperature range of 25-40°C.

[0023] As a further improvement of the present invention, the mass ratio of the multi-block polyether nonionic surfactant to the phosphate ester compound is (4-8):1.

[0024] Within this range, nonionic polyethers provide the main dispersion and dissolution capabilities, ensuring that disperse dye particles are stably coated; phosphate esters participate in the interfacial layer competitive adsorption at a lower proportion, moderately reducing the interfacial tension between the fiber and the dye liquor and improving penetration, while avoiding electrolyte sensitivity, increased foaming, or complex compatibility issues with amphoteric betaines due to excessive anions.

[0025] When the polyether:phosphate ester mass ratio is below 4:1, excess phosphate ester significantly increases system foaming and weakens the dispersing effect of polyether, easily causing increased staining. When the ratio is above 8:1, the phosphate ester content is insufficient to achieve effective wetting, penetration, and leveling effects, easily leading to uneven coloring under low liquor ratio conditions. Therefore, this ratio range allows the auxiliaries to improve leveling and tolerance to process fluctuations while ensuring high dyeing rates, especially at low liquor ratios of 1:2 to 3.5, still achieving uniform and full color.

[0026] A second aspect of the present invention provides a disperse dyeing process for the room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition as described above, comprising the following steps: (1) Add water, disperse dye and dyeing auxiliary agent composition to the dyeing equipment, adjust the pH of the dye bath to 4.2 to 5.5, make the amount of disperse dye in the dye bath 0.5 to 8 g / L, the amount of auxiliary agent composition 3 to 8 g / L, control the dye bath ratio to 1:2 to 3.5, and stir evenly at 20 to 25℃ to obtain the initial dye bath; (2) Add polyester filament, polyester staple fiber or its fabric to the initial dye bath obtained in step (1) and perform first-stage cyclic dyeing at 20-25°C for 5-15 minutes. (3) Under the condition of keeping the liquor ratio constant, the dye bath temperature is raised to 35-40℃ at a heating rate of 0.5-1.0℃ / min, and the second stage of cyclic dyeing is carried out within the range of 35-40℃ for 20-40min. The highest dyeing temperature in the entire dyeing process shall not exceed 42℃. (4) After draining the dye bath, the dyed fiber material obtained in step (3) is subjected to water washing, reduction cleaning, soap washing, rinsing with clean water and drying treatment in sequence.

[0027] This process achieves full dissolution, dispersion, and initial adsorption of dyes and auxiliaries at room temperature (first stage), and then raises the system temperature to a micro-heating range of 35-40°C at a relatively slow heating rate (second stage). By utilizing the dyeing auxiliary composition, the disperse dyes are continuously and orderly migrated and fixed into the interior of the polyester fibers without relying on traditional high temperature and high pressure (e.g., 130°C), thereby achieving dyeing rate and color fastness close to or even reaching that of conventional high temperature disperse dyeing.

[0028] Controlling the liquor ratio at 1:2 to 3.5 significantly reduces water consumption and emissions. However, in traditional systems, such a low liquor ratio often leads to excessively high dye concentration in the bath, uneven dyeing in certain areas, and severe color bleeding. The process of this invention, through its combination with the auxiliary agent system of this invention, utilizes the synergistic improvement in dispersion stability and interfacial wettability to effectively suppress color bleeding and re-staining under low liquor ratio and low temperature conditions, making low liquor ratio room temperature dispersion dyeing a feasible process route. Compared with existing dispersion dyeing processes that rely on high-temperature and high-pressure equipment, high carrier content, or large liquor ratios, this process reduces energy consumption and environmental burden while still maintaining dyeing uniformity, color fastness, and fiber properties.

[0029] The present invention, by adopting the above technical solution, has the following beneficial effects: (1) This invention constructs an auxiliary system consisting of a multi-block polyether nonionic surfactant, an alkylamide betaine amphoteric surfactant, a specific composite organic solvent phase, a phosphate ester compound with a C8-C12 chain length, an organosiloxane emulsion, and a specific pH adjustment component, and combines it with a disperse dye dyeing process that controls the maximum dyeing temperature to be no higher than 42°C, thereby achieving efficient dyeing of polyester fibers in a low temperature range of 20-40°C and a low bath ratio of 1:2-3.5.

[0030] (2) By precisely defining the EO / PO block structure, total number of alkyl oxygen units, HLB value and cloud point of the multi-block polyether, the polyether has excellent dispersion, wetting and moderate destabilization and migration characteristics in the room temperature range. It can stabilize high-concentration disperse dyes and promote the directional migration of dyes from the micelle phase to the fiber interior in the 35-40℃ range, thereby improving the dyeing rate under room temperature and micro-heating conditions.

[0031] (3) By forming a composite organic solvent phase by N-acetylmorpholine, propylene glycol phenyl ether and C2-C4 alkyl benzoate in a limited ratio and controlling the mass percentage of each of the three, the composite solvent can form a transparent or semi-transparent single-phase system with water at 25°C. It has a strong dissolving and swelling ability for disperse dyes, and avoids the problems of strong odor and high residue of traditional high-boiling-point carriers. It achieves fine dispersion and high stability of dyes at room temperature.

[0032] (4) By using a two-stage room temperature and low temperature heating dyeing process that matches the above-mentioned auxiliary agent system, the present invention can achieve a dyeing rate and color fastness close to or even reaching that of traditional high temperature and high pressure dispersion dyeing under a maximum temperature of no more than 42°C. At the same time, it significantly reduces the unit water consumption and unit energy consumption, and reduces the dependence on special high temperature and high pressure dyeing equipment. Detailed Implementation

[0033] The following provides a detailed description of specific embodiments of the present invention. It should be understood that the specific embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the scope of the invention.

[0034] Unless otherwise defined, all scientific and technical terms used in this invention have the same meaning as commonly understood by one of ordinary skill in the art.

[0035] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0036] Unless otherwise specified, all materials and reagents used in the following examples are commercially available.

[0037] The present invention will now be described in detail with reference to specific embodiments, which are intended to understand rather than limit the invention.

[0038] Example 1 This embodiment discloses a low-liquor-ratio dyeing auxiliary composition for room-temperature disperse dyes and its application process.

[0039] I. Preparation of a low-liquor-ratio dyeing auxiliary composition for disperse dyes at room temperature Weigh the following raw materials according to parts by weight: 25 parts of multi-block polyether nonionic surfactant: BASF Pluronic P-123 was selected, with an alternating EO / PO block structure, a total number of alkyl oxygen units of about 30, an EO content of about 55 wt%, a number average molecular weight of about 3000, an HLB value of about 12, and a cloud point of 44℃.

[0040] Ten parts of alkylamide betaine amphoteric surfactant: lauramidopropyl betaine (trade name: YS-CAB, active ingredient content 30%) produced by Guangzhou Yisheng Fine Chemical Co., Ltd.

[0041] The composite organic solvent phase, consisting of 30 parts, comprises the following three components: N-acetylmorpholine (NAM), 10 parts, selected from Jiangsu Dongbang Chemical Technology Co., Ltd. (industrial grade, purity ≥99%). Propylene glycol phenyl ether (PPH), 10 parts, selected from Jiangsu Hynix Chemical Co., Ltd. (model: PPH, purity ≥99%). Ethylbenzoate, 9 parts, selected from Zhejiang Longsheng Group (model: EBZ, purity ≥99%).

[0042] The mass ratio of the three components is 1:1:0.9.

[0043] Four portions of phosphate ester compounds: C10 fatty alcohol polyoxyethylene ether phosphate (model: XG-AEP-10) from Xinguo Chemical Co., Ltd.

[0044] 1.0 part of organosiloxane emulsion: The selected product is polyether-modified polydimethylsiloxane emulsion (model: DC-193, solid content 35wt%) produced by Dow Corning.

[0045] pH adjustment component 1.2 parts: Sodium acetate, Sinopharm Chemical Reagent Co., Ltd. (analytical grade).

[0046] The remainder is deionized water (make up to a total of 100 portions).

[0047] The preparation steps of the room temperature disperse dye low liquor ratio dyeing auxiliary composition are as follows: (1) Place 25 parts of Pluronic P-123 in a jacketed temperature-controlled mixing vessel, add about 20 parts of deionized water, heat to 35°C and stir at 300 rpm until completely dissolved.

[0048] (2) Add 10 parts of YS-CAB (lauramidopropyl betaine) while stirring, and continue stirring for 10 minutes to make it miscible with the polyether part to form a transparent system.

[0049] (3) Under the condition of maintaining 35°C, the composite organic solvent phase is slowly added in three parts, with an interval of 3 minutes between each addition, and the stirring speed is maintained at 400 rpm to ensure that there is no local turbidity or phase separation. After the addition is completed, continue stirring for 20 minutes.

[0050] (4) Add 4 parts of XG-AEP-10 (phosphate ester compound) and 1.0 part of DC-193 organosiloxane emulsion in sequence, and keep stirring for 10 minutes after each addition.

[0051] (5) Add 1.2 parts of sodium acetate and continue stirring until completely dissolved.

[0052] (6) Add the remaining deionized water to make the total volume of the system reach 100 parts, continue stirring for 15 minutes, and keep the temperature at 35°C to ensure that the additives are homogeneous.

[0053] (7) Finally, filter the mixture using an 80-mesh filter cloth to obtain a transparent to semi-transparent dyeing auxiliary composition free of suspended particles.

[0054] II. Room Temperature Disperse Dyeing Process with Low Liquor Ratio This embodiment utilizes the auxiliary composition prepared above to dye polyester knitted fabric. The specific steps are as follows: Step (1): Prepare the initial dye bath Add 30L of deionized water to the overflow dyeing machine. Weigh 90g of Disperse Blue 79 (Zhejiang Lonsen, model: DisperseBlue79, content ≥98%) to make the dye concentration 3g / L. Add 150g of the dyeing auxiliary composition prepared in this example to make the auxiliary dosage 5g / L. Adjust the pH of the dye bath to 4.8 using 10wt% glacial acetic acid and sodium acetate buffer. Adjust the bath ratio to 1:3 (fabric weight 10kg). Turn on the circulation pump and stir at 300rpm for 5min, controlling the temperature at 23℃. The resulting dye bath is a deep blue transparent liquid, free of suspended particles and floating flocculent matter.

[0055] Step (2): First stage of cyclic staining (room temperature pre-staining) Add 10 kg of polyester knitted fabric to the initial dye bath and allow it to spread naturally below the surface. Perform a 10-minute circulating dyeing process at 23°C, maintaining a circulation speed of 300–350 rpm to ensure the fabric does not knot or tangle. This stage primarily aims to evenly wet the dye and allow it to initially diffuse into the fiber surface. The dye bath should remain transparent throughout this process, without any precipitation or sedimentation.

[0056] Step (3): Heating and second-stage staining (low-temperature fixation) Maintaining a constant liquor ratio, increase the temperature at a rate of 0.8℃ / min. It takes approximately 19 minutes to rise from 23℃ to 38℃. Once reached, maintain this temperature for 30 minutes. Keep the circulation pump at 350 rpm to ensure even washing of the fabric surface. Throughout the dyeing process, the highest temperature did not exceed 40℃.

[0057] It was observed that the dye bath remained transparent throughout, and there were no color spots or loose dye adhering to the fabric surface.

[0058] Step (4): Post-processing After draining the dye bath, perform the following steps in sequence: Cold water washing: Wash with running water at 30℃ for 5 minutes to remove undyed dye.

[0059] Reduction cleaning: Add 1 g / L sodium dithionite and 1 g / L sodium carbonate to 30 L of freshly added water, and treat at 70 °C for 10 min.

[0060] Soap washing: Add 1g / L soaping agent (Zhejiang Lianhua Technology, model: LH-99) and soap wash for 10 minutes at 60℃.

[0061] Rinse with clean water: Rinse with running water until no visible color is visible in the water.

[0062] Drying: Dry with hot air at 80℃ for later use.

[0063] Example 2 The only difference between this embodiment and Example 1 is that the mass ratio of the multi-block polyether nonionic surfactant to the alkylamide betaine amphoteric surfactant is adjusted to 2:0.5, as detailed below: 25 parts of multi-block polyether nonionic surfactant: BASF Pluronic P-123 was selected, with an alternating EO / PO block structure, a total number of alkyl oxygen units of about 30, an EO content of about 55 wt%, a number average molecular weight of about 3000, an HLB value of about 12, and a cloud point of 44℃.

[0064] Five parts of alkylamide betaine amphoteric surfactants: lauramidopropyl betaine (trade name: YS-CAB, active ingredient content 30%) produced by Guangzhou Yisheng Fine Chemical Co., Ltd.

[0065] The composite organic solvent phase, consisting of 30 parts, comprises the following three components: N-acetylmorpholine (NAM), 10 parts, selected from Jiangsu Dongbang Chemical Technology Co., Ltd. (industrial grade, purity ≥99%). Propylene glycol phenyl ether (PPH), 10 parts, selected from Jiangsu Hynix Chemical Co., Ltd. (model: PPH, purity ≥99%). Ethylbenzoate, 9 parts, selected from Zhejiang Longsheng Group (model: EBZ, purity ≥99%).

[0066] The mass ratio of the three components is 1:1:0.9.

[0067] Four portions of phosphate ester compounds: C10 fatty alcohol polyoxyethylene ether phosphate (model: XG-AEP-10) from Xinguo Chemical Co., Ltd.

[0068] 1.0 part of organosiloxane emulsion: The selected product is polyether-modified polydimethylsiloxane emulsion (model: DC-193, solid content 35wt%) produced by Dow Corning.

[0069] pH adjustment component 1.2 parts: Sodium acetate, Sinopharm Chemical Reagent Co., Ltd. (analytical grade).

[0070] The remainder is deionized water (make up to a total of 100 portions).

[0071] Example 3 The only difference between this embodiment and Example 1 is that the NAM:PPH:EBZ ratio in the composite solvent is adjusted to 15%, 60%, and 25%, respectively.

[0072] Example 4 The only difference between this embodiment and Example 1 is that the mass ratio of the multi-block polyether nonionic surfactant to the phosphate ester compound is adjusted to 3.3:1, as detailed below: 20 parts of multi-block polyether nonionic surfactant: BASF Pluronic P-123 was selected, with an alternating EO / PO block structure, a total number of alkyl oxygen units of about 30, an EO content of about 55 wt%, a number average molecular weight of about 3000, an HLB value of about 12, and a cloud point of 44℃.

[0073] Ten parts of alkylamide betaine amphoteric surfactant: lauramidopropyl betaine (trade name: YS-CAB, active ingredient content 30%) produced by Guangzhou Yisheng Fine Chemical Co., Ltd.

[0074] The composite organic solvent phase, consisting of 30 parts, comprises the following three components: N-acetylmorpholine (NAM), 10 parts, selected from Jiangsu Dongbang Chemical Technology Co., Ltd. (industrial grade, purity ≥99%). Propylene glycol phenyl ether (PPH), 10 parts, selected from Jiangsu Hynix Chemical Co., Ltd. (model: PPH, purity ≥99%). Ethylbenzoate, 9 parts, selected from Zhejiang Longsheng Group (model: EBZ, purity ≥99%).

[0075] The mass ratio of the three components is 1:1:0.9.

[0076] Six parts of phosphate ester compounds: C10 fatty alcohol polyoxyethylene ether phosphate (model: XG-AEP-10) from Xinguo Chemical Co., Ltd.

[0077] 1.0 part of organosiloxane emulsion: The selected product is polyether-modified polydimethylsiloxane emulsion (model: DC-193, solid content 35wt%) produced by Dow Corning.

[0078] pH adjustment component 1.2 parts: Sodium acetate, Sinopharm Chemical Reagent Co., Ltd. (analytical grade).

[0079] The remainder is deionized water (make up to a total of 100 portions).

[0080] Comparative Example 1 The only difference between this comparative example and Example 1 is that glycol is used instead of glycol as the composite organic solvent phase.

[0081] Comparative Example 2 The only difference between this comparative example and Example 1 is that the maximum staining temperature in Example 1 was increased to 50°C. As a result, K / S decreased by 23%, ΔE increased by 1.8, and the wet rubbing fastness decreased by one grade. Performance testing I. Detection Methods 1. Apparent color depth (K / S value) The reflectance spectrum of dyed fabrics was measured using a reflectance spectrophotometer under D65 light source and 10° viewing angle conditions. The K / S value was calculated according to the Kubelka-Munk formula, and the K / S at the dominant wavelength was used as the apparent color depth index. Three measurements were taken for each sample, and the average value was calculated.

[0082] 2. Color difference (ΔE*ab) Using the stained sample from Example 1 as a reference, the colorimetric values ​​were measured using the same spectrophotometer under a D65 light source and a 10° viewing angle. The ΔE*ab value of each sample relative to Example 1 was calculated. Three measurements were taken for each sample, and the average value was calculated. A smaller ΔE value indicates better reproducibility of color light and color depth.

[0083] 3. Stability of dye bath dispersion Under the same liquor ratio, dye concentration, and auxiliary agent dosage as the dyeing process, dye bath samples were taken at 25℃ and 38℃ respectively. After standing for 30 min, the presence of flocculation, sedimentation, or obvious turbidity was observed, and the results were evaluated using a subjective scoring method of 0-5. Level 5: Transparent or nearly transparent, with no visible flocculation or sedimentation; Grade 4: Slightly milky, with no obvious sedimentation; Level 3: There is a small amount of fine flocculation or slight sedimentation; Grade 2: Obvious flocculation, with visible sedimentation; Level 1: Severe flocculation and sedimentation.

[0084] 4. Foaming and defoaming properties Take an auxiliary agent solution of the same concentration as the dyeing agent (excluding dye), add it to a 500 mL graduated cylinder, and stir with a standard stirrer for 5 min at 25℃. Stop stirring immediately and record the initial foam height (mm). Record the foam height after standing for 1 min and 5 min to evaluate the foaming and defoaming properties. The lower the foam and the faster the foam decays, the lower the foaming property and the better the defoaming property.

[0085] 5. Color fastness to dry rubbing The test shall be conducted in accordance with GB / T 3920-2008 "Textiles - Tests for color fastness to rubbing" using dry rubbing conditions, and the rating shall be from 1 to 5, with the higher the value indicating better fastness.

[0086] 6. Color fastness to wet rubbing According to GB / T 3920-2008 wet friction condition test, the rating is 1 to 5.

[0087] 7. Apparent uniformity (color evaluation) Visually inspect each sample under a standard light source box (D65 light source) for defects such as streaks, cloudiness, and color spots on the fabric surface, and use a subjective scoring method of 0-5 levels: Level 5: The fabric surface is uniform, with no visible color variations; Level 4: The fabric surface is generally uniform, with slight unevenness in some areas; Level 3: Visible slight color variations exist on the fabric surface; Level 2: Obvious color variations are present on the fabric surface; Level 1: The fabric surface has severe color variations and is unacceptable.

[0088] 8. Fabric hand feel and smoothness (qualitative evaluation) Three experienced evaluators compared and evaluated the fabric's hand feel and surface smoothness, classifying it into four levels: "excellent," "good," "medium," and "poor." The evaluation focused on the impact of organosiloxane emulsions and low-temperature processes on the fabric's style.

[0089] 9. Zeta potential The Zeta potential of the dye bath was measured at 25°C using electrophoretic light scattering. Dye bath samples from Examples 1, 3, and Comparative Example 1 were used for testing. A larger absolute value of the Zeta potential indicates a more stable dispersion system.

[0090] II. Test Results Table 1 lists the results of Examples 1 to 4 and Comparative Example 1 in the above tests.

[0091] Table 1

[0092] The Zeta potential of Example 1 was -28 mV, that of Example 3 was -15 mV, and that of Comparative Example 1 was -8 mV. The Zeta potential results show that the Zeta potential of the dye bath in Example 1 was -28 mV, which is significantly higher than that of Example 3 (-15 mV) and Comparative Example 1 (-8 mV), indicating that the formulation of the present invention has stronger charge stability and higher dispersion stability in the range of 25℃–40℃.

[0093] Overall results show that Example 1 of the present invention exhibits superior performance in various indicators, with high dyeing depth, relatively stable dye bath at both room temperature and low temperature heating stages, no obvious particle aggregation or sedimentation, low foaming, good leveling properties, and high dry and wet rubbing fastness, demonstrating good comprehensive performance.

[0094] When the proportion of betaine-based amphoteric surfactants was reduced (Example 2), the interfacial stability of the system weakened, the dyeing depth decreased slightly, and the dye bath was prone to slight dispersion instability under cyclic conditions. The levelness and rubbing fastness were also slightly weaker than in Example 1. This indicates that limiting the ratio of nonionic surfactants to amphoteric surfactants can effectively ensure uniform dye dispersion and consistent dyeing.

[0095] When the ratio of the three components in the composite organic solvent phase deviates from the set range (Example 3), the transparency and uniformity of the dye bath further decrease, and instability is more likely to occur in both the room temperature stage and the heating stage. The dyeing depth is reduced more significantly, and the indicators such as uniformity and rubbing fastness are also significantly worse than in Example 1. This indicates that the ratio of each solvent in the composite solvent plays an important role in the dispersion ability of the low-temperature dyeing system.

[0096] After adjusting the ratio of polyether nonionic surfactant to phosphate ester compound (Example 4), the foaming amount of the system increased, the dispersion state was not stable, the dyeing depth and leveling properties decreased to varying degrees, and the rubbing fastness also decreased, further demonstrating that this ratio range has a key impact on the system's ability to maintain low foaming and stable dispersion.

[0097] Comparative Example 1, in which the composite organic solvent system was directly replaced with glycol, performed the worst. The dye bath rapidly became unstable at room temperature, easily producing particle sedimentation and floating color, significantly increasing foam volume, significantly reducing dyeing depth, exhibiting poor leveling properties, and low rubbing fastness, failing to meet the dyeing requirements under room temperature and low liquor ratio conditions. This indicates that the composite solvent system possesses a specific synergistic swelling and dispersing ability that cannot be replaced by other common solvents.

[0098] The overall trend shows that the surfactant structure and ratio range, the composition of the composite solvent, and the proportion of phosphate ester compounds defined in this invention all have a significant impact on the dispersion stability, dyeing uniformity, and finished product fastness during low-liquid-ratio dyeing at room temperature. When any of these key proportions deviates from the set range, the system performance decreases to varying degrees. Example 1 shows the most balanced and excellent performance in all test items, indicating that the combination scheme of this invention has outstanding comprehensive technical effects under low-temperature and low-liquid-ratio conditions, and has significant advantages over conventional auxiliary agent systems.

[0099] The above description is merely a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, any improvements and modifications made without departing from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A low-liquor-ratio dyeing auxiliary composition for room-temperature disperse dyes, characterized in that, It comprises the following components in parts by weight: 15–35 parts of multi-block polyether nonionic surfactant; 5–12 parts of alkylamide betaine amphoteric surfactants; 20–35 parts of composite organic solvent phase; 2 to 6 parts of phosphate ester compounds; 0.3–1.5 parts organosiloxane emulsion; 0.5–3 parts pH adjustment component; The remainder is water; The multi-block polyether nonionic surfactant is a polyether with alternating propoxy and ethoxy units, a total number of alkyl oxy units of 10 to 40, a mass fraction of ethoxy units of 45 to 65 wt%, a number average molecular weight of 1500 to 4500, an HLB value of 11 to 14 in a 1 wt% aqueous solution, and a cloud point of 38 to 50 °C. The alkyl group of the alkylamide betaine amphoteric surfactant is a C12-C18 straight-chain or branched alkyl group. The composite organic solvent phase is composed of N-acetylmorpholine, propylene glycol phenyl ether and C2-C4 alkyl benzoate, with a mass ratio of 1:(0.7-1.3):(0.7-1.3). When the composite organic solvent phase is mixed with water at a volume ratio of 1:4 at 25°C, it forms a single-phase water-soluble system with a turbidity value not higher than 50 NTU.

2. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, The mass ratio of the multi-block polyether nonionic surfactant to the alkylamide betaine amphoteric surfactant is 2:(0.5-1.2).

3. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, The phosphate ester compound is one or more of the phosphate monoesters and / or diesters of C8-C12 fatty alcohols and / or their polyoxyethylene ethers and their neutral salts.

4. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, The organosiloxane emulsion is an aqueous emulsion of polydimethylsiloxane or polyether-modified polydimethylsiloxane.

5. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, The pH adjusting component is selected from one or more of sodium acetate, ammonium acetate, sodium formate, 2-hydroxy-2-methylpropanesulfonic acid and its sodium salt.

6. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, The mass ratio of the multi-block polyether nonionic surfactant, the alkylamide betaine amphoteric surfactant, and the composite organic solvent phase is 1:0.25-0.5:0.8-1.

6.

7. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, In the composite organic solvent phase, N-acetylmorpholine, propylene glycol phenyl ether, and C2-C4 alkyl benzoate each account for 20-45 wt% of the total mass of the composite organic solvent phase, and the mass fraction of N-acetylmorpholine is greater than or equal to the mass fraction of propylene glycol phenyl ether.

8. The room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to claim 1, characterized in that, The mass ratio of the multi-block polyether nonionic surfactant to the phosphate ester compound is (4-8):

1.

9. A disperse dyeing process using the room-temperature disperse dye low-liquor-ratio dyeing auxiliary composition according to any one of claims 1 to 8, characterized in that, Includes the following steps: (1) Add water, disperse dye and dyeing auxiliary agent composition to the dyeing equipment, adjust the pH of the dye bath to 4.2 to 5.5, make the amount of disperse dye in the dye bath 0.5 to 8 g / L, the amount of auxiliary agent composition 3 to 8 g / L, control the dye bath ratio to 1:2 to 3.5, and stir evenly at 20 to 25℃ to obtain the initial dye bath; (2) Add polyester filament, polyester staple fiber or its fabric to the initial dye bath obtained in step (1) and perform first-stage cyclic dyeing at 20-25°C for 5-15 minutes. (3) Under the condition of keeping the liquor ratio constant, the dye bath temperature is raised to 35-40℃ at a heating rate of 0.5-1.0℃ / min, and the second stage of cyclic dyeing is carried out within the range of 35-40℃ for 20-40min. The highest dyeing temperature in the entire dyeing process shall not exceed 42℃. (4) After draining the dye bath, the dyed fiber material obtained in step (3) is subjected to water washing, reduction cleaning, soap washing, rinsing with clean water and drying treatment in sequence.

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