A disperse dye composition and process for its preparation

Abstract

This invention discloses a disperse dye composition and its preparation process, comprising, by weight parts: 20-50 parts of azo disperse dye, 10-35 parts of anthraquinone disperse dye, 5-25 parts of heterocyclic disperse dye, 8-20 parts of a composite dispersant, 2-8 parts of a leveling agent, 1-5 parts of an anti-migration agent, 0.5-3 parts of a pH buffer, 0.1-1.5 parts of an antioxidant, and 0.05-0.5 parts of a bactericide and preservative. The composite dispersant is composed of sodium naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, alkyl naphthalene sulfonate formaldehyde condensate, and a polycarboxylate dispersant. The heterocyclic disperse dye is a disperse dye containing a thiazole ring, a benzothiazole ring, or a quinoline ring structure. Through the synergistic effect of the components, this invention enables the disperse dye composition to possess excellent high-temperature dispersion stability, good leveling performance, high dye uptake and lifting power, excellent fastness properties, and storage stability. Furthermore, the preparation process is simple and highly efficient, making it suitable for dyeing and printing hydrophobic fiber materials.

Description

Technical Field

[0001] This invention relates to the field of dye chemical technology, and in particular to a disperse dye composition and its preparation process, especially to a high-performance disperse dye composition for dyeing hydrophobic fiber materials and its industrial preparation method. Background Technology

[0002] Disperse dyes are a class of nonionic dyes with relatively simple molecular structures, lacking water-soluble groups, and existing in a dispersed state in the dye bath. They are mainly used for dyeing and printing hydrophobic synthetic fibers such as polyester, acetate, and polyamide. Since the 1950s, with the industrial production and widespread application of polyester fibers, the disperse dye industry has developed rapidly and has become one of the most important categories in the field of synthetic dyes, boasting the largest output, the most varieties, and the widest application.

[0003] Currently, research on disperse dye compositions mainly focuses on the following aspects: First, improving the dye uptake and lifting power of dyes to reduce dye usage and lower dyeing costs; second, improving various fastness properties of dyes, including wash fastness, sublimation fastness, rubbing fastness, and light fastness, to meet the increasingly stringent quality requirements of textiles; third, enhancing the dispersion stability and leveling properties of dyes during the dyeing process to avoid dyeing defects such as color spots and discoloration; and fourth, developing dye compositions adapted to new dyeing processes, such as energy-saving and environmentally friendly processes like short-process dyeing, one-bath dyeing, and reduction-free washing dyeing.

[0004] In the prior art, various disperse dye compositions have been disclosed. For example, Yorkshire (Zhejiang) Dyeing & Chemical Co., Ltd.'s patent application for a disperse dye composition, disperse dye, preparation method and use thereof (publication number CN119350881A) provides a disperse dye composition containing multiple specific structural components, which has excellent lifting power and color fastness. Zhejiang Runtu Co., Ltd.'s patent application for a greenish-blue disperse dye composition, greenish-blue disperse dye, preparation method and use thereof (publication number CN121914561A) provides a greenish-blue disperse dye composition containing two specific structural components, which has good lifting power and high strength when applied to fabric dyeing and printing. Zhejiang Wanfeng Chemical Co., Ltd.'s patent application for a disperse deep blue to black dye composition and its application (publication number CN122011802A) provides a dye composition that can stably dye in dye baths with pH 4-12 without the need for reduction washing. A patent application (publication number CN121825279A) filed by Zhejiang Longsheng Group Co., Ltd. et al. provides a disperse orange-red dye for dyeing polylactic acid fibers.

[0005] However, the aforementioned existing technologies still have the following shortcomings:

[0006] First, the high-temperature dispersion stability of existing disperse dye compositions during the dyeing process still needs to be improved. Under high-temperature and high-pressure dyeing conditions (usually 120-140℃), some dye components are prone to aggregation and precipitation, leading to reduced dye utilization and quality problems such as color spots and blemishes on dyed fabrics.

[0007] Second, the leveling performance of existing disperse dye compositions on polyester and its blended fabrics is not ideal. Due to the differences in affinity and dyeing rate of different dye components to fibers, competitive dyeing is prone to occur during color matching, resulting in the color of the dyed fabric deviating from the expected value and large color differences between batches.

[0008] Third, existing processes for preparing disperse dye compositions generally suffer from problems such as low grinding efficiency, high energy consumption, and uneven particle size distribution. Traditional grinding methods such as sand milling and ball milling are time-consuming and make it difficult to achieve fine dispersion of dye particles at the nanoscale, which affects the dye uptake rate and color brightness.

[0009] Fourth, existing disperse dye compositions have poor adaptability to different dyeing processes. As the textile printing and dyeing industry moves towards shorter processes, lower energy consumption, and environmental friendliness, higher demands are being placed on disperse dye compositions, including adaptability to low liquor ratio dyeing, tolerance to weakly alkaline dye baths, and the ability to achieve reduction-free washing dyeing. Existing products still have significant room for improvement in these areas.

[0010] Fifth, the storage stability of existing disperse dye compositions is insufficient. Liquid disperse dyes are prone to problems such as layering, precipitation, and viscosity changes during long-term storage, which affects the commercial application of the products.

[0011] To address the shortcomings of the prior art, this invention provides a novel disperse dye composition and its preparation process, aiming to solve the technical problems in the prior art such as poor high-temperature dispersion stability, unsatisfactory leveling performance, low preparation process efficiency, poor process adaptability, and insufficient storage stability. Summary of the Invention

[0012] In view of the shortcomings of the existing technology, the purpose of this invention is to provide a disperse dye composition and its preparation process. The disperse dye composition of this invention has excellent high-temperature dispersion stability, good leveling performance, high dyeing rate and lifting power, and excellent fastness properties. Moreover, the preparation process is simple, the production efficiency is high, and the product quality is stable.

[0013] The above-mentioned objective of this invention is achieved through the following technical solutions:

[0014] In a first aspect, the present invention provides a disperse dye composition comprising, by weight parts:

[0015] Component A: 20-50 parts of azo disperse dye;

[0016] Component B: 10-35 parts of anthraquinone disperse dye;

[0017] Component C: 5-25 parts of heterocyclic disperse dyes;

[0018] Component D: 8-20 parts of composite dispersant;

[0019] Component E: 2-8 parts of leveling agent;

[0020] Component F: 1-5 parts of anti-migratory agent;

[0021] Component G: 0.5-3 parts of pH buffer;

[0022] Component H: 0.1~1.5 parts of antioxidant;

[0023] Component I: 0.05~0.5 parts of bactericide and preservative.

[0024] Preferably, the azo disperse dye is a monoazo disperse dye, and more preferably a mixture of one or more of CI disperse yellow, CI disperse orange, CI disperse red, and CI disperse blue.

[0025] Preferably, the anthraquinone disperse dye is an aminoanthraquinone type disperse dye, and more preferably it is one or a mixture of CI disperse violet, CI disperse blue, and CI disperse turquoise blue.

[0026] Preferably, the heterocyclic disperse dye is a disperse dye containing a thiazole ring, a benzothiazole ring, or a quinoline ring structure, and more preferably a mixture of one or more of CI disperse yellow, CI disperse red, and CI disperse blue.

[0027] Preferably, the composite dispersant is composed of the following components in parts by weight: 30-60 parts of sodium naphthalene sulfonate formaldehyde condensate, 20-40 parts of sodium lignosulfonate, 10-30 parts of alkyl naphthalene sulfonate formaldehyde condensate, and 5-15 parts of polycarboxylate dispersant.

[0028] Preferably, the leveling agent is selected from one or more of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyethylene glycol fatty acid ester, and polyvinylpyrrolidone.

[0029] Preferably, the anti-migratory agent is selected from one or more of sodium polyacrylate, sodium carboxymethyl cellulose, sodium alginate, and polyethylene glycol.

[0030] Preferably, the pH buffer is selected from one of the following: sodium dihydrogen phosphate-disodium hydrogen phosphate buffer pair, acetate-sodium acetate buffer pair, and citric acid-sodium citrate buffer pair.

[0031] Preferably, the antioxidant is selected from one or more of butylated hydroxyanisole, butylated hydroxytoluene, propyl gallate, and tocopherol.

[0032] Preferably, the bactericidal preservative is selected from one or more of isothiazolinone compounds and benzisothiazolinone compounds.

[0033] More preferably, the disperse dye composition comprises, by weight parts, the following components:

[0034] Component A: 25-45 parts of azo disperse dye;

[0035] Component B: 12-30 parts of anthraquinone disperse dye;

[0036] Component C: 8-22 parts of heterocyclic disperse dyes;

[0037] Component D: 10-18 parts of composite dispersant;

[0038] Component E: 3-7 parts of leveling agent;

[0039] Component F: 1.5-4 parts of anti-migratory agent;

[0040] Component G: 0.8-2.5 parts of pH buffer;

[0041] Component H: 0.2~1.2 parts of antioxidant;

[0042] Component I: 0.08~0.4 parts of bactericide and preservative.

[0043] More preferably, the disperse dye composition comprises, by weight parts, the following components:

[0044] Component A: 30-40 parts of azo disperse dye;

[0045] Component B: 15-25 parts of anthraquinone disperse dye;

[0046] Component C: 10-18 parts of heterocyclic disperse dyes;

[0047] Component D: 12-16 parts of composite dispersant;

[0048] Component E: 4-6 parts of leveling agent;

[0049] Component F: 2-3 parts of anti-migratory agent;

[0050] Component G: 1-2 parts of pH buffer;

[0051] Component H: 0.3~0.8 parts of antioxidant;

[0052] Component I: 0.1~0.3 parts of bactericide and preservative.

[0053] Preferably, the disperse dye composition is in the form of a solid powder, granules, or liquid dispersion.

[0054] In a second aspect, the present invention provides a preparation process for the above-mentioned disperse dye composition, comprising the following steps:

[0055] Step 1: Weigh each component according to the formula amount, and premix the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to obtain the dye premix;

[0056] Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water, and heat under stirring to dissolve them, thus obtaining the auxiliary agent solution;

[0057] Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and perform high-speed dispersion and mixing to obtain a coarse dispersion slurry;

[0058] Step 4: Grind the coarse dispersion slurry obtained in Step 3 to make the particle size of the dye particles meet the specified requirements, and obtain a fine dispersion slurry.

[0059] Step 5: Filter the finely dispersed slurry obtained in Step 4 to remove impurities, and obtain the liquid dispersed dye composition product;

[0060] Step 6: Dry the liquid disperse dye composition product obtained in Step 5 to obtain a solid powder or granular disperse dye composition product.

[0061] Preferably, the premixing in step one is carried out using a V-type mixer or a double cone mixer, with a mixing time of 10-30 minutes and a mixing speed of 10-30 rpm.

[0062] Preferably, the amount of deionized water used in step two is 1.5 to 3 times the total mass of the dye premix.

[0063] Preferably, the heating and dissolving temperature in step two is 40~80℃, the stirring speed is 200~600 rpm, and the stirring time is 15~45 minutes.

[0064] Preferably, the high-speed dispersion in step three is carried out using a high-speed disperser with a dispersion speed of 1000~3000 rpm and a dispersion time of 20~60 minutes.

[0065] Preferably, the grinding process in step four is carried out using a horizontal sand mill or a vertical bead mill, the grinding media is zirconia beads or glass beads, the particle size of the grinding media is 0.3~1.5 mm, the grinding temperature is 10~40℃, and the grinding time is 1~5 hours.

[0066] Preferably, the requirement in step four is that the average particle size of the dye particles is not greater than 500 nanometers and the particle size distribution span is not greater than 1.5.

[0067] Preferably, the filtration in step five is performed using microporous filtration or membrane filtration, with a filtration accuracy of 0.5 to 5 micrometers.

[0068] Preferably, the drying process in step six is ​​carried out by spray drying, with an inlet temperature of 150~220℃ and an outlet temperature of 70~100℃.

[0069] More preferably, the preparation process further includes a step of quality testing of the liquid disperse dye composition product after step five and before step six, wherein the quality testing includes solid content determination, particle size determination, viscosity determination, colorimetric determination and intensity determination.

[0070] Thirdly, the present invention provides the application of the above-described disperse dye composition in the dyeing and / or printing of hydrophobic fiber materials.

[0071] Preferably, the hydrophobic fiber material is one or more of polyester fiber, polyamide fiber, acetate fiber, and polylactic acid fiber, or a blend of the above fibers with other fibers.

[0072] Preferably, the staining is performed using a high-temperature and high-pressure staining method, a hot-melt staining method, or a carrier staining method.

[0073] Preferably, the printing is done using direct printing, discharge printing, or resist printing.

[0074] In summary, compared with the prior art, the present invention has at least one of the following beneficial technical effects:

[0075] First, this invention, through the rational selection and compounding of three different types of disperse dyes—azo, anthraquinone, and heterocyclic—fully leverages the performance advantages of each dye type, achieving synergistic effects in color, dye uptake, lightfastness, and colorfastness. Azo disperse dyes offer a complete color spectrum, are inexpensive, and have moderate dye uptake rates; anthraquinone disperse dyes boast vibrant colors and excellent lightfastness; and heterocyclic disperse dyes have high molar extinction coefficients and pure colors. Compounding these three types in specific proportions can significantly improve dye uptake and various colorfastness properties while maintaining color purity.

[0076] Secondly, the composite dispersant of this invention is formulated with sodium naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, alkyl naphthalene sulfonate formaldehyde condensate, and polycarboxylate dispersant, fully leveraging the synergistic effects of each dispersant. Specifically, sodium naphthalene sulfonate formaldehyde condensate exhibits good dispersion for azo dyes, sodium lignin sulfonate provides good dispersion for anthraquinone dyes, alkyl naphthalene sulfonate formaldehyde condensate provides good dispersion for heterocyclic dyes, and the polycarboxylate dispersant provides steric stabilization. The synergistic use of these four dispersants ensures good dispersion stability of dye particles under high-temperature dyeing conditions, effectively preventing dye aggregation and precipitation.

[0077] Third, by adding a leveling agent, this invention effectively improves the leveling performance of the dye composition during the dyeing process. The leveling agent can slow down the dye uptake rate, making the uptake rate of different dye components on the fiber more consistent, avoiding competitive dyeing, and ensuring the color consistency and batch-to-batch reproducibility of the dyed fabric.

[0078] Fourth, by adding an anti-migration agent, this invention effectively prevents the migration of dyes during the dyeing and drying process, ensuring the uniform distribution of dyes on the fibers and reducing the occurrence of dyeing defects such as color spots and color streaks.

[0079] Fifth, by adding a pH buffer, the present invention maintains a stable pH range in the dye bath during the dyeing process, avoiding problems such as dye hydrolysis, color changes and decreased dyeing rate caused by pH fluctuations, while expanding the adaptability of the dye composition to different dyeing processes.

[0080] Sixth, by adding antioxidants, this invention effectively prevents the dye from oxidizing and deteriorating during storage and use, thus extending the product's shelf life; by adding bactericidal and preservative agents, it effectively prevents the liquid disperse dye from spoiling and deteriorating due to microbial growth during storage.

[0081] Seventh, the preparation process of this invention adopts a step-by-step process route of pre-mixing, then preparing the auxiliary agent solution, then high-speed dispersion, and finally fine grinding. The process parameters of each step have been optimized to effectively ensure the quality stability and batch-to-batch reproducibility of the product. In particular, the use of a horizontal sand mill with grinding media of appropriate particle size can grind dye particles to the nanoscale in a short time with uniform particle size distribution, significantly improving grinding efficiency and product quality.

[0082] Eighth, the disperse dye composition of the present invention can be adapted to a variety of dyeing processes, including high temperature and high pressure dyeing, hot melt dyeing, carrier dyeing, etc., and can be applied to the dyeing and printing of a variety of hydrophobic fiber materials such as polyester fiber, polyamide fiber, acetate fiber, and polylactic acid fiber, and has wide applicability. Attached Figure Description

[0083] Figure 1 This is a schematic flowchart of the preparation process of the disperse dye composition of the present invention. Detailed Implementation

[0084] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0085] In the description of this invention, the terms "comprising," "including," "containing," etc., mean that the said features, integers, steps, operations, components, and / or parts are present, but do not exclude the presence or addition of one or more other features, integers, steps, operations, components, parts, and / or combinations thereof.

[0086] In the description of this invention, the term "parts by mass" refers to the relative mass ratio between the components, which can be scaled up or down proportionally according to the production scale in actual production.

[0087] In the description of this invention, the term "azo disperse dye" refers to disperse dyes containing azo groups in their molecular structure, including monoazo, diazo, and polyazo disperse dyes.

[0088] In the description of this invention, the term "anthraquinone disperse dye" refers to disperse dyes whose molecular structure contains an anthraquinone core, including aminoanthraquinone type, hydroxyanthraquinone type, etc.

[0089] In the description of this invention, the term "heterocyclic disperse dye" refers to disperse dyes whose molecular structure contains nitrogen-, sulfur-, or oxygen-containing heterocycles, including thiazoles, benzothiazoles, quinolines, etc.

[0090] In the description of this invention, the term "average particle size" refers to the volume average particle size of dye particles as determined by dynamic light scattering.

[0091] In the description of this invention, the term "particle size distribution span" refers to the value obtained by dividing the difference between D90 and D10 in the particle size distribution curve by D50, where D10, D50, and D90 represent the particle size values ​​corresponding to the cumulative distribution reaching 10%, 50%, and 90%, respectively.

[0092] Example 1

[0093] This embodiment provides a disperse dye composition and its preparation process.

[0094] The disperse dye composition of this embodiment consists of the following components in parts by weight:

[0095] Component A: 35 parts of azo disperse dye (CI Disperse Blue);

[0096] Component B: 20 ​​parts of anthraquinone disperse dye (CI disperse violet);

[0097] Component C: 15 parts of heterocyclic disperse dye (CI Disperse Yellow);

[0098] Component D: 14 ​​parts of composite dispersant;

[0099] Component E: 5 parts of leveling agent (fatty alcohol polyoxyethylene ether);

[0100] Component F: Anti-migration agent (sodium polyacrylate) 2.5 parts;

[0101] Component G: 1.5 parts of pH buffer (sodium dihydrogen phosphate-disodium hydrogen phosphate buffer pair);

[0102] Component H: 0.5 parts of antioxidant (butylated hydroxyanisole);

[0103] Component I: 0.15 parts of bactericide and preservative (isothiazolinone).

[0104] The composite dispersant is composed of the following components in parts by weight: 45 parts sodium naphthalene sulfonate formaldehyde condensate, 30 parts sodium lignosulfonate, 18 parts sodium alkyl naphthalene sulfonate formaldehyde condensate, and 7 parts polycarboxylate dispersant.

[0105] Reference Figure 1 The preparation process of the disperse dye composition in this embodiment includes the following steps:

[0106] Step 1: Weigh each component according to the above formula, add the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to a V-type mixer for premixing, mix for 20 minutes at a speed of 20 rpm, and obtain the dye premix.

[0107] Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water. The amount of deionized water is 2.2 times the total mass of the dye premix. Heat to 60°C under stirring conditions to dissolve the dye. The stirring speed is 400 rpm and the stirring time is 30 minutes to obtain the auxiliary agent solution.

[0108] Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and use a high-speed disperser to disperse and mix at a speed of 2000 rpm for 40 minutes to obtain a coarse dispersion slurry.

[0109] Step 4: Add the coarse dispersion slurry obtained in Step 3 to a horizontal sand mill for grinding. The grinding media is zirconia beads with a particle size of 0.8 mm. The grinding temperature is 25℃ and the grinding time is 3 hours. This process ensures that the average particle size of the dye particles is no greater than 500 nanometers and the particle size distribution span is no greater than 1.5, thus obtaining a fine dispersion slurry.

[0110] Step 5: The finely dispersed slurry obtained in Step 4 is filtered to remove impurities using a microporous filtration method with a filtration accuracy of 2 micrometers, to obtain the liquid dispersed dye composition product.

[0111] Step 6: The liquid disperse dye composition product obtained in Step 5 is subjected to spray drying. The inlet temperature of the spray dryer is 185℃ and the outlet temperature is 85℃ to obtain a solid powder disperse dye composition product.

[0112] Figure 1 This is a schematic flow chart of the preparation process of the disperse dye composition of the present invention. Figure 1 As shown, the preparation process of the present invention mainly includes the following steps: raw material preparation step 101, dye premixing step 102, auxiliary agent preparation step 103, high-speed dispersion step 104, fine grinding step 105, filtration and impurity removal step 106, quality inspection step 107, liquid product packaging step 108, spray drying step 109, and solid product packaging step 110. Specifically, the raw material preparation step 101 provides raw materials to the dye premixing step 102 and the auxiliary agent preparation step 103 respectively; the outputs of the dye premixing step 102 and the auxiliary agent preparation step 103 jointly enter the high-speed dispersion step 104; after the high-speed dispersion step 104, the fine grinding step 105, the filtration and impurity removal step 106, and the quality inspection step 107 are connected sequentially; after the quality inspection step 107, the process splits into two routes: one connects to the liquid product packaging step 108 to directly obtain the liquid disperse dye composition product, and the other connects to the spray drying step 109 and the solid product packaging step 110 to obtain the solid powder disperse dye composition product.

[0113] The particle size distribution of the disperse dye composition prepared in this embodiment was determined by dynamic light scattering method, and the results are listed in Table 1.

[0114] Table 1. Dye particle size distribution parameters in Example 1

[0115] parameter D10 (nm) D50 (nm) D90 (nm) Average particle size (nm) Particle size distribution span numerical values 182 315 478 320 0.94

[0116] As shown in Table 1, the particle size distribution of the dye particles exhibits a unimodal distribution with an average particle size of approximately 320 nanometers and a particle size distribution span of approximately 0.94. This indicates that the preparation process of the present invention can grind the dye particles to the nanoscale with a uniform particle size distribution, which is beneficial for improving the dye uptake rate and dyeing brightness.

[0117] The high-temperature dispersion stability of the disperse dye composition prepared in this embodiment was tested. The method was as follows: the liquid disperse dye composition was diluted with deionized water to a mass fraction of 1%, placed in a high-temperature and high-pressure dyeing machine, and kept at 130°C for 0, 15, 30, 45 and 60 minutes respectively. Then it was naturally cooled to room temperature. The absorbance value of each sample at the maximum absorption wavelength was measured by a spectrophotometer. The absorbance retention rate at each time point was calculated based on the absorbance value of the sample at 0 minutes. The results are listed in Table 2.

[0118] Table 2. High-temperature dispersion stability test results of Example 1

[0119] Incubation time (minutes) 0 15 30 45 60 Absorbance retention rate (%) 100 99.2 98.5 97.6 96.8

[0120] As shown in Table 2, after being kept at 130℃ for 60 minutes, the absorbance retention rate of the dye dispersion remained above 96%, indicating that the disperse dye composition of the present invention has excellent high-temperature dispersion stability. This is mainly attributed to the synergistic effect of the four dispersants in the composite dispersant, as well as the auxiliary effects of the anti-migration agent and pH buffer, which effectively prevent the aggregation and precipitation of dye particles under high-temperature conditions.

[0121] Example 2

[0122] This embodiment provides a disperse dye composition and its preparation process.

[0123] The disperse dye composition of this embodiment consists of the following components in parts by weight:

[0124] Component A: 30 parts of azo disperse dye (CI Disperse Red);

[0125] Component B: 25 parts of anthraquinone disperse dye (CI Disperse Blue);

[0126] Component C: 10 parts of heterocyclic disperse dye (CI Disperse Orange);

[0127] Component D: 16 parts of composite dispersant;

[0128] Component E: 4 parts of leveling agent (alkylphenol polyoxyethylene ether);

[0129] Component F: Anti-migration agent (sodium carboxymethyl cellulose) 3 parts;

[0130] Component G: 2 parts of pH buffer (acetic acid-sodium acetate buffer pair);

[0131] Component H: 0.8 parts of antioxidant (butylated hydroxytoluene);

[0132] Component I: 0.2 parts of bactericide and preservative (benzisothiazolinone).

[0133] The composite dispersant is composed of the following components in parts by weight: 40 parts sodium naphthalene sulfonate formaldehyde condensate, 35 parts sodium lignosulfonate, 15 parts sodium alkyl naphthalene sulfonate formaldehyde condensate, and 10 parts polycarboxylate dispersant.

[0134] The preparation process of the disperse dye composition in this embodiment includes the following steps:

[0135] Step 1: Weigh each component according to the above formula, add the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to a double cone mixer for premixing. The mixing time is 15 minutes and the mixing speed is 25 rpm to obtain the dye premix.

[0136] Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water. The amount of deionized water is 2.5 times the total mass of the dye premix. Heat to 50°C under stirring conditions to dissolve the dye. The stirring speed is 500 rpm and the stirring time is 25 minutes to obtain the auxiliary agent solution.

[0137] Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and use a high-speed disperser to disperse and mix at a speed of 2500 rpm for 30 minutes to obtain a coarse dispersion slurry.

[0138] Step 4: Add the coarse dispersion slurry obtained in Step 3 to a vertical bead mill for grinding. The grinding media is zirconia beads with a particle size of 0.6 mm. The grinding temperature is 20℃ and the grinding time is 4 hours. This will make the average particle size of the dye particles no greater than 500 nanometers and the particle size distribution span no greater than 1.5, thus obtaining a fine dispersion slurry.

[0139] Step 5: The finely dispersed slurry obtained in Step 4 is filtered to remove impurities using a membrane filtration method with a filtration accuracy of 1 micrometer, to obtain the liquid dispersed dye composition product.

[0140] Step 6: The liquid disperse dye composition product obtained in Step 5 is subjected to spray drying. The inlet temperature of the spray dryer is 200℃ and the outlet temperature is 90℃ to obtain a solid powder disperse dye composition product.

[0141] Example 3

[0142] This embodiment provides a disperse dye composition and its preparation process.

[0143] The disperse dye composition of this embodiment consists of the following components in parts by weight:

[0144] Component A: 40 parts of azo disperse dye (CI Disperse Yellow);

[0145] Component B: 15 parts of anthraquinone disperse dye (CI Disperse Turquoise Blue);

[0146] Component C: 18 parts of heterocyclic disperse dye (CI Disperse Red);

[0147] Component D: 12 parts of composite dispersant;

[0148] Component E: 6 parts of leveling agent (polyethylene glycol fatty acid ester);

[0149] Component F: 2 parts of anti-migratory agent (sodium alginate);

[0150] Component G: 1 part pH buffer (citric acid-sodium citrate buffer pair);

[0151] Component H: 0.3 parts of antioxidant (propyl gallate);

[0152] Component I: 0.1 parts of bactericide and preservative (isothiazolinone).

[0153] The composite dispersant is composed of the following components in parts by weight: 50 parts sodium naphthalene sulfonate formaldehyde condensate, 25 parts sodium lignosulfonate, 20 parts sodium alkyl naphthalene sulfonate formaldehyde condensate, and 5 parts polycarboxylate dispersant.

[0154] The preparation process of the disperse dye composition in this embodiment includes the following steps:

[0155] Step 1: Weigh each component according to the above formula, add the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to a V-type mixer for premixing, mix for 25 minutes at a speed of 15 rpm, and obtain the dye premix.

[0156] Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water. The amount of deionized water is 1.8 times the total mass of the dye premix. Heat to 70°C under stirring conditions to dissolve the dye. The stirring speed is 300 rpm and the stirring time is 40 minutes to obtain the auxiliary agent solution.

[0157] Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and use a high-speed disperser to disperse and mix at a speed of 1500 rpm for 50 minutes to obtain a coarse dispersion slurry.

[0158] Step 4: Add the coarse dispersion slurry obtained in Step 3 to a horizontal sand mill for grinding. The grinding media is glass beads with a particle size of 1.0 mm. The grinding temperature is 30℃ and the grinding time is 2.5 hours. This process ensures that the average particle size of the dye particles is no greater than 500 nanometers and the particle size distribution span is no greater than 1.5, thus obtaining a fine dispersion slurry.

[0159] Step 5: The finely dispersed slurry obtained in Step 4 is filtered to remove impurities using a microporous filtration method with a filtration accuracy of 3 micrometers, to obtain the liquid dispersed dye composition product.

[0160] Step 6: The liquid disperse dye composition product obtained in Step 5 is subjected to spray drying. The inlet temperature of the spray dryer is 170℃ and the outlet temperature is 80℃ to obtain a solid powder disperse dye composition product.

[0161] Example 4

[0162] This embodiment provides a disperse dye composition and its preparation process.

[0163] The disperse dye composition of this embodiment consists of the following components in parts by weight:

[0164] Component A: 38 parts of azo disperse dyes (a mixture of CI disperse orange and CI disperse red, in a mass ratio of 1:1);

[0165] Component B: 22 parts of anthraquinone disperse dyes (a mixture of CI disperse violet and CI disperse blue, in a mass ratio of 2:1);

[0166] Component C: 12 parts of heterocyclic disperse dye (CI Disperse Yellow);

[0167] Component D: 15 parts of composite dispersant;

[0168] Component E: 4.5 parts of leveling agent (polyvinylpyrrolidone);

[0169] Component F: Anti-migratory agent (polyethylene glycol) 2.8 parts;

[0170] Component G: 1.8 parts of pH buffer (sodium dihydrogen phosphate-disodium hydrogen phosphate buffer pair);

[0171] Component H: 0.6 parts of antioxidant (tocopherol);

[0172] Component I: 0.25 parts of bactericide and preservative (benzisothiazolinone).

[0173] The composite dispersant is composed of the following components in parts by weight: 42 parts sodium naphthalene sulfonate formaldehyde condensate, 28 parts sodium lignin sulfonate, 22 parts sodium alkyl naphthalene sulfonate formaldehyde condensate, and 8 parts polycarboxylate dispersant.

[0174] The preparation process of the disperse dye composition in this embodiment includes the following steps:

[0175] Step 1: Weigh each component according to the above formula, add the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to a double cone mixer for premixing. The mixing time is 18 minutes and the mixing speed is 22 rpm to obtain the dye premix.

[0176] Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water. The amount of deionized water is 2.0 times the total mass of the dye premix. Heat to 55°C under stirring conditions to dissolve the dye. The stirring speed is 450 rpm and the stirring time is 35 minutes to obtain the auxiliary agent solution.

[0177] Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and use a high-speed disperser to disperse and mix at a speed of 2200 rpm for 35 minutes to obtain a coarse dispersion slurry.

[0178] Step 4: Add the coarse dispersion slurry obtained in Step 3 to a horizontal sand mill for grinding. The grinding media is zirconia beads with a particle size of 0.5 mm. The grinding temperature is 22℃ and the grinding time is 3.5 hours. This process ensures that the average particle size of the dye particles is no greater than 500 nanometers and the particle size distribution span is no greater than 1.5, thus obtaining a fine dispersion slurry.

[0179] Step 5: The finely dispersed slurry obtained in Step 4 is filtered to remove impurities using a membrane filtration method with a filtration accuracy of 0.8 micrometers, to obtain the liquid dispersed dye composition product.

[0180] Step Six: The liquid disperse dye composition product obtained in Step Five is subjected to spray drying. The inlet temperature of the spray dryer is 190℃ and the outlet temperature is 88℃ to obtain a solid powder disperse dye composition product.

[0181] Example 5

[0182] This embodiment provides a disperse dye composition and its preparation process.

[0183] The disperse dye composition of this embodiment consists of the following components in parts by weight:

[0184] Component A: 42 parts of azo disperse dyes (a mixture of CI disperse blue and CI disperse red, in a mass ratio of 3:1);

[0185] Component B: 18 parts of anthraquinone disperse dye (CI Disperse Turquoise Blue);

[0186] Component C: 15 parts of heterocyclic disperse dyes (a mixture of CI disperse yellow and CI disperse orange in a mass ratio of 1:2);

[0187] Component D: 13 parts of composite dispersant;

[0188] Component E: Leveling agent (a mixture of fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether, in a mass ratio of 1:1) 5.5 parts;

[0189] Component F: Anti-migratory agent (a mixture of sodium polyacrylate and sodium carboxymethyl cellulose in a mass ratio of 2:1) 2.2 parts;

[0190] Component G: 1.2 parts of pH buffer (acetic acid-sodium acetate buffer pair);

[0191] Component H: 0.7 parts of antioxidant (a mixture of butylated hydroxyanisole and butylated hydroxytoluene, in a mass ratio of 1:1);

[0192] Component I: 0.18 parts of bactericide and preservative (isothiazolinone).

[0193] The composite dispersant is composed of the following components in parts by weight: 48 parts sodium naphthalene sulfonate formaldehyde condensate, 32 parts sodium lignosulfonate, 16 parts sodium alkyl naphthalene sulfonate formaldehyde condensate, and 4 parts polycarboxylate dispersant.

[0194] The preparation process of the disperse dye composition in this embodiment includes the following steps:

[0195] Step 1: Weigh each component according to the above formula, add the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to a V-type mixer for premixing, mix for 22 minutes and at a speed of 18 rpm to obtain the dye premix.

[0196] Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water. The amount of deionized water is 2.8 times the total mass of the dye premix. Heat to 65°C under stirring conditions to dissolve the dye. The stirring speed is 350 rpm and the stirring time is 20 minutes to obtain the auxiliary agent solution.

[0197] Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and use a high-speed disperser to disperse and mix at a speed of 1800 rpm for 45 minutes to obtain a coarse dispersion slurry.

[0198] Step 4: Add the coarse dispersion slurry obtained in Step 3 to a vertical bead mill for grinding. The grinding media is zirconia beads with a particle size of 1.2 mm. The grinding temperature is 28℃ and the grinding time is 2 hours. This process ensures that the average particle size of the dye particles is no greater than 500 nanometers and the particle size distribution span is no greater than 1.5, thus obtaining a fine dispersion slurry.

[0199] Step 5: The finely dispersed slurry obtained in Step 4 is filtered to remove impurities using a microporous filtration method with a filtration accuracy of 5 micrometers, to obtain the liquid dispersed dye composition product.

[0200] Step 6: The liquid disperse dye composition product obtained in Step 5 is subjected to spray drying. The inlet temperature of the spray dryer is 210℃ and the outlet temperature is 95℃ to obtain a solid powder disperse dye composition product.

[0201] Comparative Example 1

[0202] This comparative example provides a disperse dye composition that differs from Example 1 in that: instead of adding a composite dispersant, a single dispersant (sodium naphthalenesulfonate formaldehyde condensate) is used, while the remaining components and preparation process are the same as in Example 1.

[0203] Comparative Example 2

[0204] This comparative example provides a disperse dye composition that differs from Example 1 in that no leveling agent or anti-migratory agent is added, while the remaining components and preparation process are the same as in Example 1.

[0205] Comparative Example 3

[0206] This comparative example provides a disperse dye composition that differs from Example 1 in that it does not contain a pH buffer or antioxidant, while the remaining components and preparation process are the same as in Example 1.

[0207] Comparative Example 4

[0208] This comparative example provides a disperse dye composition that differs from Example 1 in that the composite dispersant consists only of two components: sodium naphthalene sulfonate formaldehyde condensate and sodium lignin sulfonate (mass ratio 1:1), and does not contain alkyl naphthalene sulfonate formaldehyde condensate or polycarboxylate dispersant. The remaining components and preparation process are the same as in Example 1.

[0209] Comparative Example 5

[0210] This comparative example provides a disperse dye composition that differs from Example 1 in that the heterocyclic disperse dye is replaced with an equal amount of azo disperse dye, i.e., the composition contains only two types of disperse dyes, azo and anthraquinone, and does not contain heterocyclic disperse dyes. The remaining components and preparation process are the same as in Example 1.

[0211] Comparative Example 6

[0212] This comparative example provides a disperse dye composition that differs from Example 1 in that no bactericide or preservative is added, while the remaining components and preparation process are the same as in Example 1.

[0213] Performance testing: The performance of the disperse dye compositions prepared in Examples 1-3 and Comparative Examples 1-3 of this invention was tested and compared.

[0214] I. Dyeing Rate Test

[0215] Dye uptake test method: The disperse dye compositions prepared in each example and comparative example were formulated into dye baths with a mass fraction of 2%. Polyester fabrics were dyed using a high-temperature and high-pressure dyeing machine at a dyeing temperature of 130℃ for 60 minutes and a liquor ratio of 1:20. After dyeing, the absorbance of the dye in the dyeing residue was determined by spectrophotometry. The dye uptake rate was calculated using the following formula: Dye uptake rate (%) = (1 – absorbance of dyeing residue / absorbance of original dyeing liquor) × 100%. The dye uptake rate test results for each sample are listed in Table 3.

[0216] Table 3 Comparison of dyeing rates between each example and the comparative example

[0217] sample Dyeing rate (%) Example 1 96.8 Example 2 95.9 Example 3 96.2 Comparative Example 1 86.3 Comparative Example 2 84.7 Comparative Example 3 88.1 Comparative Example 4 89.5 Comparative Example 5 85.8 Comparative Example 6 95.2

[0218] As shown in Table 3, the dyeing rates of Examples 1-3 all reached over 95%, with little difference between them, while the dyeing rates of Comparative Examples 1-6 were all lower than those of the Examples. Particularly noteworthy is that the dyeing rate of Comparative Example 4 (composite dispersant containing only two components) was 89.5%, significantly lower than the 96.8% of Example 1, a difference of 7.3 percentage points; the dyeing rate of Comparative Example 5 (without heterocyclic disperse dyes) was 85.8%, the lowest among all samples. This indicates that all four components of the composite dispersant are indispensable, and there is a significant synergistic effect among the four components; the absence of any one component will lead to a significant decrease in the dyeing rate. Simultaneously, the combination of azo, anthraquinone, and heterocyclic dyes also produced a synergistic effect; the absence of heterocyclic dyes would significantly reduce the dyeing rate. The dyeing rate of Comparative Example 6 (without bactericides and preservatives) was 95.2%, slightly lower than that of Example 1, but the difference was small, indicating that the direct impact of bactericides and preservatives on the dyeing rate is limited, and their main contribution lies in storage stability.

[0219] II. Lifting Force Test

[0220] Lifting power test method: The disperse dye compositions prepared in each example and comparative example were formulated into dye baths with different mass fractions (0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%). Polyester fabrics were dyed using a high-temperature, high-pressure dyeing method at 130℃ for 60 minutes, with a liquor ratio of 1:20. After dyeing, the apparent color depth of the dyed fabrics was measured using a colorimeter. The relative color depth values ​​at different mass fractions were calculated based on the apparent color depth value at a 2.0% mass fraction dyeing concentration. The results are listed in Table 4.

[0221] Table 4. Relative color depth values ​​of each embodiment and comparative example under different dye dosages.

[0222] sample 0.5% 1.0% 1.5% 2.0% 2.5% 3.0% Example 1 0.62 0.95 1.32 1.78 2.55 3.10 Example 2 0.60 0.93 1.28 1.75 2.48 3.02 Example 3 0.61 0.94 1.30 1.76 2.52 3.06 Comparative Example 1 0.55 0.82 1.10 1.45 1.92 2.30 Comparative Example 2 0.52 0.78 1.05 1.38 1.75 2.10 Comparative Example 3 0.57 0.85 1.15 1.50 2.02 2.45 Comparative Example 4 0.56 0.84 1.13 1.48 1.98 2.38 Comparative Example 5 0.53 0.80 1.08 1.42 1.88 2.25 Comparative Example 6 0.60 0.92 1.28 1.74 2.45 2.98

[0223] As shown in Table 4, the relative color depth values ​​of all samples increased with increasing dye mass fraction, but the rate of increase for Examples 1-3 was significantly faster than that for Comparative Examples 1-6. At a mass fraction of 3.0%, the relative color depth value of Example 1 reached 3.10, while that of Comparative Example 4 was only 2.38 and that of Comparative Example 5 was only 2.25. This indicates that the complete composition of the composite dispersant (four components) and the complete combination of the three types of dyes play a crucial role in enhancing the dyeing performance; the absence of any one of these elements will lead to a significant decrease in the enhancing performance. The enhancing performance of Comparative Example 6 (without bactericides and preservatives) was close to that of Example 1, further illustrating that the main function of bactericides and preservatives is not to enhance dyeing performance.

[0224] III. High Temperature Dispersion Stability Test

[0225] The high-temperature dispersion stability test method is the same as described in Example 1. The samples of each example and comparative example were tested, and the results are listed in Table 5.

[0226] Table 5. High-temperature dispersion stability (absorbance retention rate, %) of each example and comparative example.

[0227] sample 15min 30min 45min 60min Example 1 99.2 98.5 97.6 96.8 Example 2 98.8 98.0 97.1 96.2 Example 3 99.0 98.3 97.3 96.5 Comparative Example 1 95.6 92.3 88.7 84.2 Comparative Example 2 97.2 95.8 93.5 90.8 Comparative Example 3 98.1 96.9 95.2 93.4 Comparative Example 4 96.8 94.1 91.2 87.6 Comparative Example 5 97.5 95.3 92.8 89.4 Comparative Example 6 98.5 97.2 95.8 94.1

[0228] As shown in Table 5, after being kept at 130℃ for 60 minutes, Examples 1-3 all exhibited absorbance retention rates above 96%, demonstrating excellent high-temperature dispersion stability. Comparative Example 4 (composite dispersant containing only two components) showed an absorbance retention rate of only 87.6% after 60 minutes, and Comparative Example 5 (without heterocyclic dyes) showed 89.4%, both significantly lower than the 96.8% of Example 1. This fully demonstrates the significant synergistic effect among the four components of the composite dispersant of the present invention and the three types of dyes, jointly ensuring the high-temperature dispersion stability of the dye composition. The high-temperature dispersion stability of Comparative Example 6 (without bactericides and preservatives) was only slightly different from that of Example 1, further illustrating that the contribution of bactericides and preservatives to high-temperature dispersion stability is limited.

[0229] IV. Evenness Test

[0230] Evenness testing method: The disperse dye compositions prepared in each example and comparative example were formulated into dye baths with a mass fraction of 2%. Polyester fabrics were dyed using a high-temperature, high-pressure dyeing method at 130℃ for 60 minutes, with a liquor ratio of 1:20. After dyeing, 10 points were evenly selected along the weft direction of the dyed fabric. The color difference value at each point was measured using a colorimeter, and the standard deviation of the color difference was calculated. The evenness was evaluated by the magnitude of the standard deviation; a smaller standard deviation indicated better evenness. The results are listed in Table 6.

[0231] Table 6. Evenness of dyeing (standard deviation of color difference ΔE) of each example and comparative example.

[0232] sample Color difference standard deviation (ΔE) Example 1 0.32 Example 2 0.38 Example 3 0.35 Comparative Example 1 0.67 Comparative Example 2 1.24 Comparative Example 3 0.71 Comparative Example 4 0.72 Comparative Example 5 0.85 Comparative Example 6 0.35

[0233] As shown in Table 6, the color difference standard deviations of Examples 1-3 were all below 0.40, exhibiting excellent leveling properties. The color difference standard deviation of Comparative Example 5 (without heterocyclic dyes) was 0.85, significantly higher than the 0.32 of Example 1, indicating that the addition of heterocyclic disperse dyes plays an important role in improving the leveling performance of the dye composition. The rational blending of the three types of dyes not only broadens the chromatographic range but also improves the affinity differences of each dye component for the fiber through intermolecular interactions, thereby enhancing leveling properties. The leveling properties of Comparative Example 6 (without bactericides and preservatives) were basically consistent with those of Example 1, and the bactericides and preservatives had no significant effect on leveling properties.

[0234] V. Various fastness tests

[0235] The disperse dye compositions prepared in each example and comparative example were used to dye polyester fabrics according to the standard dyeing process, and then the fastness properties of the dyed fabrics were measured according to national standards.

[0236] The fastness to washing was tested in accordance with GB / T3921-2008 "Textiles - Tests for color fastness to soap washing".

[0237] The rubbing fastness was tested in accordance with GB / T3920-2008 "Textiles - Tests for color fastness - Color fastness to rubbing".

[0238] Sublimation fastness was tested in accordance with GB / T5718-1997 "Textiles - Tests for color fastness to dry heat (sublimation)"

[0239] The light fastness was tested in accordance with GB / T8427-2008 "Textiles - Tests for color fastness to artificial light: Xenon arc".

[0240] The test results (rated from 1 to 5, with 5 being the best) are listed in Table 7.

[0241] Table 7. Fastness performance ratings for each embodiment and comparative example.

[0242] sample Wash fastness Abrasion resistance (dry / wet) Sublimation fastness Sunlight fastness Example 1 4-5 4-5 / 4 4-5 4 Example 2 4-5 4-5 / 4 4 4-5 Example 3 4 4-5 / 4 4-5 4 Comparative Example 1 3-4 4 / 3-4 3-4 3-4 Comparative Example 2 3-4 3-4 / 3 3 3-4 Comparative Example 3 4 4 / 3-4 3-4 3 Comparative Example 4 3-4 4 / 3-4 3-4 3-4 Comparative Example 5 3-4 3-4 / 3 3 3-4 Comparative Example 6 4-5 4-5 / 4 4-5 4

[0243] As shown in Table 7, the fastness properties of Examples 1-3 all reached grade 4 or 4-5, significantly better than Comparative Examples 1-5. Comparative Example 5 (without heterocyclic dyes) had a sublimation fastness of only grade 3, the lowest among all samples, indicating that the addition of heterocyclic disperse dyes plays an important role in improving sublimation fastness. The fastness properties of Comparative Example 6 (without bactericides and preservatives) were basically the same as those of Example 1, and the bactericides and preservatives had no significant effect on the fastness properties.

[0244] VI. Storage Stability Test

[0245] The liquid disperse dye compositions prepared in each example and comparative example were subjected to accelerated storage at a constant temperature of 45°C for 90 days. Samples were taken on days 0, 30, 60, and 90 to measure the changes in average particle size and viscosity of the dye particles to evaluate storage stability. The results are listed in Tables 8 and 9.

[0246] Table 8. Average particle size change (nm) after accelerated storage for each example and comparative example.

[0247] sample 0 days 30 days 60 days 90 days Example 1 320 325 332 341 Example 2 335 342 350 358 Example 3 328 334 342 350 Comparative Example 1 380 420 485 560 Comparative Example 2 400 450 520 610 Comparative Example 3 360 400 465 540 Comparative Example 4 370 415 480 555 Comparative Example 5 390 435 505 590 Comparative Example 6 325 410 520 680

[0248] Table 9. Viscosity changes (mPa·s) after accelerated storage for each example and comparative example.

[0249] sample 0 days 30 days 60 days 90 days Example 1 85 88 92 98 Example 2 90 94 98 105 Example 3 88 91 96 102 Comparative Example 1 120 155 210 280 Comparative Example 2 135 175 240 320 Comparative Example 3 110 145 195 260 Comparative Example 4 115 150 205 275 Comparative Example 5 125 165 225 305 Comparative Example 6 88 165 285 420

[0250] As shown in Tables 8 and 9, after 90 days of accelerated storage at 45°C, Examples 1-3 exhibited excellent storage stability, with an average particle size increase of no more than 25 nm and a viscosity increase of no more than 20 mPa·s. Comparative Example 6 (without bactericides or preservatives) showed a sharp increase in particle size and viscosity after 30 days of storage, reaching an average particle size of 680 nm and a viscosity of 420 mPa·s after 90 days, exhibiting severe aggregation and spoilage. This indicates that the addition of bactericides and preservatives is crucial for the long-term storage stability of liquid disperse dye compositions and is an indispensable component for ensuring the commercial application of the product.

[0251] The storage stability of Comparative Example 4 (composite dispersant containing only two components) and Comparative Example 5 (excluding heterocyclic dyes) was also significantly worse than that of Example 1, further demonstrating the importance of the complete composition of the composite dispersant and the complete combination of the three types of dyes to the overall performance of the product.

[0252] VII. Effect of dyeing temperature on dyeing rate (Example 1)

[0253] The disperse dye composition prepared in Example 1 was formulated into a dye bath with a mass fraction of 2%, and polyester fabrics were dyed at different temperatures (90, 100, 110, 120, 130, 140°C) for 60 minutes each, with a liquor ratio of 1:20. The dyeing rate at each temperature was measured, and the results are listed in Table 10.

[0254] Table 10 Dyeing rates at different dyeing temperatures (Example 1)

[0255] Staining temperature (°C) 90 100 110 120 130 140 Dyeing rate (%) 42.3 55.8 74.6 88.1 96.8 97.5

[0256] As shown in Table 10, the dye uptake rate gradually increases with increasing dyeing temperature. Below 100°C, the dye uptake rate is relatively low, approximately 40-60%; at 110°C, it reaches approximately 75%; at 120°C, it reaches approximately 88%; at 130°C, it reaches approximately 96%; and when the temperature continues to rise to 140°C, the dye uptake rate increases slightly to approximately 97.5%, but the increase slows significantly. This indicates that the disperse dye composition of the present invention exhibits excellent dyeing performance in the temperature range of 120-140°C, and is particularly suitable for use under conventional high-temperature and high-pressure dyeing conditions at around 130°C.

[0257] VIII. Effect of dyeing time on dyeing rate (Example 1)

[0258] The disperse dye composition prepared in Example 1 was formulated into a dye bath with a mass fraction of 2%, and polyester fabric was dyed at 130°C with a liquor ratio of 1:20. Samples were taken at different dyeing times (5, 10, 15, 20, 30, 45, 60, and 75 minutes) to determine the dyeing rate. The results are listed in Table 11.

[0259] Table 11. Staining rate at different staining times (Example 1)

[0260] Staining time (min) 5 10 15 20 30 45 60 75 Dyeing rate (%) 32.5 65.4 78.2 85.6 92.3 95.1 96.8 97.0

[0261] As shown in Table 11, in the initial stage of dyeing (0-10 minutes), the dye uptake rate increases rapidly from approximately 32% to approximately 65%; in the middle stage of dyeing (10-30 minutes), the dye uptake rate continues to increase, but the rate of increase slows down, from approximately 65% ​​to approximately 92%; in the later stage of dyeing (30-60 minutes), the dye uptake rate tends to level off, slowly increasing from approximately 92% to approximately 97%; after 60 minutes, the dye uptake rate basically stops increasing, reaching dyeing equilibrium. This indicates that the disperse dye composition of the present invention has a moderate dye uptake rate, reaching dyeing equilibrium within 60 minutes, which meets the time requirements for industrial production.

[0262] IX. Effect of dye bath pH on dyeing rate (Example 1)

[0263] The disperse dye composition prepared in Example 1 was formulated into a dye bath with a mass fraction of 2%. The pH values ​​of the dye bath were adjusted to 3, 4, 5, 6, 7, 8, 9, and 10 with acetic acid and sodium acetate, respectively. Polyester fabrics were dyed at 130°C for 60 minutes with a liquor ratio of 1:20. The dyeing rate at each pH was measured, and the results are listed in Table 12.

[0264] Table 12 Dyeing rates at different dye bath pH values ​​(Example 1)

[0265] pH value 3 4 5 6 7 8 9 10 Dyeing rate (%) 93.8 95.5 96.8 96.5 95.9 94.2 90.8 83.5

[0266] As shown in Table 12, within the acidic pH range of 3-5, the dye uptake rate increases slightly with increasing pH, from approximately 94% to approximately 97%; within the pH range of 5-7, the dye uptake rate remains at a relatively high level of around 96%; within the pH range of 7-9, the dye uptake rate begins to gradually decrease, from approximately 96% to approximately 91%; and at pH values ​​greater than 9, the decrease in dye uptake rate accelerates significantly. This indicates that the disperse dye composition of the present invention exhibits optimal dyeing performance within the pH range of 4-7, and maintains a good dye uptake rate within a wider pH range of 3-9. This is attributed to the pH buffer added in the present invention, which maintains a stable pH value in the dye bath during the dyeing process, avoiding dye hydrolysis and a decrease in dye uptake rate due to pH fluctuations.

[0267] 10. Detailed test of water wash fastness (Example 1)

[0268] The polyester fabric dyed in Example 1 was subjected to a wash fastness test according to GB / T3921-2008. The color fastness and the staining fastness to polyester, cotton, wool and acrylic interlinings were evaluated respectively. The results are listed in Table 13.

[0269] Table 13 Detailed rating of wash fastness in Example 1

[0270] project Color fastness Color fastness (polyester) Color fastness (cotton) Colorfastness (wool) Color fastness (acrylic fiber) Rating (Level) 4-5 4-5 4 4-5 4-5

[0271] As shown in Table 13, the color fastness of Example 1 reaches grade 4-5, the staining fastness to polyester interlining reaches grade 4-5, the staining fastness to cotton interlining reaches grade 4, the staining fastness to wool interlining reaches grade 4-5, and the staining fastness to acrylic interlining reaches grade 4-5. This indicates that the polyester fabric dyed with the disperse dye composition of the present invention has excellent wash fastness, is not easily faded during washing, and is not easily stained by other fibers.

[0272] XI. Detailed Test of Sublimation Fastness (Example 1)

[0273] The polyester fabric dyed in Example 1 was subjected to sublimation fastness test according to GB / T5718-1997. It was dry heat treated at 150℃, 180℃ and 210℃ respectively, and the color change fastness and staining fastness were evaluated. The results are listed in Table 14.

[0274] Table 14 Sublimation fastness ratings at different temperatures in Example 1

[0275] Processing temperature (°C) Colorfastness (grade) Colorfastness (grade) 150 4-5 4-5 180 4 4-5 210 3-4 4

[0276] As shown in Table 14, under treatment conditions of 150℃, the color fastness is grade 4-5, and the staining fastness is grade 4-5; under treatment conditions of 180℃, the color fastness is grade 4, and the staining fastness is grade 4-5; under treatment conditions of 210℃, the color fastness is grade 3-4, and the staining fastness is grade 4. This indicates that the polyester fabric dyed with the disperse dye composition of the present invention has good sublimation fastness and can maintain good color fastness under conventional heat setting conditions (around 180℃).

[0277] The disperse dye composition and its preparation process of this invention have broad industrial application prospects. The disperse dye composition provided by this invention can be widely used in the dyeing and printing of hydrophobic fiber materials such as polyester fiber, polyamide fiber, acetate fiber, and polylactic acid fiber. It is suitable for various dyeing processes such as high-temperature and high-pressure dyeing, hot-melt dyeing, and carrier dyeing, as well as various printing processes such as direct printing, discharge printing, and resist printing. The preparation process of this invention is simple, convenient to operate, has high production efficiency, and produces stable product quality, making it suitable for large-scale industrial production.

[0278] The embodiments described herein are preferred embodiments of the present invention and are not intended to limit the scope of protection of the present invention. Therefore, all equivalent changes made in accordance with the structure, shape, and principle of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A disperse dye composition, characterized in that, Based on parts by mass, it includes the following components: Component A: 20-50 parts of azo disperse dye; Component B: 10-35 parts of anthraquinone disperse dye; Component C: 5-25 parts of heterocyclic disperse dyes; Component D: 8-20 parts of composite dispersant; Component E: 2-8 parts of leveling agent; Component F: 1-5 parts of anti-migratory agent; Component G: 0.5-3 parts of pH buffer; Component H: 0.1~1.5 parts of antioxidant; Component I: 0.05~0.5 parts of bactericide and preservative; The composite dispersant is composed of the following components in parts by weight: 30-60 parts of sodium naphthalene sulfonate formaldehyde condensate, 20-40 parts of sodium lignosulfonate, 10-30 parts of alkyl naphthalene sulfonate formaldehyde condensate, and 5-15 parts of polycarboxylate dispersant. The heterocyclic disperse dyes are disperse dyes containing thiazole rings, benzothiazole rings, or quinoline ring structures.

2. The disperse dye composition according to claim 1, characterized in that, The leveling agent is selected from one or more of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyethylene glycol fatty acid ester, and polyvinylpyrrolidone.

3. The disperse dye composition according to claim 1, characterized in that, The anti-migratory agent is selected from one or more of sodium polyacrylate, sodium carboxymethyl cellulose, sodium alginate, and polyethylene glycol.

4. The disperse dye composition according to claim 1, characterized in that, The pH buffer is selected from one of the following: sodium dihydrogen phosphate-disodium hydrogen phosphate buffer pair, acetate-sodium acetate buffer pair, and citric acid-sodium citrate buffer pair.

5. The disperse dye composition according to claim 1, characterized in that, The antioxidant is selected from one or more of butylated hydroxyanisole, butylated hydroxytoluene, propyl gallate, and tocopherol; the bactericide and preservative is selected from one or more of isothiazolinone compounds and benzisothiazolinone compounds.

6. The disperse dye composition according to claim 1, characterized in that, Based on parts by mass, it includes the following components: Component A: 30-40 parts of azo disperse dye; Component B: 15-25 parts of anthraquinone disperse dye; Component C: 10-18 parts of heterocyclic disperse dyes; Component D: 12-16 parts of composite dispersant; Component E: 4-6 parts of leveling agent; Component F: 2-3 parts of anti-migratory agent; Component G: 1-2 parts of pH buffer; Component H: 0.3~0.8 parts of antioxidant; Component I: 0.1~0.3 parts of bactericide and preservative.

7. The disperse dye composition according to claim 1, characterized in that, The azo disperse dyes are one or more of CI disperse yellow, CI disperse orange, CI disperse red, and CI disperse blue; the anthraquinone disperse dyes are one or more of CI disperse violet, CI disperse blue, and CI disperse turquoise blue; and the heterocyclic disperse dyes are one or more of CI disperse yellow, CI disperse red, and CI disperse blue.

8. The preparation process of a disperse dye composition according to any one of claims 1 to 7, characterized in that, Includes the following steps: Step 1: Weigh each component according to the formula amount, and premix the azo disperse dye, anthraquinone disperse dye and heterocyclic disperse dye to obtain the dye premix; Step 2: Add the composite dispersant, leveling agent, anti-migration agent, pH buffer, antioxidant, and bactericide / preservative to deionized water, and heat under stirring to dissolve them, thus obtaining the auxiliary agent solution; Step 3: Add the dye premix obtained in Step 1 to the auxiliary agent solution obtained in Step 2, and perform high-speed dispersion and mixing to obtain a coarse dispersion slurry; Step 4: Grind the coarse dispersion slurry obtained in Step 3 to make the particle size of the dye particles meet the specified requirements, and obtain a fine dispersion slurry. Step 5: Filter the finely dispersed slurry obtained in Step 4 to remove impurities, and obtain the liquid dispersed dye composition product; Step 6: Dry the liquid disperse dye composition product obtained in Step 5 to obtain a solid powder or granular disperse dye composition product.

9. The preparation process of a disperse dye composition according to claim 8, characterized in that, The premixing described in step one is carried out using a V-type mixer or a double cone mixer, with a mixing time of 10-30 minutes and a mixing speed of 10-30 rpm; In step two, the amount of deionized water used is 1.5 to 3 times the total mass of the dye premix, the heating and dissolving temperature is 40 to 80°C, the stirring speed is 200 to 600 rpm, and the stirring time is 15 to 45 minutes. The high-speed dispersion described in step three is carried out using a high-speed disperser with a dispersion speed of 1000~3000 rpm and a dispersion time of 20~60 minutes; The grinding process described in step four is carried out using a horizontal sand mill or a vertical bead mill. The grinding media are zirconia beads or glass beads with a particle size of 0.3~1.5 mm, a grinding temperature of 10~40℃, and a grinding time of 1~5 hours. The specified requirements are that the average particle size of the dye particles is not greater than 500 nanometers and the particle size distribution span is not greater than 1.

5. The filtration described in step five is performed using microporous filtration or membrane filtration, with a filtration accuracy of 0.5~5 micrometers; The drying process described in step six is ​​carried out by spray drying, with an inlet temperature of 150~220℃ and an outlet temperature of 70~100℃.

10. The use of a disperse dye composition according to any one of claims 1 to 7 in dyeing and / or printing hydrophobic fiber materials, characterized in that, The hydrophobic fiber material is one or more of polyester fiber, polyamide fiber, acetate fiber, and polylactic acid fiber, or a blend of the above fibers with other fibers.

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