Dyeing method and application of sulfur dye

By controlling the order and time of addition of reducing agents during the sulfur dye dye dye, ensuring sufficient reduction potential, the problem of reduction potential loss during the sulfur dye dye dye dye dye dye dye is solved, and uniform dyeing effect and high-quality dyeing fabrics are achieved.

CN120401250APending Publication Date: 2025-08-01GUANGDONG ZHENYUAN TEXTILE TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510523134.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-24
Publication Date
2025-08-01

AI Technical Summary

Technical Problem

The existing technology processes are complex and difficult to control due to the loss of reduction potential during the dyeing process of sulfurized dyes.

Method used

After the alkali treatment is used, the insulating powder and glucose are added as the reducing agent, and then the sulfurized dye is added. The order and time of addition of the reducing agent are controlled through oxidation treatment to ensure sufficient reduction potential and avoid oxidation of the reducing agent and air.

Benefits of technology

It significantly reduces dyeing and color circle phenomena, ensures uniformity and color depth of dyeing effect, and improves dye utilization and color fastness.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a dyeing method of a sulfur dye, which comprises the following steps: providing a to-be-dyed fabric, treating the to-be-dyed fabric by using alkali liquor, preparing a first treated fabric, treating the first treated fabric for a preset time by using a first reducing agent, adding a second reducing agent for treating for a preset time, and adding the sulfur dye for reaction. Preparing a second treated fabric; the first reducing agent comprises sodium hydrosulfite and / or thiourea dioxide; according to the method, the reduction-oxidation process of the sulfur dye is regulated and controlled, so that reduction potential deficiency caused by oxidation of the reducing agents is greatly reduced, sufficient reduction potential in a system is ensured, the sulfur dye is fully reduced, and the dyeing quality is improved. The problems of easy dyeing flower, color circle, inside and outside color difference and the like of the fabric in the traditional dyeing process are obviously reduced, and the dyeing effect of sulfur dye is ensured.
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Description

Technical Field

[0001] The present invention relates to the technical field of textile printing and dyeing, and particularly relates to a dyeing method and application of sulfur dyes. Background Art

[0002] Sulfur dyes are a class of dyes that can only be dyed after reduction. Sulfur dyes are insoluble in water. When dyeing, sodium sulfide or other reducing agents are required to reduce the dyes into soluble leuco bodies, so that the dyes have an affinity for cellulose and dye the fibers. Then, after oxidation, they are restored to the original insoluble dyes and fixed on the fibers. Based on the binding mode of the sulfur dyes and the fibers, compared with the dyeing of reactive dyes, the use of sulfur dyes can avoid color fading caused by bond breakage after washing like reactive dyes, and can be used to improve the problem of abrasion whitening of fabrics after washing. However, sulfur dyes are accompanied by reduction-oxidation reactions during the dyeing process. Therefore, during the reduction process, the reducing agent is prone to oxidation reaction, resulting in the lack of reduction potential. Therefore, the sulfur dyeing process in the production process is complex and requires high requirements. If the process design is unreasonable, it is very easy to cause problems such as dyeing flowers, color rings, and internal and external color differences. Summary of the Invention

[0003] Based on this, it is necessary to provide a dyeing method of sulfur dyes that can provide sufficient reduction potential for sulfur dyes and ensure the dyeing effect.

[0004] In the first aspect, the present invention provides a dyeing method of sulfur dyes, including the following steps:

[0005] Provide a fabric to be dyed;

[0006] Treat the fabric to be dyed with an alkali solution to prepare a first treated fabric;

[0007] Treat the first treated fabric with a first reducing agent for a predetermined time, add a second reducing agent and treat for a predetermined time, and add sulfur dyes for reaction to prepare a second treated fabric; the first reducing agent includes sodium dithionite and / or thiourea dioxide; the second reducing agent includes glucose;

[0008] Oxidize the second treated fabric to prepare a dyed fabric.

[0009] In some embodiments, the concentration of the first reducing agent is 1 g / L - 6 g / L; and / or, the concentration of the second reducing agent is 5 g / L - 20 g / L.

[0010] Optionally, the treatment time of the first reducing agent on the first treated fabric is 5 min - 20 min; and / or, the treatment time of the second reducing agent is 5 min - 20 min.

[0011] In some embodiments, before treating the fabric to be dyed with an alkali solution, it further includes treating the fabric to be dyed with a dye accelerator;

[0012] Optionally, the dye accelerator is selected from one or more of sodium sulfate, sodium chloride, calcium chloride, and potassium chloride;

[0013] Optionally, the concentration of the dye accelerator is 20 g / L - 50 g / L;

[0014] Optionally, the temperature for treating with the dye accelerator is 20°C - 60°C;

[0015] Optionally, the time for treating with the dye accelerator is 5 min - 35 min.

[0016] In some embodiments, the alkali solution includes one or several alkali agents such as sodium hydroxide, potassium hydroxide, urea, potassium hydrogen phosphate, potassium dihydrogen phosphate, ammonium sulfate, sodium carbonate, and sodium bicarbonate; and / or, the addition amount of the alkali agent is 6 g / L - 15 g / L.

[0017] In some embodiments, the temperature for treating with the alkali solution is 20°C - 80°C; and / or, the time for treating with the alkali solution is 5 min - 20 min.

[0018] In some embodiments, a scouring agent and / or a dispersant are further added to the alkali solution;

[0019] Optionally, the scouring agent includes one or more of an alkaline scouring agent, an acidic scouring agent, a neutral scouring agent, and an enzyme preparation scouring agent;

[0020] Optionally, the dispersant includes a chemically synthesized dispersant and / or a natural polymer.

[0021] In some embodiments, the concentration of the scouring agent is 0.5 g / L - 3 g / L; and / or, the concentration of the dispersant is 0.5 g / L - 3 g / L.

[0022] In some embodiments, the reaction temperature for adding the sulfur dye is 90°C - 100°C.

[0023] In some embodiments, the oxidation treatment further satisfies the following (1) and / or (2):

[0024] (1) The oxidant components in the oxidation treatment process include one or more of hydrogen peroxide, sodium hypochlorite, sodium chlorite, persulfates, and ozone;

[0025] Optionally, an acid agent is further added to the oxidant;

[0026] (2) The concentration of the oxidant in the oxidation treatment process is 3 g / L - 10 g / L.

[0027] Compared with the traditional dyeing technology of sulfur dyes, the beneficial effects of the technology of the present invention are as follows:

[0028] By improving the traditional dyeing process of sulfur dyes and regulating the reduction-oxidation process of sulfur dyes, the present invention greatly reduces the loss of reduction potential caused by the reaction of reducing agents with oxygen in the air, ensures sufficient reduction potential in the system, enables the full reduction of sulfur dyes, significantly reduces problems such as easy dyeing defects, color rings, and internal and external color differences in the traditional dyeing process, and ensures the dyeing effect of sulfur dyes. Description of the Drawings

[0029] Figure 1 It is a schematic diagram of the dyeing process flow of the sulfur dye of the present invention. Detailed Embodiments

[0030] To facilitate the understanding of the present invention, the following provides a more comprehensive description of the technical solution of the present invention with reference to the preferred embodiments of the present invention. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0031] It should be noted that the experimental methods without specific conditions in the following embodiments of the present invention are usually carried out under conventional conditions or according to the conditions recommended by the manufacturers. All common chemical reagents used in the embodiments are commercially available products.

[0032] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which the present invention belongs. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0033] In the present application, in relation to "the first aspect", "the second aspect", "the third aspect", "the fourth aspect", etc., the terms "first", "second", "third", "fourth", etc. are only for descriptive purposes and cannot be understood as indicating or implying relative importance or quantity, nor can they be understood as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first", "second", "third", "fourth", etc. only serve the purpose of non-exhaustive enumerative description and should be understood not to constitute a closed limitation on quantity.

[0034] The term "bath ratio" is a term in textile dyeing and finishing, referring to the mass ratio of the fabric to the dye liquor (or treatment liquor) in the impregnation method; also known as the liquor ratio, referring to the weight ratio of the fabric to the dye liquor (or treatment liquor).

[0035] The term "owf" means "on weight of fabric", referring to the dye concentration. In this embodiment, based on the weight of the yarn, for example, for 686 kg of yarn, adding 10% dye means adding 68.6 kg of dye.

[0036] During the dyeing process of sulfur dyes, the reactions between various raw materials and reagents will affect the reduction effect of the sulfur dyeing process. Therefore, during the sulfur dyeing process, the feeding time, feeding amount, and treatment time of the reducing agent need to be strictly controlled and inspected. Otherwise, when the reducing agent undergoes an oxidation reaction with air in the vat, resulting in insufficient reduction potential when the dye is added, problems such as light color and color streaks will occur. Therefore, the dosage and feeding operation of the reducing reagent need to be particularly controlled to ensure that fabrics with uniform color and high quality can be produced. The present invention aims to solve the technical problems of insufficient reduction potential, large feeding amount, and poor dyeing effect during the sulfur dyeing process.

[0037] In a first aspect, the present invention provides a method for dyeing sulfur dyes. The specific process flow is shown in the appendix Figure 1 as follows, including the following steps:

[0038] S10. Provide the fabric to be dyed.

[0039] S20. Treat the fabric to be dyed with an alkali solution to prepare a first treated fabric.

[0040] S30. Treat the first treated fabric with a first reducing agent for a predetermined time, add a second reducing agent and treat for a predetermined time, and add sulfur dye for reaction to prepare a second treated fabric; the first reducing agent includes sodium hydrosulfite and / or thiourea dioxide; the second reducing agent includes glucose.

[0041] S40. Perform an oxidation treatment on the second treated fabric to prepare a dyed fabric.

[0042] In the method for dyeing sulfur dyes of the present invention, after treating the fabric to be dyed with an alkali solution, the first reducing agent and the second reducing agent are added successively and then the dye is added. This not only avoids the hydrolysis of the reducing dye caused by being exposed to the alkali solution for too long and reduces the oxidation process of the reducing agent, ensures sufficient reduction potential of the reducing agent, ensures that the dye can fully react with the reducing agent, ensures the reduction rate, and meets the utilization rate and dyeing quality of sulfur dyes. In addition, the present invention uses a first reducing agent including sodium hydrosulfite and / or thiourea dioxide and a second reducing agent including glucose for synergistic treatment, which can better meet the reduction effect of sulfur dyes.

[0043] The present invention strictly controls the addition order of the first reducing agent, the second reducing agent and the dye. When the dye is added in advance, there is not enough reduction potential, which will cause the dye to directly adhere to the inner part of the dye bobbin yarn, and there is not enough time for leveling.

[0044] In some embodiments, the concentration of the first reducing agent is 1 g / L - 6 g / L, including but not limited to 1 g / L, 2 g / L, 3 g / L, 4 g / L, 5 g / L, 6 g / L, or any concentration within the range formed by any two of the foregoing.

[0045] In some embodiments, the concentration of the second reducing agent is 5 g / L - 20 g / L, including but not limited to 5 g / L, 8 g / L, 10 g / L, 12 g / L, 15 g / L, 20 g / L, or any concentration within the range formed by any two of the foregoing.

[0046] By adding 1 g / L - 6 g / L of the first reducing agent and 5 g / L - 20 g / L of the second reducing agent, the present invention satisfies the sufficient reduction potential required by the sulfur dye, enables the sulfur dye to be rapidly and completely converted into the leuco form, makes the concentration of the leuco form reach the optimal state, is conducive to the dye fully dyeing the fiber, and can obtain a higher dyeing rate and dyeing depth. The fabric has bright and full colors and good color fastness. When the concentration of the reducing agent is lower than this addition range, the sulfur dye cannot be fully reduced, the concentration distribution of the leuco form is uneven, the amount of dye adsorbed on different parts of the fabric is different, and it is easy to cause uneven dyeing and color streaks; when the concentration of the reducing agent exceeds this addition range, it may cause excessive reduction of the dye leuco form, generating some unnecessary reduction products, which may affect the normal dyeing of the dye and make the dyeing effect worse, such as the color becoming lighter and the hue changing, etc.; at the same time, it causes too high reduction potential, destroys the stability of the dye, and also increases the economic cost.

[0047] In some embodiments, the first reducing agent treats the first treated fabric for a predetermined time of 5 min - 20 min, including but not limited to 5 min, 8 min, 10 min, 12 min, 15 min, 20 min, or any time within the range formed by any two of the foregoing.

[0048] In some embodiments, the second reducing agent is treated for a predetermined time of 5 min - 20 min, including but not limited to 5 min, 8 min, 10 min, 12 min, 15 min, 20 min, or any time within the range formed by any two of the foregoing.

[0049] Furthermore, the treatment time of the first reducing agent and the second reducing agent is respectively controlled within 5 min - 20 min, which can greatly improve the dispersibility of sulfur dyes in the reducing agent, prevent the aggregation or precipitation of sulfur dyes in the unreduced state, keep the dye molecules in a dispersed state, avoid affecting the dyeing uniformity due to over-large dye particles, and contribute to achieving uniform dyeing. Meanwhile, within this treatment time, there is no obvious potential drop in the reducing agent, which will not affect the reducibility of the reducing agent. Therefore, this process enables the reduction system to have sufficient reduction potential and obtain excellent dyeing effects.

[0050] In some embodiments, the first reducing agent and the second reducing agent are both added within 5 min - 20 min. By controlling the addition rate of the reducing agent, the reaction process between the reducing agent and air can be further reduced, ensuring sufficient reduction potential.

[0051] In some embodiments, the fabric to be dyed of the present invention is selected from linen, pure cotton, viscose, cotton-linen blend, cotton-tencel blend yarn, cotton-polyester blend, or cotton-nylon blend, but is not limited to the types of fabrics described above.

[0052] In some embodiments, the fabric to be dyed of the present invention is selected from pure cotton grey yarn with a density of 0.32 g / cm 3 - 0.42 g / cm 3

[0053] In some embodiments, the bath ratio for treating the fabric to be dyed with the alkali solution is 1:(4 - 20), including but not limited to 1:4, 1:5, 1:8, 1:10, 1:15, 1:20, or any bath ratio formed by any two of the foregoing and any bath ratio within the range.

[0054] In some embodiments, the fabric to be dyed of the present invention can be the fabric to be dyed after scouring and bleaching treatment.

[0055] In some embodiments, before treating the fabric to be dyed with the alkali solution, it further includes treating the fabric to be dyed with a dye accelerator.

[0056] In some embodiments, the dye accelerator is selected from one or more of sodium sulfate, sodium chloride, calcium chloride, and potassium chloride.

[0057] In some embodiments, the concentration of the dye accelerator is 20 g / L - 50 g / L, including but not limited to 20 g / L, 25 g / L, 30 g / L, 35 g / L, 40 g / L, 45 g / L, 50 g / L, or any concentration formed by any two of the foregoing and any concentration within the range.

[0058] ​In some embodiments, the temperature for treating with the accelerating agent is 20°C - 60°C, including but not limited to 20°C, 25°C, 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, or any temperature within the range formed by any two of the foregoing and any temperature within that range.

[0059] In some embodiments, the time for treating with the accelerating agent is 5 min - 35 min, including but not limited to 5 min, 8 min, 10 min, 15 min, 20 min, 25 min, 30 min, or any time within the range formed by any two of the foregoing and any time within that range.

[0060] In some embodiments, the process of treating the fabric to be dyed with the accelerating agent includes: first heating to 40°C - 60°C and treating for 5 min - 20 min, and then cooling to room temperature and treating for 5 min - 15 min.

[0061] Using the accelerating agent for treatment can further enhance the dyeing ability of the dye, thereby improving the dye uptake rate and dyeing rate of the fabric. At the same time, the accelerating agent helps to achieve a more uniform dyeing effect, ensure the same color on the fabric surface, and can improve the color and shade, color light, and dyeing fastness.

[0062] In some embodiments, the alkali solution includes one or several of sodium hydroxide, potassium hydroxide, urea, potassium hydrogen phosphate, potassium dihydrogen phosphate, ammonium sulfate, sodium carbonate, and sodium bicarbonate as alkali agents.

[0063] In some embodiments, the addition amount of the alkali agent is 6 g / L - 15 g / L, including but not limited to 6 g / L, 8 g / L, 10 g / L, 12 g / L, 15 g / L, or any addition amount within the range formed by any two of the foregoing and any addition amount within that range.

[0064] In some embodiments, the temperature for treating with the alkali solution is 20°C - 80°C, including but not limited to 20°C, 25°C, 30°C, 35°C, 40°C, or any temperature within the range formed by any two of the foregoing and any temperature within that range.

[0065] In some embodiments, the time for treating with the alkali solution is 5 min - 20 min, including but not limited to 5 min, 8 min, 10 min, 12 min, 15 min, 18 min, 20 min, or any time within the range formed by any two of the foregoing and any time within that range.

[0066] Using the process of treating with the alkali solution can make the sulfur dye better transform into hydrophilic molecules, dissolve fully in the aqueous phase / reducing agent, enable its dye molecules to react quickly and fully with the reducing agent, and improve the utilization rate and dyeing effect of the sulfur dye.

[0067] In some embodiments, a refining agent and / or a dispersant is also added to the lye.

[0068] In some embodiments, the refining agent includes one or more of an alkaline refining agent, an acidic refining agent, a neutral refining agent, and an enzyme preparation refining agent. By adding the refining agent in the present invention, it helps to remove impurities such as grease, wax, pectin, etc. on the fabric, as well as impurities such as sizing agents and oil agents remaining in the processing process, thereby improving the wettability of the fabric, promoting the contact between dye molecules and the fabric, facilitating the full contact between dye molecules and the fiber surface, enabling the dye molecules to better penetrate into the interior of the fabric, promoting dyeing, improving the uniformity and penetration of dyeing, and ensuring uniform dyeing and bright color.

[0069] In some embodiments, the dispersant includes a chemically synthesized dispersant and / or a natural polymer. Sulfide dyes have poor solubility in water and tend to form aggregates or precipitates. In the present invention, the added dispersant adsorbs on the surface of dye particles, and through steric hindrance and electrostatic repulsion, the dye particles are evenly dispersed in the dye solution, preventing the aggregation of dye particles and maintaining the stability and uniformity of the dye in the dye solution.

[0070] As non-exemplary, the chemically synthesized dispersant includes organic phosphates and / or phosphorus-free environmental protection types; further optionally, the phosphorus-free environmental protection type includes amino carboxylic acids and / or hydroxy carboxylic acids.

[0071] In some embodiments, the concentration of the refining agent is 0.5 g / L - 3 g / L, including but not limited to 0.5 g / L, 1 g / L, 1.5 g / L, 2 g / L, 2.5 g / L, 3 g / L, or any range formed by any two of the foregoing and any concentration within the range.

[0072] In some embodiments, the concentration of the dispersant is 0.5 g / L - 3 g / L, including but not limited to 0.5 g / L, 1 g / L, 1.5 g / L, 2 g / L, 2.5 g / L, 3 g / L, or any range formed by any two of the foregoing and any concentration within the range.

[0073] In some embodiments, the sulfur dye includes sulfur dyes.

[0074] In some embodiments, the composition of the sulfur dye contains auxiliaries such as sodium hydroxide and / or sodium hydrosulfide.

[0075] In some embodiments, the concentration of the sulfur dye is 0.01 g / L - 60 g / L, including but not limited to 0.01 g / L, 5 g / L, 10 g / L, 15 g / L, 20 g / L, 25 g / L, 30 g / L, 35 g / L, 40 g / L, 45 g / L, 50 g / L, 55 g / L, 60 g / L, or any range formed by any two of the foregoing and any concentration within the range.

[0076] In some embodiments, the sulfur dye is added completely within 5 min - 20 min, which can further ensure the reduction potential and reduction effect of the reducing agent and also ensure that the dye can be fully reduced.

[0077] In some embodiments, the reaction temperature for adding the sulfur dye is 90°C - 100°C, including but not limited to 90°C, 92°C, 95°C, 98°C, 100°C, or any temperature within the range formed by any two of the foregoing.

[0078] In some embodiments, after adding the sulfur dye for reaction, it further includes processes such as draining water and / or overflowing water for washing.

[0079] In some embodiments, the concentration of the oxidizing agent in the oxidation treatment process is 3 g / L - 10 g / L.

[0080] In some embodiments, the components of the oxidizing agent in the oxidation treatment process include one or more of hydrogen peroxide, sodium hypochlorite, sodium chlorite, persulfates, and ozone; further, using hydrogen peroxide for oxidation treatment in the present invention can better achieve the technical effects of the present invention.

[0081] In some embodiments, the concentration of the hydrogen peroxide is 3 g / L - 8 g / L, including but not limited to 3 g / L, 4 g / L, 5 g / L, 6 g / L, 7 g / L, 8 g / L, or any concentration within the range formed by any two of the foregoing.

[0082] In some embodiments, an acid agent is further added to the oxidizing agent.

[0083] In some embodiments, the acid agent is selected from one or more of glacial acetic acid, citric acid, hydrochloric acid, and sulfuric acid.

[0084] In some embodiments, the concentration of the acid agent is 0.2 g / L - 2 g / L, including but not limited to 0.2 g / L, 0.5 g / L, 0.8 g / L, 1 g / L, 1.5 g / L, 2 g / L, or any concentration within the range formed by any two of the foregoing.

[0085] In some embodiments, before the oxidation treatment, it further includes scouring the second treated fabric; optionally, scouring 2 - 3 times.

[0086] In some embodiments, the scouring agent used includes one or more of sodium dodecyl sulfate, polyvinylpyrrolidone, polymaleic anhydride, and sodium carbonate.

[0087] In some embodiments, the concentration of the soaping agent is 0.5 g / L - 2 g / L, including but not limited to 0.5 g / L, 0.8 g / L, 1 g / L, 1.5 g / L, 2 g / L, or any concentration within the range formed by any two of the foregoing and within that range.

[0088] In some embodiments, the temperature of the soaping is 40°C - 70°C, including but not limited to 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, or any temperature within the range formed by any two of the foregoing and within that range.

[0089] In some embodiments, the time of the soaping is 5 min - 20 min, including but not limited to 5 min, 8 min, 10 min, 12 min, 15 min, 18 min, 20 min, or any time within the range formed by any two of the foregoing and within that range.

[0090] In some embodiments, after the oxidation treatment, a water washing and / or alkali washing process is further included.

[0091] In some embodiments, the temperature of the water washing and / or alkali washing process is 40°C - 70°C, including but not limited to 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, or any temperature within the range formed by any two of the foregoing and within that range.

[0092] In some embodiments, the time of the water washing and / or alkali washing process is 5 min - 20 min, including but not limited to 5 min, 8 min, 10 min, 12 min, 15 min, 18 min, 20 min, or any time within the range formed by any two of the foregoing and within that range.

[0093] The dyeing method of the sulfur dye of the present invention can fully ensure the reduction potential during the dyeing process, ensure excellent dyeing effects of the sulfur dye, and at the same time prepare a dyed fabric with uniform dyeing and good color.

[0094] For the experimental parameters not specified in the following specific embodiments, preferably refer to the guidance given in the present application document, and may also refer to the experimental manuals in the art or other experimental methods known in the art, or refer to the experimental conditions recommended by the manufacturers.

[0095] The substrates and reagents involved in the following specific embodiments can be obtained commercially, or those skilled in the art can prepare them according to known means.

[0096] The models and sources of some raw materials and reagents used in the specific embodiments of the present invention are as follows:

[0097] Scouring agent: Model EPDC01, purchased from Kekai Fine Chemical Co., Ltd.

[0098] Dispersant: Model SQB-113, purchased from Fuying Chemical Co., Ltd.

[0099] Soap scouring agent: Model TF-231YA, purchased from Guangdong Transfar Fulian Fine Chemical Co., Ltd.

[0100] Example 1

[0101] The dyeing method of sulfur dyes in this example is as follows:

[0102] In a dyeing vat with a diameter of 1.8 meters, a single yarn with a weight of 1 kg and a density of 0.34 g / cm 3 -0.38 g / cm 3 of 40S pure cotton cheese yarn, with a yarn weight of 686 kg, a bath ratio of 1:6.3, and the dye used is DIR BLACK RDT-KAS.CN LIQ: 10% owf.

[0103] After scouring and bleaching the cotton grey yarn, put it into the vat, add clear water according to the bath ratio, add 20 g / L accelerating agent (sodium sulfate), then heat up to 50 °C and keep warm for 20 min, then cool down to room temperature and keep warm for 10 min, then add 0.5 g / L refining agent (EPDC01), 3 g / L dispersant (SQB-113) and 15 g / L alkali agent (sodium hydroxide), after keeping warm for 20 min, prepare the first treated fabric.

[0104] Then add 1 g / L of the first reducing agent (sodium hydrosulfite) to the first treated fabric, add the first reducing agent within 5 min and keep warm for 5 min, then add 20 g / L of glucose, add the glucose within 20 min and keep warm for 20 min, then add 20 g / L of sulfur dye, and at the same time heat up to 95 °C and react for 30 min, after draining the water, do overflow rinsing for 20 min to prepare the second treated fabric.

[0105] After the dyeing is completed, without opening the lid of the vat, immediately carry out sulfur post-treatment on the second treated fabric. First, use 0.5 g / L of soap scouring agent (TF-231YA) to do soap scouring at 50 °C for 15 min. After soap scouring 2 - 3 times, then add 3 g / L of hydrogen peroxide (mass concentration of 27.5%) and 0.2 g / L of acid agent (glacial acetic acid) for oxidation, the oxidation time is 20 min, after completion, wash with water at 50 °C for 20 min to prepare the dyed fabric.

[0106] The cheese yarn dyed by the above dyeing method did not show dyeing unevenness, made into weft plain color fabric, did not need to pick yarn, the utilization rate was 100%, and the fastness of washing, water stain, sweat stain, etc. was all 4.5 grades.

[0107] Example 2

[0108] The dyeing method of sulfur dyes in this example is as follows:

[0109] Dye a cylinder of single yarn weighing 1 kg with a density of 0.34 g / cm 3 -0.38 g / cm 3 in a dye vat with a diameter of 1.4 meters. The 80S / 2 pure cotton cheese yarn weighs 469 kg, the liquor ratio is 1:4.3, and the dye used is DIR BLACK RDT-KAS.CN LIQ: 10% owf.

[0110] Put the cotton grey yarn into the vat after scouring and bleaching, add clear water according to the liquor ratio, add 50 g / L accelerating agent (sodium sulfate), then heat up to 60 °C and keep warm for 5 min, then cool down to room temperature and run for 15 min, then add 3 g / L refining agent (EPDC01), 0.5 g / L dispersant (SQB-113) and 6 g / L alkali agent (sodium hydroxide), and run for 20 min to prepare the first treated fabric.

[0111] Then add 6 g / L of the first reducing agent (sodium hydrosulfite) to the first treated fabric. The first reducing agent is added within 20 min and kept warm for 5 min, then add 5 g / L of glucose. The glucose is added within 5 min and kept warm for 5 min, then add 5 g / L of sulfur dye, and at the same time heat up to 90 °C and react for 20 min. After draining the water, perform overflow water washing for 20 min to prepare the second treated fabric.

[0112] After the dyeing is completed, without opening the vat lid, immediately carry out the after-treatment of sulfurization on the second treated fabric. First, use 2 g / L of soaping agent (TF-231YA) to soap wash at 50 °C for 20 min. After soaping 2 - 3 times, then add 8 g / L of hydrogen peroxide (mass concentration 27.5%) and 2 g / L of acid agent (glacial acetic acid) for oxidation. The oxidation time is 20 min. After completion, wash with water at 40 °C for 20 min to prepare the dyed fabric.

[0113] The cheese yarn dyed by the above dyeing method did not show dyeing unevenness. When making weft plain color fabric, there is no need to pick yarn, and the utilization rate is 100%. The fastness to washing, water stain, sweat stain, etc. is all > 4.5 levels.

[0114] Example 3

[0115] The difference from Example 2 is that the concentrations of the first reducing agent and the second reducing agent are different. In this example, 1 g / L of the first reducing agent is added and 3 g / L of the second reducing agent is added, and the other steps are the same as those in Example 2.

[0116] The overall color of the cheese yarn dyed by the above dyeing method is significantly lighter, and there is a slight phenomenon of uneven dyeing.

[0117] Example 4

[0118] The difference from Example 2 is that no acid agent is added in the oxidation treatment, and the remaining steps are the same as those in Example 2.

[0119] The cheese yarn dyed by the above dyeing method has serious floating color and unqualified fastness, and the washing fastness is 3 levels.

[0120] Example 5

[0121] The difference from Example 2 is that the treatment time of the first reducing agent on the first treated fabric and the treatment time of adding the second reducing agent are different. In this example, the first reducing agent is used to treat the first treated fabric for 25 minutes, and then the second reducing agent is added and treated for 25 minutes. The remaining steps are the same as those in Example 2.

[0122] The cheese yarn dyed by the above dyeing method has a lighter color, the overall color is inconsistent and has a dyed flower performance, and the quality is unqualified.

[0123] Example 6

[0124] The difference from Example 2 is that the dye feeding time is postponed. In this example, the dye is added 40 minutes after the glucose heat preservation treatment. The remaining steps are the same as those in Example 2.

[0125] The overall color of the cheese yarn dyed by the above dyeing method is relatively light.

[0126] Example 7

[0127] The difference from Example 2 is that the dosage of the accelerating agent is increased. In this example, the accelerating agent is changed to 90 g / L, and the remaining steps are the same as those in Example 2.

[0128] The difference between the inner and outer layers of the cheese yarn dyed by the above dyeing method is large, the inner layer is relatively dark, and the quality is unqualified.

[0129] Comparative Example 1

[0130] The difference from Example 2 is that the addition order of the reducing agent and the sulfur dye is different. In this comparative example, the sulfur dye is added before the first reducing agent, and the remaining steps are the same as those in Example 2.

[0131] The overall color of the cheese yarn dyed by the above dyeing method is inconsistent, with a serious dyed flower performance, and the inner layer is significantly darker, and the quality is unqualified.

[0132] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope described in this specification.

[0133] The above-described embodiments merely represent several implementation manners of the present invention. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all fall within the protection scope of the present invention. Therefore, the protection scope of the present invention patent shall be subject to the appended claims.

Claims

1. A dyeing method of sulfur dyes, characterized in that, It includes the following steps: Provide the fabric to be dyed; Treat the fabric to be dyed with an alkali solution to prepare a first treated fabric; Treat the first treated fabric with a first reducing agent for a predetermined time, add a second reducing agent and treat for a predetermined time, and add a sulfur dye for reaction to prepare a second treated fabric; the first reducing agent includes sodium dithionite and / or thiourea dioxide; the second reducing agent includes glucose; Perform an oxidation treatment on the second treated fabric to prepare a dyed fabric.

2. The dyeing method of the sulfur dye according to claim 1, characterized in that, The concentration of the first reducing agent is 1 g / L - 6 g / L; and / or, the concentration of the second reducing agent is 5 g / L - 20 g / L.

3. The dyeing method of the sulfur dye according to claim 1, characterized in that The treatment time of the first reducing agent on the first treated fabric is 5 min - 20 min; and / or, the treatment time of the second reducing agent is 5 min - 20 min.

4. The dyeing method of the sulfur dye according to any one of claims 1 to 3, characterized in that Before treating the fabric to be dyed with an alkali solution, it also includes treating the fabric to be dyed with an accelerating agent; Optionally, the accelerating agent is selected from one or more of sodium sulfate, sodium chloride, calcium chloride, and potassium chloride; Optionally, the concentration of the accelerating agent is 20 g / L - 50 g / L; Optionally, the temperature for treating with the accelerating agent is 20°C - 60°C; Optionally, the treatment time with the accelerating agent is 5 min - 35 min.

5. The dyeing method of the sulfur dye according to any one of claims 1 to 3, characterized in that, The alkali solution includes one or several alkali agents such as sodium hydroxide, potassium hydroxide, urea, potassium hydrogen phosphate, potassium dihydrogen phosphate, ammonium sulfate, sodium carbonate, and sodium bicarbonate; Optionally, the addition amount of the alkali agent is 6 g / L - 15 g / L.

6. The dyeing method of the sulfur dye according to any one of claims 1 to 3, characterized in that, The temperature of the alkali solution treatment is 20°C - 80°C; and / or, the treatment time of the alkali solution is 5 min - 20 min.

7. The dyeing method of the sulfur dye according to any one of claims 1 to 3, characterized in that, A scouring agent and / or a dispersant is also added to the alkali solution; Optionally, the scouring agent includes one or more of an alkaline scouring agent, an acidic scouring agent, a neutral scouring agent, and an enzyme preparation scouring agent; Optionally, the dispersant includes a chemically synthesized dispersant and / or a natural polymer.

8. The dyeing method of the sulfur dye according to claim 7, characterized in that, The concentration of the scouring agent is 0.5 g / L - 3 g / L; and / or, the concentration of the dispersant is 0.5 g / L - 3 g / L.

9. The dyeing method of the sulfur dye according to claim 1 or 2, characterized in that, The reaction temperature for adding the sulfur dye is 90°C - 100°C.

10. The dyeing method of the sulfur dye according to claim 1, characterized in that, The oxidation treatment also satisfies the following (1) and / or (2): (1) The oxidant components in the oxidation treatment process include one or more of hydrogen peroxide, sodium hypochlorite, sodium chlorite, persulfates, and ozone; Optionally, an acid agent is also added to the oxidant; (2) The concentration of the oxidant in the oxidation treatment process is 3 g / L - 10 g / L.