Improved dyeing reduction cleaning process for polyester fiber fabric
By using a sulfur-free reducing cleaning solution, and utilizing a complex of phosphovanadium molybdenum-based metal oxoacid salts and copper ions, as well as N-fluorenemethoxycarbonyl-L-lysine and α-cyclodextrin, the problem of difficult removal of floating dye after dyeing polyester fiber fabrics was solved, achieving efficient color fastness and environmentally friendly cleaning effect.
Patent Information
- Application Number
- CN202511956094.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-23
- Publication Date
- 2026-02-24
AI Technical Summary
The loose dye on existing polyester fiber fabrics is difficult to remove completely after dyeing, resulting in poor color fastness. In addition, the commonly used reducing cleaning agents contain sulfur compounds, which pollute the environment and harm health.
A sulfur-free reducing cleaning solution is used, which combines N-fluorenemethyloxycarbonyl-L-lysine and α-cyclodextrin with a phosphovanadium-molybdenum-based metal oxoacid salt and copper ion complex to improve the efficiency of floating color removal and avoid damage to the dye inside the fiber.
It effectively removes loose dye from the surface of polyester fiber fabrics, improves color fastness and color, and reduces environmental pollution and health risks.
Smart Images
Figure SMS_1
Abstract
Description
Technical Field
[0001] This invention relates to the field of textile and apparel fabric dyeing technology, specifically to an improved dyeing and reduction cleaning process for polyester fiber fabrics. Background Technology
[0002] Polyester fiber fabric is a commonly used synthetic fiber clothing fabric in daily life. It has excellent properties such as good resilience, high mechanical strength, strong chemical stability, and resistance to mildew and moths, making it suitable for various fitness wear, sportswear, loungewear, outdoor mountaineering clothing, and so on. However, polyester fiber has poor moisture absorption, making its dyeing process more difficult. It usually requires high temperature and high pressure conditions. Although disperse dye molecules are small, due to their hydrophobic nature, it is difficult to ensure that all dyes can completely penetrate into the fiber. After dyeing, some disperse dyes that have not penetrated into the fiber may adhere to the fiber surface. If not removed, this will affect the dyeing fastness. In addition to the dye adhering to the fabric surface causing floating color, the violent movement of polyester fiber molecules during the high temperature and high pressure dyeing process increases the gaps between molecules. Oligomers formed during the fiber molecule polymerization stage migrate from the fiber interior to the surface and deposit on the fabric surface during cooling, forming color spots and affecting the dyeing quality.
[0003] Therefore, after dyeing, a reduction cleaning method is usually required. A strong reducing agent is used to break down the dye molecules that have not entered the fiber, remove the floating color on the fiber surface, thereby improving the color fastness and color. Commonly used reducing cleaning agents are mainly divided into two categories: one is strong reducing agents, such as sodium dithionite (Sodium hydrosulfite) and thiourea dioxide, which have strong reducing ability under alkaline conditions. Among them, sodium hydrosulfite poses significant safety hazards during transportation, storage, and production, and the treated wastewater is highly polluting, causing great harm to the environment. The other is acidic reducing cleaning agents, such as the new acidic reducing cleaning agents ARC and SH, which do not require drainage after disperse dyeing and can directly carry out reducing cleaning under acidic conditions. Both types of reducing cleaning agents have their advantages in the cleaning process, but most of them contain reducing sulfur compounds. Therefore, the sulfur content in the wastewater generated by reducing cleaning is high. Sulfur compounds increase the hardness of water, deteriorate the quality of groundwater, and thus have a significant impact on industrial products. The quality of drinking water will also deteriorate, posing a significant threat to human health. According to GB4287-2012 "Water Pollutant Discharge Standard for Textile Dyeing and Finishing Industry", the standard for direct discharge of sulfides is not higher than 1 mg / L. As people's demands for environmental protection increase, in this new stage of development of the printing and dyeing industry, printing and dyeing enterprises must move towards a green and sustainable direction. Summary of the Invention
[0004] To address the above problems, this invention provides an improved dyeing and reduction cleaning process for polyester fiber fabrics.
[0005] The objective of this invention is achieved through the following technical solution: An improved dyeing and reduction cleaning process for polyester fiber fabrics includes the dissolution and diffusion of disperse dye molecules, dyeing of the polyester fiber fabric, and reduction cleaning after dyeing. The reduction cleaning process after dyeing involves rinsing in a cleaning solution at a temperature of 50-80°C for 10-60 minutes. The preparation method of the cleaning solution includes the following steps: (1) Weigh out disodium hydrogen phosphate and dissolve it in deionized water. After it is fully dissolved, heat it to 50-80℃, add sodium metavanadate and stir until dissolved, add concentrated sulfuric acid to acidify, cool and add sodium molybdate and stir until dissolved, continue to stir the reaction at room temperature for 1-4 hours, add diethyl ether to extract, and evaporate the solvent from the diethyl ether phase to obtain product A. (2) Weigh N-fluorenylmethoxycarbonyl-L-lysine and dissolve it in deionized water. Let it stand for 24-72 hours. Add copper chloride solution and α-cyclodextrin solution in sequence and mix thoroughly. Adjust the pH to 5-6. Let it stand for 0.5-2 hours. Add the product A. Adjust the pH to 5-6. Let it stand for 0.5-2 hours. After dilution, add a nonionic surfactant to obtain the cleaning solution.
[0006] In some preferred embodiments, the dyeing process involves contacting the polyester fiber fabric to be dyed with a dye solution under high temperature conditions; wherein the dye solution includes disperse dye, degreasing agent and surfactant, and the surfactant is anionic surfactant or nonionic surfactant or a combination of both.
[0007] In some preferred embodiments, the concentration of the surfactant in the dye solution is 0.5-3 g / L.
[0008] In some preferred embodiments, the concentration of the degreasing agent in the dye solution is 0.5-1 g / L.
[0009] In some preferred embodiments, the mass ratio of the dye solution to the polyester fiber fabric is (10-40):1.
[0010] In some preferred embodiments, the mass ratio of the disperse dye in the dye solution to the polyester fiber fabric is 1:(10-1000).
[0011] In some preferred embodiments, the mass ratio of disodium hydrogen phosphate to sodium metavanadate and sodium molybdate in step (1) is 1:(0.8-0.9):(12-17); the volume ratio of deionized water to concentrated sulfuric acid is (8-10):1.
[0012] In some preferred embodiments, the mass ratio of N-fluorenemethoxycarbonyl-L-lysine to copper chloride, α-cyclodextrin and product A in step (2) is (28-32):1:(40-50):(3-4.2).
[0013] In some preferred embodiments, the mass concentration of copper chloride in the cleaning solution obtained after dilution in step (2) is 0.01-0.05 g / L.
[0014] In some preferred embodiments, the nonionic surfactant in step (2) is phenoxylate or nonylphenol polyoxyethylene ether, and the concentration of the nonionic surfactant in the cleaning solution is 0.01-0.03 g / L; adding a nonionic surfactant helps to dissolve and disperse the floating color and prevents re-contamination.
[0015] The beneficial effects of this invention are as follows: This invention improves the existing dyeing reduction cleaning process for polyester fiber fabrics, providing a sulfur-free reduction cleaning solution and its cleaning process. This solution can remove surface dye after dyeing polyester fiber fabrics, improving colorfastness and color. The main components of the reduction cleaning solution are co-coordination products based on copper ions. Product A is a compound mainly composed of phosphovanadium molybdenum-based metal oxophosphates, which, in conjunction with copper ions, removes surface dye from the fiber. N-fluorenemethoxycarbonyl-L-lysine, in conjunction with copper ions, utilizes the hydrophilic-hydrophobic amphoteric structure of lysine to reduce the penetration of the reduction cleaning agent into the fiber, preventing damage to the dyes inside the fiber. α-Cyclodextrin is used to increase the affinity of the reduction cleaning agent for disperse dyes, increasing its contact with disperse dyes on the fiber surface and improving the efficiency of removing surface dye. Detailed Implementation
[0016] The present invention will be further described in conjunction with the following embodiments. Example 1
[0017] An improved dyeing and reduction cleaning process for polyester fiber fabrics includes the dissolution and diffusion of disperse dye molecules, dyeing of polyester fiber fabrics, and reduction cleaning after dyeing. The dissolution and diffusion process of the disperse dye molecules is the preparation of the dye solution, which includes disperse dye, degreasing agent and nonylphenol polyoxyethylene ether NP-10. The concentration of nonylphenol polyoxyethylene ether NP-10 in the dye solution is 1 g / L, and the concentration of degreasing agent in the dye solution is 0.8 g / L. The dyeing process involves contacting the polyester fiber fabric to be dyed with a dye solution under high temperature conditions. The mass ratio of the dye solution to the polyester fiber fabric is 34:1, and the mass ratio of the disperse dye in the dye solution to the polyester fiber fabric is 1:100. The dyeing conditions are as follows: on a high-temperature and high-pressure dyeing machine, the temperature is raised to 80°C at a rate of 2-3°C / min and held for 15 minutes, then raised to 130°C and held for 45 minutes. After the high-temperature dyeing is completed, the temperature is lowered to below 80°C at a rate of 2-3°C / min, and the residual dye solution is discharged. The reduction and cleaning process after staining involves rinsing in a cleaning solution at a temperature of 75°C for 40 minutes, followed by rinsing with clean water. The cleaning solution is prepared using the following steps: (1) Weigh disodium hydrogen phosphate and dissolve it in deionized water. After it is fully dissolved, heat it to 65°C, add sodium metavanadate and stir until dissolved. Add concentrated sulfuric acid to acidify it. After cooling, add sodium molybdate and stir until dissolved. Continue stirring at room temperature for 2 hours. Add diethyl ether to extract the product. After evaporating the solvent from the diethyl ether phase, product A is obtained. The mass ratio of disodium hydrogen phosphate to sodium metavanadate and sodium molybdate is 1:0.857:15.9. The volume ratio of deionized water to concentrated sulfuric acid is 8:1. (2) Weigh N-fluorenemethoxycarbonyl-L-lysine and dissolve it in deionized water. Let it stand for 48 hours. Add copper chloride solution and α-cyclodextrin solution in sequence and mix thoroughly. Adjust the pH to 5-6 and let it stand for 2 hours. Add product A and adjust the pH to 5-6. Let it stand for 2 hours. After dilution, add nonylphenol polyoxyethylene ether NP-10 to obtain the cleaning solution. The mass ratio of N-fluorenemethoxycarbonyl-L-lysine to copper chloride, α-cyclodextrin and product A is 31.2:1:45.5:3.5. The mass concentration of copper chloride in the diluted cleaning solution is 0.02 g / L. The concentration of nonylphenol polyoxyethylene ether NP-10 in the cleaning solution is 0.02 g / L. Example 2
[0018] A dyeing and reduction cleaning process for polyester fiber fabric includes the dissolution and diffusion of disperse dye molecules, dyeing of polyester fiber fabric, and reduction cleaning after dyeing. The dissolution and diffusion process of the disperse dye molecules is the preparation of the dye solution, which includes disperse dye, degreasing agent and nonylphenol polyoxyethylene ether NP-10. The concentration of nonylphenol polyoxyethylene ether NP-10 in the dye solution is 1 g / L, and the concentration of degreasing agent in the dye solution is 0.8 g / L. The dyeing process involves contacting the polyester fiber fabric to be dyed with a dye solution under high temperature conditions. The mass ratio of the dye solution to the polyester fiber fabric is 34:1, and the mass ratio of the disperse dye in the dye solution to the polyester fiber fabric is 1:100. The dyeing conditions are as follows: on a high-temperature and high-pressure dyeing machine, the temperature is raised to 80°C at a rate of 2-3°C / min and held for 15 minutes, then raised to 130°C and held for 45 minutes. After the high-temperature dyeing is completed, the temperature is lowered to below 80°C at a rate of 2-3°C / min, and the residual dye solution is discharged. The reduction and cleaning process after staining involves rinsing in a cleaning solution at a temperature of 75°C for 40 minutes, followed by rinsing with clean water. The cleaning solution is prepared using the following steps: (1) Weigh N-fluorenemethoxycarbonyl-L-lysine and dissolve it in deionized water. Let it stand for 48 hours. Add copper chloride solution and α-cyclodextrin solution in sequence and mix thoroughly. Adjust the pH to 5-6 and let it stand for 2 hours. After dilution, add nonylphenol polyoxyethylene ether NP-10 to obtain the cleaning solution. The mass ratio of N-fluorenemethoxycarbonyl-L-lysine to copper chloride and α-cyclodextrin is 31.2:1:45.5. The mass concentration of copper chloride in the cleaning solution obtained after dilution is 0.02 g / L. The concentration of nonylphenol polyoxyethylene ether NP-10 in the cleaning solution is 0.02 g / L. Example 3
[0019] A dyeing and reduction cleaning process for polyester fiber fabric includes the dissolution and diffusion of disperse dye molecules, dyeing of polyester fiber fabric, and reduction cleaning after dyeing. The dissolution and diffusion process of the disperse dye molecules is the preparation of the dye solution, which includes disperse dye, degreasing agent and nonylphenol polyoxyethylene ether NP-10. The concentration of nonylphenol polyoxyethylene ether NP-10 in the dye solution is 1 g / L, and the concentration of degreasing agent in the dye solution is 0.8 g / L. The dyeing process involves contacting the polyester fiber fabric to be dyed with a dye solution under high temperature conditions. The mass ratio of the dye solution to the polyester fiber fabric is 34:1, and the mass ratio of the disperse dye in the dye solution to the polyester fiber fabric is 1:100. The dyeing conditions are as follows: on a high-temperature and high-pressure dyeing machine, the temperature is raised to 80°C at a rate of 2-3°C / min and held for 15 minutes, then raised to 130°C and held for 45 minutes. After the high-temperature dyeing is completed, the temperature is lowered to below 80°C at a rate of 2-3°C / min, and the residual dye solution is discharged. The reduction and cleaning process after staining involves rinsing in a cleaning solution at a temperature of 75°C for 40 minutes, followed by rinsing with clean water. The cleaning solution is prepared using the following steps: (1) Weigh disodium hydrogen phosphate and dissolve it in deionized water. After it is fully dissolved, heat it to 65°C, add sodium metavanadate and stir until dissolved. Add concentrated sulfuric acid to acidify it. After cooling, add sodium molybdate and stir until dissolved. Continue stirring at room temperature for 2 hours. Add diethyl ether to extract the product. After evaporating the solvent from the diethyl ether phase, product A is obtained. The mass ratio of disodium hydrogen phosphate to sodium metavanadate and sodium molybdate is 1:0.857:15.9. The volume ratio of deionized water to concentrated sulfuric acid is 8:1. (2) Weigh copper chloride and dissolve it in deionized water, add α-cyclodextrin solution and mix thoroughly, adjust pH to 5-6, let stand for 2 hours, add product A, adjust pH to 5-6, let stand for 2 hours, dilute and add nonylphenol polyoxyethylene ether NP-10 to obtain the cleaning solution; the mass ratio of copper chloride to α-cyclodextrin and product A is 1:45.5:3.5; the mass concentration of copper chloride in the diluted cleaning solution is 0.02 g / L; the concentration of nonylphenol polyoxyethylene ether NP-10 in the cleaning solution is 0.02 g / L. Example 4
[0020] A dyeing and reduction cleaning process for polyester fiber fabric includes the dissolution and diffusion of disperse dye molecules, dyeing of polyester fiber fabric, and reduction cleaning after dyeing. The dissolution and diffusion process of the disperse dye molecules is the preparation of the dye solution, which includes disperse dye, degreasing agent and nonylphenol polyoxyethylene ether NP-10. The concentration of nonylphenol polyoxyethylene ether NP-10 in the dye solution is 1 g / L, and the concentration of degreasing agent in the dye solution is 0.8 g / L. The dyeing process involves contacting the polyester fiber fabric to be dyed with a dye solution under high temperature conditions. The mass ratio of the dye solution to the polyester fiber fabric is 34:1, and the mass ratio of the disperse dye in the dye solution to the polyester fiber fabric is 1:100. The dyeing conditions are as follows: on a high-temperature and high-pressure dyeing machine, the temperature is raised to 80°C at a rate of 2-3°C / min and held for 15 minutes, then raised to 130°C and held for 45 minutes. After the high-temperature dyeing is completed, the temperature is lowered to below 80°C at a rate of 2-3°C / min, and the residual dye solution is discharged. The reduction and cleaning process after staining involves rinsing in a cleaning solution at a temperature of 75°C for 40 minutes, followed by rinsing with clean water. The cleaning solution is prepared using the following steps: (1) Weigh disodium hydrogen phosphate and dissolve it in deionized water. After it is fully dissolved, heat it to 65°C, add sodium metavanadate and stir until dissolved. Add concentrated sulfuric acid to acidify it. After cooling, add sodium molybdate and stir until dissolved. Continue stirring at room temperature for 2 hours. Add diethyl ether to extract the product. After evaporating the solvent from the diethyl ether phase, product A is obtained. The mass ratio of disodium hydrogen phosphate to sodium metavanadate and sodium molybdate is 1:0.857:15.9. The volume ratio of deionized water to concentrated sulfuric acid is 8:1. (2) Weigh N-fluorenemethoxycarbonyl-L-lysine and dissolve it in deionized water. Let it stand for 48 hours, add copper chloride solution and mix thoroughly. Adjust the pH to 5-6 and let it stand for 2 hours. Add the product A, adjust the pH to 5-6, and let it stand for 2 hours. After dilution, add nonylphenol polyoxyethylene ether NP-10 to prepare the cleaning solution. The mass ratio of N-fluorenemethoxycarbonyl-L-lysine to copper chloride and product A is 31.2:1:3.5. The mass concentration of copper chloride in the diluted cleaning solution is 0.02 g / L. The concentration of nonylphenol polyoxyethylene ether NP-10 in the cleaning solution is 0.02 g / L.
[0021] Comparative Example A dyeing and reduction cleaning process for polyester fiber fabric includes the dissolution and diffusion of disperse dye molecules, dyeing of polyester fiber fabric, and reduction cleaning after dyeing. The dye dissolution, diffusion, and dyeing process are the same as in Example 1. The reduction cleaning is carried out under conventional alkaline conditions using sodium hydrosulfite as a reducing agent in combination with soaping agent for reduction cleaning and then neutralization.
[0022] Taking bright red disperse dye as an example, the color characteristics and color fastness before and after washing are shown in the table below:
[0023] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. An improved dyeing and reduction washing process for polyester fiber fabrics, characterized in that, This includes the dissolution and diffusion of disperse dye molecules, the dyeing of polyester fiber fabric, and the reduction cleaning after dyeing. The reduction cleaning process after dyeing involves rinsing in a cleaning solution at a temperature of 50-80℃ for 10-60 minutes. The preparation method of the cleaning solution includes the following steps: (1) Weigh out disodium hydrogen phosphate and dissolve it in deionized water. After it is fully dissolved, heat it to 50-80℃, add sodium metavanadate and stir until dissolved, add concentrated sulfuric acid to acidify, cool and add sodium molybdate and stir until dissolved, continue to stir the reaction at room temperature for 1-4 hours, add diethyl ether to extract, and evaporate the solvent from the diethyl ether phase to obtain product A. (2) Weigh N-fluorenylmethoxycarbonyl-L-lysine and dissolve it in deionized water. Let it stand for 24-72 hours. Add copper chloride solution and α-cyclodextrin solution in sequence and mix thoroughly. Adjust the pH to 5-6. Let it stand for 0.5-2 hours. Add the product A. Adjust the pH to 5-6. Let it stand for 0.5-2 hours. After dilution, add a nonionic surfactant to obtain the cleaning solution.
2. The improved dyeing and reduction washing process for polyester fiber fabric according to claim 1, characterized in that, The dyeing process involves contacting the polyester fiber fabric to be dyed with a dye solution under high temperature conditions; wherein, the dye solution includes disperse dye, degreasing agent and surfactant, and the surfactant is anionic surfactant or nonionic surfactant or a combination of both.
3. The improved dyeing and reduction cleaning process for polyester fiber fabric according to claim 2, characterized in that, The concentration of the surfactant in the dye solution is 0.5-3 g / L.
4. The improved dyeing and reduction washing process for polyester fiber fabric according to claim 2, characterized in that, The concentration of the degreasing agent in the dye solution is 0.5-1 g / L.
5. The improved dyeing and reduction cleaning process for polyester fiber fabric according to claim 2, characterized in that, The mass ratio of the dye solution to the polyester fiber fabric is (10-40):
1.
6. The improved dyeing and reduction cleaning process for polyester fiber fabric according to claim 2, characterized in that, The mass ratio of the disperse dye to the polyester fiber fabric in the dye solution is 1:(10-1000).
7. The improved dyeing and reduction washing process for polyester fiber fabric according to claim 1, characterized in that, In step (1), the mass ratio of disodium hydrogen phosphate to sodium metavanadate and sodium molybdate is 1:(0.8-0.9):(12-17); the volume ratio of deionized water to concentrated sulfuric acid is (8-10):
1.
8. The improved dyeing and reduction cleaning process for polyester fiber fabric according to claim 1, characterized in that, In step (2), the mass ratio of N-fluorenemethoxycarbonyl-L-lysine to copper chloride, α-cyclodextrin, and product A is (28-32):1:(40-50):(3-4.2).
9. The improved dyeing and reduction washing process for polyester fiber fabric according to claim 1, characterized in that, The mass concentration of copper chloride in the cleaning solution obtained after dilution in step (2) is 0.01-0.05 g / L.
10. The improved dyeing and reduction cleaning process for polyester fiber fabric according to claim 1, characterized in that, The nonionic surfactant mentioned in step (2) is phenoxyacetic acid O or nonylphenol polyoxyethylene ether, and the concentration of the nonionic surfactant in the cleaning solution is 0.01-0.03 g / L.