Environment-friendly acidic color fixing agent and preparation method thereof
By preparing an environmentally friendly acidic fixing agent, the problem of poor wet fastness of nylon fabrics was solved, acid dye fixation with high color fastness was achieved, harmful substance residues were avoided, and the washing and water fastness of the fabric were improved.
Patent Information
- Application Number
- CN202510822725.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-19
- Publication Date
- 2025-09-16
AI Technical Summary
Existing acid dyes have poor wet fastness on nylon or nylon/spandex fabrics and are easily shed during soaping. In addition, traditional acid fixing agents contain harmful residual substances.
The environmentally friendly acidic fixing agent is composed of water, ethanol, sodium chloride, benzoic acid, emulsifier and sulfonic acid solution. It is prepared through a specific reaction to form a fixing agent that can form multi-layer adsorption and chemical bonds with fibers and dyes to enhance color fastness.
The color fastness of nylon fabrics, especially the color fastness to washing and water fastness, has been improved to level 5, avoiding the residue of harmful substances.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] The present invention relates to the field of textile fabrics, and in particular to an environmentally friendly acidic color fixing agent and a preparation method thereof. Background Art
[0002] Acid dyes need to be dyed on nylon or nylon / spandex fabrics under acidic conditions. The amino groups at the ends of nylon or nylon / spandex fibers absorb cationic hydrogen ions. The anionic acid dyes adsorbed on the fabric have poor wet fastness and are easily shed during soaping.
[0003] Acidic fixing agents are currently used to improve the wet color fastness of acid dyes or acid mordant dyes on nylon and nylon / spandex fabrics. Currently, some acidic fixing agents on the market are synthesized using phenolsulfonic acid, bisphenol S / F / A, and formaldehyde under alkaline conditions. Others are synthesized using acetic anhydride as a solvent through the sulfonation of bisphenol S, followed by a condensation reaction between the sulfonated bisphenol S and formaldehyde under strongly acidic conditions. Acidic fixing agents synthesized using these methods all contain residual phenols and / or bisphenols. Summary of the Invention
[0004] In view of this, the object of the present invention is to provide an environmentally friendly acidic color fixing agent and a preparation method thereof to improve the color fastness of nylon fabrics or nylon / spandex fabrics.
[0005] In order to achieve the above object, the present invention provides the following technical solutions: An environmentally friendly acidic color fixing agent comprises the following raw materials in parts by weight: 40-60 parts of water, 40-60 parts of ethanol, 4-6 parts of sodium chloride, 4-6 parts of benzoic acid, 20-30 parts of an emulsifier and 40-60 parts of a sulfonic acid solution.
[0006] Preferably, the emulsifier is at least one of isomeric tridecanol polyoxyethylene ether, isomeric decanol polyoxyethylene ether, and sodium dodecylbenzene sulfonate.
[0007] Preferably, the raw materials include the following parts by weight: 50 parts of water, 50 parts of ethanol, 5 parts of sodium chloride, 5 parts of benzoic acid, 25 parts of emulsifier and 50 parts of sulfonic acid solution.
[0008] A method for preparing an environmentally friendly acidic color fixing agent comprises the following steps: Step S1: mixing bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride to react to obtain an intermediate mixed product; Step S2: adding hydroxyethylpiperazine to the intermediate mixed product to react to obtain a sulfonic acid solution; Step S3: Mix water, ethanol, sodium chloride, benzoic acid, an emulsifier and a sulfonic acid solution to obtain a color fixing agent.
[0009] Preferably, the weight ratio of bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride in step S1 is 1:2:6:1.
[0010] Preferably, the mixing reaction conditions in step S1 are: stirring, heating to 80-90° C., and keeping warm for 2-3 hours.
[0011] Preferably, the reaction conditions in step S2 are: continue heating to 100-110° C. and stirring the reaction, and add sodium hydroxide solution and continue the reaction for 4-5 hours.
[0012] Preferably, the weight ratio of the hydroxyethylpiperazine to the intermediate mixed product is 1:2.
[0013] Preferably, the weight ratio of the sodium hydroxide solution to hydroxyethylpiperazine is 2:1.
[0014] Preferably, the weight ratio of the water, ethanol, sodium chloride, benzoic acid, emulsifier and sulfonic acid solution is 10:10:1:1:5:10.
[0015] The color fixing agent of the present invention contains a long chain of the mixture, has a stable structure, increases the activity of the reactive sites and the activity of the active sites, can undergo a cross-linking reaction with the hydroxyl groups in the acid dye, thereby being better embedded in the surface of the fabric, and is combined with the effect of strong hydrogen bonds to be more stably adsorbed on the surface of the fabric, relies on physical effects and chemical bonds to combine with the fiber, seals the dye molecules in the fiber, has good affinity for both the fiber and the dye, can combine with the fiber and the dye, and be adsorbed on the fiber surface to form multi-layer adsorption, continuously and massively penetrate and embed into the fabric surface, and further contains a large number of sulfonic acid groups in the molecular structure, which generate electrostatic repulsion with the dye anion to prevent the dye from diffusing to the outside of the fiber, and plays a color fixing role through the coordination effect of the macromolecules. DETAILED DESCRIPTION
[0016] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work are within the scope of protection of the present invention. In addition, it is specifically stated that the raw materials and equipment of the present invention can be obtained from commercial sources and are no longer listed one by one. Among them, the raw materials of the present invention can be obtained from commercial sources and are well known to those skilled in the art. Example 1
[0017] An environmentally friendly acidic color fixing agent comprises the following raw materials in parts by weight: 40 parts of water, 40 parts of ethanol, 4 parts of sodium chloride, 4 parts of benzoic acid, 20 parts of isomeric tridecyl alcohol polyoxyethylene ether and 40 parts of sulfonic acid solution.
[0018] A method for preparing an environmentally friendly acidic color fixing agent comprises the following steps: Step S1: bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride are mixed in a weight ratio of 1:2:6:1, stirred and heated to 80° C., and kept warm for 2 hours to obtain an intermediate mixed product; Step S2: adding hydroxyethylpiperazine to the intermediate mixed product in a weight ratio of 1:2, heating to 100° C. with stirring for reaction, adding sodium hydroxide solution in a weight ratio of 2:1, and continuing the reaction for 4 hours to obtain a sulfonic acid solution; Step S3: Mix the above-mentioned parts by weight of water, ethanol, sodium chloride, benzoic acid, emulsifier and sulfonic acid solution to obtain a color fixing agent. Example 2
[0019] An environmentally friendly acidic color fixing agent comprises the following raw materials in parts by weight: 50 parts of water, 50 parts of ethanol, 5 parts of sodium chloride, 5 parts of benzoic acid, 25 parts of isomeric decanol polyoxyethylene ether and 50 parts of sulfonic acid solution.
[0020] A method for preparing an environmentally friendly acidic color fixing agent comprises the following steps: Step S1: bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride are mixed in a weight ratio of 1:2:6:1, stirred and heated to 90° C., and kept warm for 3 hours to obtain an intermediate mixed product; Step S2: adding hydroxyethylpiperazine to the intermediate mixed product in a weight ratio of 1:2, heating to 110° C. with stirring for reaction, adding sodium hydroxide solution in a weight ratio of 2:1, and continuing the reaction for 5 hours to obtain a sulfonic acid solution; Step S3: Mix the above-mentioned parts by weight of water, ethanol, sodium chloride, benzoic acid, emulsifier and sulfonic acid solution to obtain a color fixing agent. Example 3
[0021] An environmentally friendly acidic color fixing agent comprises the following raw materials in parts by weight: 60 parts of water, 60 parts of ethanol, 6 parts of sodium chloride, 6 parts of benzoic acid, 30 parts of sodium dodecylbenzenesulfonate and 60 parts of sulfonic acid solution.
[0022] A method for preparing an environmentally friendly acidic color fixing agent comprises the following steps: Step S1: bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride were mixed in a weight ratio of 1:2:6:1, stirred and heated to 85° C., and kept warm for 2.5 hours to obtain an intermediate mixed product; Step S2: adding hydroxyethylpiperazine to the intermediate mixed product in a weight ratio of 1:2, heating to 105° C. with stirring for reaction, adding sodium hydroxide solution in a weight ratio of 2:1, and continuing the reaction for 4.5 hours to obtain a sulfonic acid solution; Step S3: Mix the above-mentioned parts by weight of water, ethanol, sodium chloride, benzoic acid, emulsifier and sulfonic acid solution to obtain a color fixing agent. Comparative Example 1
[0023] The preparation process of Comparative Example 1 is substantially the same as that of Example 1, except that hydroxyethylpiperazine is not used. Specifically, the process is as follows: An environmentally friendly acidic color fixing agent comprises the following raw materials in parts by weight: 40 parts of water, 40 parts of ethanol, 4 parts of sodium chloride, 4 parts of benzoic acid, 20 parts of isomeric tridecyl alcohol polyoxyethylene ether and 40 parts of an intermediate mixed product.
[0024] A method for preparing an environmentally friendly acidic color fixing agent comprises the following steps: Step S1: bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride are mixed in a weight ratio of 1:2:6:1, stirred and heated to 80° C., and kept warm for 2 hours to obtain an intermediate mixed product; Step S2: Mix the above-mentioned parts by weight of water, ethanol, sodium chloride, benzoic acid, emulsifier and intermediate mixed product to obtain a color fixing agent.
[0025] The fabric samples were fixed using Examples 1-3, Comparative Example 1, and the commercially available color fixing agent, acidic color fixing agent RH-NB-2040 (Ningbo Runhe High-tech Materials Co., Ltd.): 10 g of the fabric sample was accurately weighed, the bath ratio was 1:10, the amount of the color fixing agent was 3% (owf), the pH value of the working solution was adjusted to 4-4.5 with glacial acetic acid, preheated to 40°C before entering the vat, heated to 70°C at a rate of 2°C / min for 20 minutes, and then washed with water, dehydrated, and dried for later use.
[0026] The color fastness to washing is determined according to GB / T 3921-2008 Textiles - Color fastness to washing with soap. The fixed test cloth is sewn together with a standard six-fiber test cloth. 5g / l detergent and 2g / l soda ash are added. The cloth is placed in a washing vat at 60°C for 30 minutes. After washing, the cloth is dehydrated and dried. The staining effect of the cloth is compared with that of the standard six-fiber test cloth. The staining is rated on a scale of 1-5, with 5 being the best.
[0027] Determination of water fastness: Liby washing powder 2g / l, bath ratio 1:50, soak the above-mentioned cloth with color fixing treatment in 60℃ working solution for 30 minutes, then take it out and compare the water fastness effect. Rating is 1-5, with 5 being the best.
[0028] The test results are shown in Table 1.
[0029] Table 1 Test data of color fixing agents of Examples 1-3, commercially available and Comparative Example 1
[0030] As can be seen from the above table, the environmentally friendly acidic color fixing agent prepared by the present invention can make the color fastness to washing and the water fastness of the cloth sample after the color fixing treatment not less than level 3, and even reach level 5; while the comparative example and commercially available products can only maintain the color fastness to washing and the water fastness of the cloth sample at level 3-4.
[0031] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. An environmentally friendly acidic fixing agent, characterized in that: The method comprises the following raw materials in parts by weight: 40-60 parts of water, 40-60 parts of ethanol, 4-6 parts of sodium chloride, 4-6 parts of benzoic acid, 20-30 parts of emulsifier and 40-60 parts of sulfonic acid solution.
2. The environmentally friendly acidic color fixing agent according to claim 1, characterized in that: The emulsifier is at least one of isomeric tridecanol polyoxyethylene ether, isomeric decanol polyoxyethylene ether, and sodium dodecylbenzene sulfonate.
3. The environmentally friendly acidic color fixing agent according to claim 1, characterized in that: The method comprises the following raw materials in parts by weight: 50 parts of water, 50 parts of ethanol, 5 parts of sodium chloride, 5 parts of benzoic acid, 25 parts of emulsifier and 50 parts of sulfonic acid solution.
4. A method for preparing the environmentally friendly acidic color fixing agent according to claim 1, characterized in that: The following steps are involved: Step S1: mixing bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride to react to obtain an intermediate mixed product; Step S2: adding hydroxyethylpiperazine to the intermediate mixed product to react to obtain a sulfonic acid solution; Step S3: Mix water, ethanol, sodium chloride, benzoic acid, an emulsifier and a sulfonic acid solution to obtain a color fixing agent.
5. The method for preparing the environmentally friendly acidic color fixing agent according to claim 4, wherein: The weight ratio of bisphenol A, formaldehyde, sodium sulfite and ethylene dichloride in step S1 is 1:2:6:
1.
6. The method for preparing the environmentally friendly acidic color fixing agent according to claim 5, wherein: The conditions for the mixing reaction in step S1 are: stirring, heating to 80-90° C., and keeping warm for 2-3 hours.
7. The method for preparing the environmentally friendly acidic color fixing agent according to claim 6, wherein: The reaction conditions in step S2 are: continue heating to 100-110° C. with stirring, add sodium hydroxide solution, and continue the reaction for 4-5 hours.
8. The method for preparing the environmentally friendly acidic color fixing agent according to claim 7, wherein: The weight ratio of the hydroxyethylpiperazine to the intermediate mixed product is 1:
2.
9. The method for preparing the environmentally friendly acidic color fixing agent according to claim 8, wherein: The weight ratio of the sodium hydroxide solution to hydroxyethylpiperazine is 2:
1.
10. The method for preparing the environmentally friendly acidic color fixing agent according to claim 9, characterized in that: The weight ratio of the water, ethanol, sodium chloride, benzoic acid, emulsifier and sulfonic acid solution is 10:10:1:1:5:10.