阅读说明：本技术 一种酸性黑染料染色织物固色、增深剂的制备及使用方法 (Preparation and use method of color fixing and deepening agent for acid black dye dyed fabric ) 是由 戴志坚 于 2019-10-28 设计创作，主要内容包括：本发明公开了一种酸性黑染料染色织物固色、增深剂的制备及使用方法,通过利用金属盐类化合物、1,10-邻二氮杂菲和天然单宁酸和合成单宁混合物以一定质量比进行络合得到酸性黑染料染色织物固色、增深剂,酸性染料和该固色、增深剂对蛋白质纤维或锦纶织物一浴进行染整加工处理,可实现酸性黑染色织物的固色和增深。通过本发明的方法实现酸性黑染料染色蛋白质纤维或锦纶织物的固色和增深,降低了酸性黑染料的用量,减少了印染废水中酸性黑染料的含量,提高了染色织物的牢度,且染色织物的乌黑度增加。(The invention discloses a preparation method and a use method of an acid black dye dyed fabric color fixing and deepening agent. The method realizes the color fixation and the deepening of the protein fiber or the nylon fabric dyed by the acid black dye, reduces the using amount of the acid black dye, reduces the content of the acid black dye in printing and dyeing wastewater, improves the fastness of the dyed fabric, and increases the blackness of the dyed fabric.)

1. A preparation method of a color fixing and deepening agent for acid black dye dyed fabrics is characterized by comprising the following steps:

Respectively putting a metal salt compound, 1, 10-phenanthroline and tannic acid into a conical flask filled with a proper amount of distilled water, performing acoustic stirring under an ultrasonic condition to completely dissolve the metal salt compound, then slowly pouring an aqueous solution of the metal salt compound into an aqueous solution of the 1, 10-phenanthroline under the ultrasonic condition of 50-80 ℃, performing ultrasonic stirring for 10min, slowly adding a mixed aqueous solution of natural tannic acid and synthetic tannin into the solution, adjusting the pH of the solution to 4-6 by using acetic acid after 10min, continuing stirring and reacting at 50-80 ℃ by ultrasonic heat preservation for 20-90 min, and standing and cooling the reacted aqueous solution at room temperature to obtain a stable acid black dye dyed fabric color fixing and deepening agent solution.

2. The method for preparing the dye fixing and deepening agent for the acid black dye dyed fabric according to claim 1 is characterized in that: the metal salt compound is one or more of ferric sulfate, ferric chloride, ferrous sulfate and ferrous chloride.

3. The method for preparing the dye fixing and deepening agent for the acid black dye dyed fabric according to claim 1 is characterized in that: the mass ratio of the metal salt compound to the 1, 10-phenanthroline to the mixture of natural tannic acid and synthetic tannin is 1:3: 10-1: 10: 50.

4. The method for preparing the dye fixing and deepening agent for the acid black dye dyed fabric according to claim 1 is characterized in that: the mass ratio of the natural tannin to the synthetic tannin mixture is 1: 1.

5. The method for carrying out color fixation, darkening dyeing and finishing on the dyed fabric by using the acid black dye prepared by any one of claims 1 to 4 is characterized by comprising the following steps:

1.5-3% of acid black dye, 1-5 g/L of color fixing and deepening agent, adjusting the pH value of a dye solution to 4-6, and the bath ratio to be 1: 5-50, adding the fabric after the temperature of the dye solution rises to 60 ℃, raising the temperature to 90-105 ℃ at the speed of 1-3 ℃/min, preserving the temperature for 30-60 min, discharging liquor after dyeing, taking out the fabric, washing with water, and drying to obtain the dyed fabric with excellent fastness and increased blackness.

6. the color fixing, deepening dyeing and finishing method for the acid black dye dyed fabric according to claim 5, characterized in that: the acid black is one or more of acid black 10B, acid black SSR, acid black ATT, acid black NR, acid black DR, acid black NB-G, acid black VLG, acid black ACE and acid black NT.

7. the color fixing, deepening dyeing and finishing method for the acid black dye dyed fabric according to claim 5, characterized in that: the fabric is one or a blended fabric of fibers such as wool, silk, chinlon, soybean protein fiber, milk protein fiber and the like.

8. The color fixing, deepening dyeing and finishing method for the acid black dye dyed fabric according to claim 5, characterized in that: the dyeing, the deepening and the color fixing of the fabric are carried out in one bath.

Technical Field

The invention belongs to the technical field of dyeing and finishing, and particularly relates to a preparation method and a use method of a color fixing and deepening agent for an acid black dye dyed fabric.

Background

The nylon is a leisure fabric widely applied at present, has the most outstanding advantages that the wear resistance is higher than that of all other fibers, is 10 times higher than that of cotton and 20 times higher than that of wool, has the strength 1-2 times higher than that of cotton and 4-5 times higher than that of wool and 3 times higher than that of viscose, and has the advantages of comfort in wearing, good elasticity, softness and the like. The acid dye is also called anion dye, which contains acid groups in dye molecules, can be combined with amino groups in protein fiber molecules by ionic bonds and is suitable for acid, weak acid or neutral conditions. Mainly azo and anthraquinone structures, and a few arylmethane structures. Dyes and colors are generally compounds that are inherently colored and that can impart a vivid and strong hue to other materials in a molecular or dispersed state. The acid dye is one of the most common dye varieties for nylon dyeing, black is the color of nylon fabric dyed frequently, but the current factory practice shows that the dye consumption is large when pure nylon fabric is dyed in acid black, and the fastness of the dyed fabric is not very high, thus being not beneficial to environmental protection and wastewater treatment. Therefore, the pursuit of an acid black dye dyeing chinlon fabric fixing and darkening auxiliary agent and a using method thereof are pursuit targets of dyeing and finishing science workers.

The invention patent CN 102850500B discloses an acid-resistant reaction type polyamide color fixing agent, which is prepared by performing condensation reaction on a phenolic substance and two aromatic sulfonic acid compounds with formaldehyde under the action of a composite catalyst, adding epoxy chloropropane and a modifier into the reaction system for modification, and finally adjusting the pH value of a multi-copolymerization high-molecular aromatic sulfonic acid formaldehyde condensate obtained by modification to 2.0-4.0 by using strong acid or concentrated acid. The invention patent CN 107724124A discloses a preparation method of a nylon fabric color fixing agent, which comprises the following raw materials in parts by weight: 20-30 parts of bisphenol S, 20-30 parts of epoxy chloropropane, 5-10 parts of a catalyst, 20-25 parts of fatty alcohol-polyoxyethylene ether, 3-5 parts of octadecyl dimethyl amine oxide, 5-9 parts of hydroxypropyl methyl cellulose, 5-10 parts of acrylate, 10-20 parts of ethanol and 30-50 parts of deionized water. After the nylon fabric color fixing agent is applied, the soaping fastness of the dyed fabric can reach 4-5 levels, and the rubbing fastness reaches 4-5 levels. The invention patent CN 104060484B discloses a formula of a no-clean agent for digital printing of nylon carpet, which is characterized in that: the formula of the lotion-free agent consists of amino modified organic silicon, tricarboxylic acid, a water-soluble epoxy cross-linking agent EPTA and water, wherein the percentage of the amino modified organic silicon, the tricarboxylic acid, the water-soluble epoxy cross-linking agent EPTA and the water is 20-40%: 15-20%: 5-10%: 30-60%. The invention patent CN 106930125A discloses a synthesis method of a Gemini color fixing agent NLF for nylon, (1) a quaternary ammonium salt cationic Gemini surfactant is synthesized by adopting 1, 4-dibromobutane and tetradecyl dimethyl tertiary amine; (2) the gemini fixing agent NLF for nylon is compounded by the following components in parts by mass: conc NLF: 20-25 parts; SWF: 25-30 parts of a solvent; trideceth ether (1307): 3-5 parts; trideceth (1305): 3-5 parts; SAG-622 (antifoam): 3 parts of a mixture; the balance being water. The invention patent CN 106192475B discloses a chinlon dyeing deepening agent, which comprises the following formula raw materials in percentage by mass: 5.0-10.0% of emulsifier; 10.0-20.0% fatty amines; 25.0-35.0% of fatty amine derivative; 3.0% acid; 5.0-8.0% fatty alcohols; 3.0-5.0% of urea and the balance of deionized water. The invention patent CN 106245356A discloses a preparation method of water-based black natural dye ink-jet printing ink, which comprises the following steps: respectively dissolving tannic acid and hematoxylin in an acidic aqueous solution to prepare a dye solution, uniformly mixing, dropwise adding a ferrous sulfate solution under stirring, heating to 50-90 ℃, reacting at a constant temperature for 10-30 h, and salting out, filtering and drying after the reaction is finished to obtain a black natural dye raw material; adding black natural dye raw materials, a surfactant, a moisture absorption cosolvent, a rheological property regulator, a preservative, a pH regulator and deionized water into a ball milling tank, adding zirconia balls with the same mass, grinding and dispersing on a ball mill, and filtering to remove the zirconia balls to obtain the aqueous black natural dye ink-jet printing ink. The method can improve the clean production level of textile processing and overcome the defect that no black dye exists in natural dye. According to the literature (Guobao, Lichao, Zhengqingkang, bear Jianbo. the fixation mechanism of tannin synthesized by acid dye dyed nylon fabric is discussed [ J ] wool spinning technology, 2017,45(01):41-46.), the fixation of the synthesized tannin with different structures on the nylon fabric is observed, so that the synthesized tannin has good affinity to the fiber, can be adsorbed to the surface of the fiber in a short time, forms a film on the surface of the fiber, has electrostatic repulsive force with dye molecules, and slows down the diffusion speed of the acid dye on the nylon fabric into water through hydrogen bonds, Van der Waals force and electrostatic repulsive force, reduces the dissolution probability of the dye molecules, and plays a role in fixing the color of the nylon acid dye dyed fabric through the effect. The patent reports and literatures report the preparation and application of various chinlon color fixing agents or deepening agents, report that synthetic tannin is used as a chinlon acid dye dyeing color fixing agent, and do not relate to the report of preparing chinlon color fixing and deepening multifunctional auxiliary agents by using tannin, metal ions and 1, 10-phenanthroline.

Disclosure of Invention

the invention aims to solve the technical problems that the current acid black dye dyeing protein or nylon fabric needs to be dyed under the condition of higher black dye dosage, the dye utilization rate is low, the dyed fabric has poor fastness, the printing and dyeing wastewater is difficult to treat, the dyeing cost is high, and the practical difficulty is brought to printing and dyeing enterprises, so that the preparation method of the color fixing and deepening agent and the dyeing and finishing processing method of the acid black dye dyed nylon fabric are provided, the color fixing and deepening and finishing processing of the acid black dye dyed nylon fabric can be realized, the dyeing dosage of the acid black dye is reduced, and the requirements of excellent dyeing fastness and blackness of the acid black dye can be particularly realized.

In order to solve the technical problems, the invention adopts the following technical scheme:

A preparation method of a color fixing and deepening agent for acid black dye dyed fabrics is characterized by comprising the following steps:

Respectively putting a metal salt compound, 1, 10-phenanthroline and tannic acid into a conical flask filled with a proper amount of distilled water, performing acoustic stirring under an ultrasonic condition to completely dissolve the metal salt compound, then slowly pouring an aqueous solution of the metal salt compound into an aqueous solution of the 1, 10-phenanthroline under the ultrasonic condition of 50-80 ℃, performing ultrasonic stirring for 10min, slowly adding a mixed aqueous solution of natural tannic acid and synthetic tannin into the solution, adjusting the pH of the solution to 4-6 by using acetic acid after 10min, continuing stirring and reacting at 50-80 ℃ by ultrasonic heat preservation for 20-90 min, and standing and cooling the reacted aqueous solution at room temperature to obtain a stable acid black dye dyed fabric color fixing and deepening agent solution.

The metal salt compound is one or more of ferric sulfate, ferric chloride, ferrous sulfate and ferrous chloride.

The mass ratio of the metal salt compound to the 1, 10-phenanthroline to the mixture of natural tannic acid and synthetic tannin is 1:3: 10-1: 10: 50.

The mass ratio of the natural tannin to the synthetic tannin mixture is 1: 1.

The method for carrying out color fixation, darkening dyeing and finishing on the dyed fabric by using the acid black dye prepared by any one of claims 1 to 4 is characterized by comprising the following steps:

1.5-3% of acid black dye, 1-5 g/L of color fixing and deepening agent, adjusting the pH value of a dye solution to 4-6, and the bath ratio to be 1: 5-50, adding the fabric after the temperature of the dye solution rises to 60 ℃, raising the temperature to 90-105 ℃ at the speed of 1-3 ℃/min, preserving the temperature for 30-60 min, discharging liquor after dyeing, taking out the fabric, washing with water, and drying to obtain the dyed fabric with excellent fastness and increased blackness.

The acid black is one or more of acid black 10B, acid black SSR, acid black ATT, acid black NR, acid black DR, acid black NB-G, acid black VLG, acid black ACE and acid black NT.

The fabric is one or a blended fabric of fibers such as wool, silk, chinlon, soybean protein fiber, milk protein fiber and the like.

The dyeing, the deepening and the color fixing of the fabric are carried out in one bath.

The invention has the beneficial effects that: according to the invention, a metal salt compound, 1, 10-phenanthroline, natural tannin and a synthetic tannin mixture are complexed according to a certain mass ratio to obtain the color fixing and deepening agent for the acid black dye dyed nylon fabric, and the color fastness and the color deepening of the nylon fabric can be improved through an auxiliary agent. The metal salt compound, the 1, 10-phenanthroline, the natural tannin and the synthetic tannin mixture form a compact film on the surface of the fabric, the color of the film is black, the blackness of the fabric is enhanced, the film has a good protection effect on acid dyes, and the fastness of the dyed fabric is improved.

According to the invention, the metal salt compound, the 1, 10-phenanthroline and the tannic acid are complexed according to a certain mass ratio to obtain the color fixing and deepening agent for the acid black dye dyed fabric, and the color fixing and deepening agent is used for treating the protein fiber or nylon fabric dyed by the acid black dye, so that the color fixing and deepening of the acid black dyed fabric can be realized. The method realizes the fixation and the deepening of the protein fiber or the chinlon fabric dyed by the acid black dye, reduces the using amount of the acid black dye, reduces the content of the acid black dye in printing and dyeing wastewater, improves the fastness of the dyed fabric, and increases the blackness of the dyed fabric. The technical scheme of the invention has simple and feasible process, has no special requirements on raw materials and acid black dye, can realize large-scale production by utilizing acid dye dyeing equipment of a conventional printing and dyeing mill, and has wide application prospect.

Detailed Description

The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.

The preparation method of the color fixing and deepening agent for the acid black dye dyed fabric comprises the following steps:

Respectively putting a metal salt compound, 1, 10-phenanthroline and tannic acid into a conical flask filled with a proper amount of distilled water, performing sound stirring under an ultrasonic condition to completely dissolve the metal salt compound, then slowly pouring an aqueous solution of the metal salt compound into an aqueous solution of the 1, 10-phenanthroline under the condition of ultrasonic 50-80 ℃, performing ultrasonic stirring for 10min, slowly adding a mixed aqueous solution of natural tannic acid and synthetic tannin in a mass ratio of 1:1 into the solution, adjusting the pH of the solution to 4-6 by using acetic acid after 10min, further continuously performing ultrasonic heat preservation for 50-80 ℃, stirring and reacting for 20-90 min, standing and cooling the reacted aqueous solution at room temperature to obtain a stable color fixing and deepening agent solution for the acid black dye dyed fabric.

The method for carrying out color fixation, darkening dyeing and finishing processing by using the acid black dye for dyeing the fabric comprises the following steps:

1.5-3% of acid black dye, 1-5 g/L of color fixing and deepening agent, adjusting the pH value of a dye solution to 4-6, and the bath ratio to be 1: 5-50, adding the fabric after the temperature of the dye solution rises to 60 ℃, raising the temperature to 90-105 ℃ at the speed of 1-3 ℃/min, preserving the temperature for 30-60 min, discharging liquor after dyeing, taking out the fabric, washing with water, and drying to obtain the dyed fabric with excellent fastness and increased blackness.