阅读说明：本技术 一种植物靛蓝染牛仔面料抗氧化生产工艺 (Antioxidant production process of plant indigo-dyed jean fabric ) 是由 温晓凤 黄友洪 朱晓英 张晓东 郑聪 于 2021-08-16 设计创作，主要内容包括：本申请提供一种植物靛蓝染牛仔面料抗氧化生产工艺,属于以采用特殊纱线原料为主要特征的针织、机织或经编织物或产品技术领域。将待处理牛仔面料置于抗氧化试剂中,所述抗氧化试剂中包含有抗氧化助剂,抗氧化助剂为水杨酸酯类、二苯甲酮类或是苯并三唑类中的任一种,抗氧化处理方法为：抗氧化助剂的浓度20-30g/L、以后整理方式,二浸二轧,保持80%带液率,烘干。本案处理后的牛仔面料的抗氧化处理,可抑制氧气与染料发生反应,赋予面料良好的上染效果。(The application provides an antioxidant production process of a plant indigo-dyed jean fabric, belonging to the technical field of knitted, woven or warp-knitted fabrics or products which are mainly characterized by adopting special yarn raw materials. Placing the denim fabric to be treated in an antioxidant reagent, wherein the antioxidant reagent contains an antioxidant auxiliary agent, the antioxidant auxiliary agent is any one of salicylate, benzophenone or benzotriazole, and the antioxidant treatment method comprises the following steps: the concentration of the antioxidant auxiliary agent is 20-30g/L, the finishing mode is carried out, the second soaking and the second rolling are carried out, the liquid carrying rate is kept at 80%, and the drying is carried out. The treated jean fabric is subjected to anti-oxidation treatment, so that the reaction of oxygen and dye can be inhibited, and the fabric is endowed with a good dyeing effect.)

1. An anti-oxidation production process of denim fabric is characterized by comprising the following steps:

step one, fully washing the dyed jean fabric until the jean fabric is neutral and does not contain electrolytic impurities;

soaking the wetted fabric in an antioxidant agent, soaking and rolling for two times, keeping the liquid carrying rate of the fabric after the rolling liquid to be 60-80%, and passing through a forming machine at the speed of 20-30 m/min;

step three, drying, cooling and discharging the cloth,

the antioxidant reagent comprises an antioxidant auxiliary agent and water, wherein the antioxidant auxiliary agent is any one of salicylate, benzophenone or benzotriazole, and the concentration of the antioxidant auxiliary agent is 10-15%.

2. The oxidation-resistant production process of denim fabric according to claim 1, characterized in that: the antioxidant reagent also comprises a surfactant, the concentration of the surfactant in the antioxidant reagent is 4-9%, and the surfactant is any one of aliphatic polyoxyethylene ether, sodium laurate and sodium dodecyl benzene sulfonate.

3. The oxidation-resistant production process of denim fabric according to claim 1, characterized in that: the antioxidant reagent also comprises a pH regulator, wherein the concentration of the pH regulator in the antioxidant reagent is 2-6%, and the pH regulator is any one of tetraethylammonium hydroxide/sodium bicarbonate mixed solution and tetrabutylammonium hydroxide/sodium carbonate mixed solution.

4. An anti-oxidation production process of denim fabric, which is characterized by comprising the following steps: the antioxidant reagent contains an antioxidant auxiliary agent, wherein the antioxidant auxiliary agent is any one of natural tannin, natural tannin and natural polyphenol, and the concentration of the antioxidant auxiliary agent is 20-30%;

the antioxidant production process of the antioxidant agent comprises the following three modes:

the method comprises the following steps that firstly, the antioxidant is used for pretreatment, and the denim fabric to be treated is placed in the antioxidant for treatment and then enters a dyeing process;

adding the antioxidant agent into the indigo dye for one-bath dyeing;

and thirdly, the antioxidant is used for after finishing, the dyed jean fabric is placed in the antioxidant to be fully soaked, the jean fabric is soaked and rolled for two times, the liquid carrying rate after the liquid rolling is kept to be 60-80%, and finally the jean fabric is dried.

5. The antioxidant production process of plant indigo-dyed jean fabric according to claim 4, characterized in that: the natural tannin is tannin in gallnut extract, the natural tannin is tannic acid in pomegranate peel extract, and the natural polyphenol is polyphenol extracted from tea leaves.

6. The antioxidant production process of plant indigo-dyed jean fabric according to claim 4, characterized in that: the antioxidant treatment also comprises a surfactant, wherein the surfactant is any one of tea saponin, soapberry extract and tea fruit shell extract, and the concentration of the natural surfactant is 10-15%.

7. The antioxidant production process of plant indigo-dyed jean fabric according to claim 4, characterized in that: the antioxidant reagent also comprises a pH regulator, and the concentration of the pH regulator is 5-10%.

8. The antioxidant production process of plant indigo-dyed jean fabric according to claim 7, characterized in that: the pH regulator is any one of a sodium carbonate/sodium bicarbonate mixed solution and an ammonium sulfate/sodium bicarbonate mixed solution.

9. An antioxidant agent comprises an antioxidant auxiliary agent, a surfactant and a pH regulator, and is characterized in that: the concentration of the antioxidant auxiliary agent is 20-30%, the concentration of the surfactant is 10-15%, the concentration of the pH regulator is 5-10%, and the balance is water; the antioxidant auxiliary agent is any one of tannin in gallnut extract, tannic acid in pomegranate peel extract and polyphenol obtained by tea extraction, the surfactant is any one of tea saponin, soapberry extract and tea fruit shell extract, and the pH regulator is any one of sodium carbonate/sodium bicarbonate mixed solution and ammonium sulfate/sodium bicarbonate mixed solution.

10. An antioxidant agent comprises an antioxidant auxiliary agent, a surfactant and a pH regulator, and is characterized in that: the concentration of the antioxidant auxiliary agent is 10-15%, the concentration of the surfactant is 4-9%, the concentration of the pH regulator is 2-6%, and the balance is water; the antioxidant auxiliary agent is any one of salicylate, benzophenone or benzotriazole, the surfactant is any one of aliphatic polyoxyethylene ether, sodium laurate and sodium dodecyl benzene sulfonate, and the pH regulator is any one of tetraethylammonium hydroxide/sodium bicarbonate mixed solution and tetrabutylammonium hydroxide/sodium carbonate mixed solution.

Technical Field

The application relates to an antioxidant production process of a plant indigo-dyed jean fabric, belonging to the technical field of knitted, woven or warp-knitted fabrics or products which are mainly characterized by adopting special yarn raw materials.

Background

The plant indigo dye is taken from bluegrass plants such as Indigofera tinctoria, Polygonum tinctoria and isatis tinctoria, and has obvious differences from industrial synthetic indigo dyes in production preparation, dyeing mode, dyeing effect and functionality. As the only blue vat dye in a plurality of natural dyes, the dyeing process is more complicated than that of the conventional dye, and the dye mainly goes through three processes (dye reduction, leuco body dyeing and leuco body oxidation). The key to the quality of indigo dyeing is whether the indigo dye can be fully reduced into leuco bodies.

In the production practice, the fabric is subjected to plant indigo reduction dyeing, and after the fabric is placed for a period of time, large-area dyeing defects or white spots at folds often appear. Researchers propose that the color fading phenomenon of the fabric can be caused by that indigo dye molecules are contacted with singlet oxygen molecules to react to generate superoxide anion free radicals, and active oxygen molecules such as the superoxide anion free radicals can damage the molecular structure of the dye.

Disclosure of Invention

In view of the above, the application provides an antioxidant production process of a plant indigo-dyed jean fabric, which endows the jean fabric with antioxidant performance, and an antioxidant auxiliary agent has a special performance of inhibiting oxygen and dye from reacting, and is applied to the pretreatment, dyeing or after-finishing processes of fabrics to realize the antioxidant treatment of the indigo-dyed jean fabric.

Specifically, the method is realized through the following scheme:

in view of the above, the application provides an antioxidant production process of a plant indigo-dyed jean fabric, which endows the jean fabric with antioxidant performance, and an antioxidant auxiliary agent has a special performance of inhibiting oxygen and dye from reacting, and is applied to the pretreatment, dyeing or after-finishing processes of fabrics to realize the antioxidant treatment of the indigo-dyed jean fabric.

Specifically, the method is realized through the following scheme:

an antioxidizing technology for preparing the indigo plant dyed jean fabric includes such steps as putting the jean fabric to be treated in antioxidizing agent, which contains surfactant and pH regulator, and antioxidizing assistant. The antioxidant auxiliary agent comprises natural antioxidant substances and synthetic compounds, and different antioxidant auxiliary agents comprise suitable surfactants and pH regulators, so that the proportional relation among the antioxidant auxiliary agent, the surfactant and the pH regulator and the internal connection mechanism are explained in detail respectively by starting from two types of antioxidant auxiliary agents and combining with the structural characteristics and the specific production process of the plant indigo dye.

The first method comprises the following steps: natural antioxidant auxiliary agent

The main component of the natural antioxidant auxiliary agent is any one of natural tannin, natural tannin and natural polyphenol compounds, and the proportion of the main component is 20-30%; the auxiliary components are 10 to 15 percent of surfactant and 5 to 10 percent of pH regulator respectively, and the balance is deionized water.

Preferably:

the surfactant is any one of tea saponin, soapberry extract and tea fruit shell extract. Based on the fact that the adopted natural antioxidant auxiliary agents are extracted and purified from plants, the proper surfactant is screened to be co-dissolved with the natural antioxidant auxiliary agents, compatibility and ecological environmental protection of the natural antioxidant auxiliary agents and the proper surfactant are reflected, and the penetration, solubilization and diffusion properties of the surfactant are utilized to promote the natural antioxidant substances to be dispersed in the solution.

The natural antioxidant auxiliary agent such as tannin, tannic acid and tea polyphenol needs to be combined with fiber and dye under a certain pH environment to exert the antioxidant capacity of the natural antioxidant auxiliary agent, the phenomenon of light fading of fabrics is reduced, and a proper pH system is helpful for maintaining the chemical stability of the natural antioxidant agent, so the natural antioxidant auxiliary agent is also provided with a pH regulator which is any one of a sodium carbonate/sodium bicarbonate mixed solution and an ammonium sulfate/sodium bicarbonate mixed solution.

In order to obtain a better antioxidant effect of the indigo jean fabric, the application applies the antioxidant auxiliary agent to pretreatment, dyeing and after-finishing respectively according to the structural characteristics of the natural antioxidant auxiliary agent, and the three are mutually enhanced and act together. Therefore, the process of applying the natural antioxidant additive has three types: firstly, the natural antioxidant auxiliary agent is used as a pretreatment agent, a fabric to be dyed is placed in a prepared solution, the temperature is raised to a certain temperature, the operation is carried out for a period of time, and the fabric is taken out for dyeing; secondly, natural antioxidant auxiliary agents are placed in the indigo dye solution and used as co-bath dyeing auxiliary agents to act on the fabric together; and thirdly, taking a natural antioxidant auxiliary agent as an after-finishing agent, putting the indigo dyed fabric into the natural antioxidant auxiliary agent, fully soaking, soaking twice, rolling twice and drying at 70 ℃.

And the second method comprises the following steps: synthetic antioxidant agents

The main component of the synthetic antioxidant reagent is any one of salicylate, benzotriazole and benzophenone, and the proportion of the synthetic antioxidant reagent is 10-15%; the auxiliary materials are synthetic surfactant and pH regulator which respectively account for 4% -9% and 2% -6%, and the balance is deionized water.

Preferably, the surfactant is any one of aliphatic polyoxyethylene ether (such as fatty alcohol polyoxyethylene ether, abbreviated as AEO), sodium laurate and sodium dodecyl benzene sulfonate (abbreviated as LAS), and the nonionic characteristics of the surfactant, such as aliphatic polyoxyethylene ether, are utilized to enable the antioxidant to be sufficiently dispersed and dissolved in the solution system.

The pH regulator is any one of tetraethylammonium hydroxide/sodium bicarbonate mixed solution and tetrabutylammonium hydroxide/sodium carbonate mixed solution. Because synthetic antioxidants such as salicylate, benzotriazole and benzophenone need to be combined with fibers and dyes under a certain pH environment, the antioxidant capacity of the synthetic antioxidants is exerted, and the phenomenon of light fading of fabrics is reduced. In addition, a proper pH system helps maintain the chemical stability of the synthetic antioxidant agent.

The process for synthesizing the antioxidant auxiliary agent is applied, firstly, indigo jean fabric is fully washed, so that the surface of the fabric is neutral and does not contain electrolytic impurities such as salt, alkali and the like; secondly, preparing a synthetic antioxidant auxiliary agent solution in advance, immersing the wetted fabric into the synthetic antioxidant auxiliary agent solution, performing two-time immersion and two-time rolling, keeping the liquid carrying rate at 80%, and passing through a 120 ℃ forming machine at the speed of 20-30 m/min; and cooling and discharging the cloth after drying.

Detailed Description

Example 1: natural antioxidant auxiliary agent

The antioxidant agent mainly comprises:

natural tannin/tea polyphenols/natural tannin 20%

Surfactant (tea saponin) 10%

pH regulator (sodium carbonate/sodium bicarbonate) 5%

The balance of deionized water

Basic performance indexes of the plant indigo denim fabric are as follows: the fastness to dry rubbing is more than 3 grade, the fastness to wet rubbing is more than 3 grade, the fastness to soaping is more than 3 grade, the fastness to sunlight is more than 3 grade, and the phenomenon of dull fading exists.

The natural antioxidant auxiliary agent process is applied, and the antioxidant auxiliary agent is applied to the pretreatment, dyeing and after-finishing processes of the plant indigo jean fabric for combined action.

(1) Preparing antioxidant auxiliary mother liquor in advance, adding the antioxidant auxiliary mother liquor successively according to the formula proportion, and taking natural tea polyphenol as an antioxidant reagent for example to carry out the development of the scheme.

(2) Fully soaking and wetting the fabric to be dyed, putting the fabric in an overflow dyeing machine, adding an antioxidant agent of 5-15 g/L, heating to 80 ℃ at the speed of 1 ℃/min, preserving the heat for 40min, draining water, and taking out;

(3) placing the prepared natural antioxidant reagent in an indigo dye vat at a ratio of 20g/L, putting the fabric into the dye vat to act together with the indigo dye liquor and the antioxidant auxiliary agent, and washing the fabric after overflow dyeing for 60min, wherein the surface of the fabric is neutral and does not contain impurities such as salt, alkali and the like;

(4) preparing a natural antioxidant agent in advance, putting the natural antioxidant agent into a tank according to the proportion of 30-50g/L, soaking and rolling the fabric twice after the fabric is fully wetted, keeping the liquid carrying rate at 80 percent, and drying the fabric at 70 ℃.

The comparison of the plant indigo denim fabric after the anti-oxidation treatment and the non-treatment is shown in table 1.

Table 1: comparison of Natural Oxidation resistant treated Fabric and untreated Fabric Performance

Example 2: synthetic antioxidant aid

The antioxidant agent composition is shown in Table 2, and the balance of Table 2 is made up with deionized water.

Table 2: the remaining constituents of the antioxidant in this example other than water

Serial number	Antioxidant agent	Surface active agent	pH regulator
				1	12% of salicylic acid ester	4％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
2	12% benzotriazole	4％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
				3	12% of benzophenone	4％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
4	10% of salicylic acid ester	5％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
				5	14% of salicylic acid ester	5％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
6	15% of salicylic acid ester	5％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
				7	15% of salicylic acid ester	6％AEO	Mixed solution of tetrabutylammonium hydroxide and sodium carbonate, 6%
8	15% of salicylic acid ester	9％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
				9	15% of salicylic acid ester	6％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
10	15% of salicylic acid ester	6% sodium laurate	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
				11	15% of salicylic acid ester	6％LAS	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
12	12% of benzophenone	9％AEO	4 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
				13	12% of benzophenone	9％AEO	Mixed solution of tetrabutylammonium hydroxide and sodium carbonate, 4%
14	12% of benzophenone	6％LAS	Mixed solution of tetrabutylammonium hydroxide and sodium carbonate, 6%
				15	12% of benzophenone	6％LAS	Mixed solution of tetrabutylammonium hydroxide and sodium carbonate, 5%
16	12% of benzophenone	6％LAS	Mixed solution of tetrabutylammonium hydroxide and sodium carbonate, 4%
				17	15% of salicylic acid ester	4％AEO	5 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate
18	15% of salicylic acid ester	4％AEO	6 percent of mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate

Basic performance indexes of the plant indigo denim fabric are as follows: the fastness to dry rubbing is more than 3 grade, the fastness to wet rubbing is more than 3 grade, the fastness to soaping is more than 3 grade, the fastness to sunlight is more than 3 grade, and the phenomenon of dull fading exists.

The process for synthesizing the antioxidant auxiliary agent comprises the following steps:

(1) fully washing the indigo jean fabric with water to make the surface of the fabric neutral without electrolytic impurities such as salt, alkali and the like;

(2) preparing a synthetic antioxidant agent in advance according to the proportion shown in the table 2, immersing the wetted fabric into the synthetic antioxidant agent, carrying out two-time immersion and two-time rolling, keeping the liquid carrying rate at 80%, and passing through a 120 ℃ forming machine at the speed of 20-30 m/min;

(3) and cooling and discharging the cloth after drying.

The jean fabric is treated by adopting the process, the influence of the antioxidant agents with different configurations in the table 2 on the antioxidant effect of the jean fabric is mainly reflected in the aspects of the color fastness and the light fading of the fabric, and the following can be seen by combining the table 2:

(1) when the same surfactant and pH regulator are adopted, different antioxidants (serial numbers 1, 2 and 3 in a comparison table 2) have different antioxidant effects, salicylate is favorable for improving the characteristic of the fastness to sunlight, benzotriazole is favorable for improving the characteristic of the fastness to soaping of the fabric, benzophenone is favorable for improving the characteristic of the fabric in the aspect of photobleaching, and salicylate is used as a better comprehensive effect; with increasing concentration (compare numbers 1, 4, 5 in table 2), the concentration of antioxidant increases significantly in the fastness to light and in the photobleaching of the fabric.

(2) When the same antioxidant and pH regulator are adopted, different surfactants (the serial numbers 9, 10 and 11 in the comparison table 2) have different effects, the fatty alcohol-polyoxyethylene ether is favorable for improving the characteristic of the color fastness to sunlight of the fabric, the sodium laurate is favorable for improving the characteristic of the fabric, the sodium dodecyl benzene sulfonate is favorable for improving the characteristic of the color fastness to soaping of the fabric, and the fatty alcohol-polyoxyethylene ether is used as a better comprehensive effect; the concentration increases significantly for the surfactant in terms of the fastness of the fabric to sunlight and soaping as the concentration increases (see comparison of numbers 6 and 8 and 3 and 13 in table 2).

(3) When the same antioxidant and surfactant are adopted, different pH regulators (numbers 12 and 13 in the comparison table 2) have different effects, the mixed solution of tetraethyl ammonium hydroxide and sodium bicarbonate is favorable for improving the fastness to soaping of the fabric, the mixed solution of tetrabutyl ammonium hydroxide and sodium carbonate is favorable for improving the fastness to sunlight of the fabric, and the combined effect is better by using the mixed solution of tetraethyl ammonium hydroxide and sodium carbonate; the concentration increases significantly for the surfactant in terms of fabric light fastness and photooxidative fading as the concentration increases (see the comparison of numbers 14, 15 and 16, and 17 and 18 in table 2).

The comparison between the treated and untreated plant indigo denim fabric with the antioxidant agent of the formula No. 8 (preferred example) is shown in Table 3.

Table 3: comparison of the Performance of the synthetic antioxidant Assistant-treated Fabric with untreated Fabric

Comparative example 1: indigo dyeing of conventional fabrics

The conventional plant indigo denim fabric treatment process comprises the following steps:

after the fabric to be dyed is fully wetted and placed in a dyeing machine body, the operation is carried out for 10 to 15 minutes, 2g/L sodium hydrosulfite and 1.5g/L caustic soda are added, so that the dyeing bath and the fabric are in an alkaline environment, and the dye is easy to adsorb and dye;

pre-reduction of plant indigo dye liquor: fully mixing and dissolving the plant indigo powder, the sodium hydrosulfite and the sodium hydroxide according to the proportion of 1:1.25:1 and the bath ratio of 1:50 with clear water to ensure that the solution is yellow green and the pH value is between 11 and 12 for later use;

dyeing of plant indigo: the dye liquor with the concentration of 20 percent of the mother liquor is taken and placed in an auxiliary cylinder of a dyeing machine, and is added in a circulating reflux manner. Refluxing to the auxiliary tank every 20 minutes, measuring the pH value, adding 1.25g/L of sodium hydrosulfite and 1g/L of caustic soda, draining liquid and washing with water after 3 times;

washing the plant indigo dyed fabric: the water enters the washing machine to overflow and wash for 10-15min, the liquor is discharged, the water enters the washing machine to wash, the hydrogen peroxide is added for 1.5g/L, the washing machine is washed by hot water at 80 ℃ for 30min, the washing machine is washed by the clear water, the acetic acid is added for 1.5g/L, the washing machine is washed by the clear water, the oxygenase is added for 1.5g/L, the washing machine is washed by the clear water, the washing machine is dried and the cloth is discharged.

The performance of the conventional plant indigo dyed jean fabric and the fabric subjected to antioxidant treatment are compared as follows:

table 3: conventional plant indigo dyed jean fabric and performance index of treated fabric