Method for fixing color of cotton fabric dyed by plant dye liquor based on compound enzyme catalysis

Abstract

The invention relates to a textile dyeing technology, in particular to a method for fixing a cotton fabric dyed by plant dye liquor based on compound enzyme catalysis. The method comprises the following steps: step 1, extracting plant dye liquor: weighing a plant dye material, adding the plant dye material into distilled water, carrying out extraction treatment, and carrying out solid-liquid separation after the extraction treatment is completed, so as to obtain the plant dye liquor; step 2, dyeing and fixation of the cotton fabric with plant dye liquor: the cotton fabric is placed in the plant dye liquor for dyeing treatment, and after dyeing treatment is completed, the dyed cotton fabric is taken out; adding a color fixing agent into the plant dye liquor of the dyed cotton fabric, and mixing and dissolving to obtain plant dye liquor containing the color fixing agent; and putting the dyed cotton fabric into a plant dyeing solution containing a color fixing agent, and carrying out color fixing treatment to obtain the dyed and fixed cotton fabric. The dyed cotton fabric subjected to compound enzyme catalytic color fixation treatment has good color fastness, the color changing and fading fastness is improved, the staining grade is high, and the light fastness is improved.

Description

Technical Field

[0001] The invention relates to textile dyeing technology, in particular to a color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis. Background Art

[0002] In nature, there are many plant materials that can be used for natural fiber dyeing. Fiber coloring usually uses plant skin, leaves, roots, fruits, flowers and stems. Plant dyeing was formed in the process of human understanding of nature and living in harmony with nature. In the long-term production practice, people have mastered the extraction and dyeing techniques of various plant dyes and produced a variety of textile products. This process is a reflection of the ancient Chinese working people's compliance with nature and protection of nature. To this day, this skill is still being developed and inherited. With the development of the textile industry, the dyeing technology of plant dyes has also been greatly improved. Fabrics dyed with plant dyes can present various patterns and textures. The well-known ones are tie-dyeing, batik, blue printed cloth, etc. Plant dyes can be divided into indoles, anthraquinones, α-naphthoquinones, flavonoids, diketones, chalcone, dihydropyrans, carotenoids, isoquinolines, anthocyanins, chlorophylls and polyphenols according to their chemical structure.

[0003] Since plant dyes are derived from nature and are green and safe, they meet people's demand for nature and green safety. Therefore, the production of plant dyes, plant dyeing and the development of related products have received extensive attention. However, due to the disadvantages of low dye uptake and poor color fastness of plant dyes, mordants are generally required during dyeing. The application of mordants can enrich the hue and lightness of plant dyeing. In addition, mordants also play a certain role in improving the dye uptake and color fastness of plant dyes. However, the unfriendly nature of heavy metal salts as mordants to the human body and the environment restricts their application in the textile industry. Summary of the invention

[0004] In view of the shortcomings of the prior art, the present invention provides a color fixation method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis to solve the problems of low dye uptake, poor color fastness, harm of mordant containing heavy metal ions and wastewater treatment in the prior art of plant dyeing.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is as follows:

[0006] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0007] Step 1: Extraction of plant dye solution

[0008] Weighing the plant dye material, adding it into distilled water, and performing extraction treatment, after the extraction treatment is completed, performing solid-liquid separation to obtain the plant dye solution;

[0009] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0010] placing the cotton fabric in the plant dye solution for dyeing, and taking out the dyed cotton fabric after the dyeing is completed;

[0011] Adding a composite enzyme color-fixing agent to the plant dyeing solution of the dyed cotton fabric, mixing and dissolving, and obtaining a plant dyeing solution containing the composite enzyme color-fixing agent;

[0012] The dyed cotton fabric is placed in a plant dye solution containing a composite enzyme color-fixing agent to perform a color-fixing treatment. After the color-fixing treatment is completed, the fabric is taken out, washed with water, and dried to obtain the dyed and color-fixed cotton fabric.

[0013] Preferably, in step 1, the plant dyes include Sappanwood, Rubia cordifolia, Sophora japonica, Gardenia jasminoides, Curcuma longa, and Lithospermum officinale.

[0014] Preferably, the plant dye is hematoxylin.

[0015] Preferably, in step 1, the mass volume of the plant dye and distilled water is 20-300 g / L, and the extraction treatment condition is to extract at a temperature of 80-100° C. for 20-60 min.

[0016] Preferably, in step 2, the bath ratio of the cotton fabric to the plant dye liquor is 1:(20-50).

[0017] Preferably, in step 2, the dyeing treatment is performed at 30-100° C. for 20-60 min.

[0018] Preferably, in step 2, the mass volume of the complex enzyme fixing agent and the plant dye solution is 1-5 g / L.

[0019] Preferably, in step 2, the complex enzyme color-fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid.

[0020] Preferably, in the composite enzyme color-fixing agent, the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:(1-1.5):(0.05-0.25).

[0021] Preferably, in step 2, the color fixing treatment is performed at a temperature of 30-90° C. for 0.5-4 h.

[0022] In the present invention, laccase, as a copper-containing polyphenol oxidase, can catalyze the self-crosslinking of polyphenol plant dyes containing phenolic hydroxyl groups in the molecular structure through free radical coupling, replace the complex coupling effect of metal mordants on plant dyes, and generate dyes with larger molecular weight, so as to improve the dyeing properties of textiles (such as color depth, dye uptake, color fastness, etc.). In addition, since it does not contain heavy metal ions, the formed color light is bright and close to the color tone of the plant dye itself, without the dull feeling caused by the complexation of metal mordants; tetramethylpiperidinium nitrogen oxide is a selective oxidant, with the assistance of which the action substrate range of laccase can be expanded from phenolic substances to cellulose substances, and the primary hydroxyl groups of cellulose in cotton fabrics are catalytically oxidized to form aldehyde groups, and react with the plant dyes after enzymatic coupling to form covalent bonds, thereby realizing the use of an enzyme system instead of metal mordants for mordant-free fixation of plant dyes.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] In the present invention, since the composite enzyme can catalyze the phenolic hydroxyl groups in the structure of the plant dye and the primary alcohol hydroxyl groups in the cellulose of the cotton fabric, the plant dye can undergo cross-linking or even polymerization to produce a high-molecular-weight colored substance with a dark-color effect, and the high-molecular-weight colored substance is bonded to the cotton fabric by means of the covalent bonds generated by the reaction with the cellulose aldehyde group, thereby improving the color depth, color fastness to washing, color fastness to sunlight, etc. of the dyed cotton fabric. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The K / S curves of cotton fabrics dyed and fixed with different concentrations of hematoxylin dye solutions as the absorption wavelength changes;

[0026] Figure 2 The K / S curves of cotton fabric dyed and fixed by hematoxylin dye solution at different fixation temperatures as the absorption wavelength changes;

[0027] Figure 3 The maximum K / S value at 460 nm of the cotton fabric dyed and fixed by the hematoxylin dye solution prepared in Example 3 and Comparative Example 1 of the present invention varies with the fixing time;

[0028] Figure 4 The maximum K / S value at 460 nm of the cotton fabric dyed and fixed by the hematoxylin dye solution prepared in Example 4 and Comparative Example 2 of the present invention varies with the fixing time;

[0029] Figure 5 The maximum K / S value at 460 nm of the cotton fabric dyed and fixed by the hematoxylin dye solution prepared in Example 5 and Comparative Example 3 of the present invention varies with the fixing time;

[0030] Figure 6The maximum K / S value at 460 nm of the cotton fabric dyed and fixed by the hematoxylin dye solution prepared in Example 6 and Comparative Example 4 of the present invention varies with the fixing time;

[0031] Figure 7 This is a physical comparison diagram of the cotton fabric samples obtained by fixing for 30 minutes in Comparative Example 1 of the present invention, the cotton fabric obtained by fixing for 30 minutes in Example 3, the cotton fabric obtained by fixing for 2 hours in Comparative Example 3, and the cotton fabric samples obtained by fixing for 2 hours in Example 5. DETAILED DESCRIPTION

[0032] 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 part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0033] Example 1

[0034] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0035] Weigh 7 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 30g / L, 50g / L, 70g / L, 90g / L, 130g / L, 200g / L, 300g / L respectively, extract at 95℃ for 30min, after the extraction treatment is completed, perform solid-liquid separation, and obtain 7 groups of hematoxylin dye solution;

[0036] Among them, when the mass volume ratio of hematoxylin heartwood to distilled water is 30g / L, the obtained hematoxylin dye solution is recorded as 30g / L hematoxylin dye solution; when the mass volume ratio of hematoxylin heartwood to distilled water is 50g / L, the obtained hematoxylin dye solution is recorded as 50g / L hematoxylin dye solution; when the mass volume ratio of hematoxylin heartwood to distilled water is 70g / L, the obtained hematoxylin dye solution is recorded as 70g / L hematoxylin dye solution; when the mass volume ratio of hematoxylin heartwood to distilled water is 90g / L, The obtained hematoxylin dye solution is recorded as 90 g / L hematoxylin dye solution; when the mass volume ratio of hematoxylin heartwood to distilled water is 130 g / L, the obtained hematoxylin dye solution is recorded as 130 g / L hematoxylin dye solution; when the mass volume ratio of hematoxylin heartwood to distilled water is 200 g / L, the obtained hematoxylin dye solution is recorded as 200 g / L hematoxylin dye solution; when the mass volume ratio of hematoxylin heartwood to distilled water is 300 g / L, the obtained hematoxylin dye solution is recorded as 300 g / L hematoxylin dye solution;

[0037] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0038] The cotton fabrics were placed in 7 groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0039] Adding a composite enzyme fixing agent to 7 groups of hematoxylin dye solutions of the dyed cotton fabric respectively, the mass volume ratio of the composite enzyme fixing agent to the hematoxylin dye solution is 1 g / L, and after mixing and dissolving, 7 groups of hematoxylin dye solutions containing the composite enzyme fixing agent are obtained, namely, 30 g / L hematoxylin dye solution containing the composite enzyme fixing agent, 50 g / L hematoxylin dye solution containing the composite enzyme fixing agent, 70 g / L hematoxylin dye solution containing the composite enzyme fixing agent, 90 g / L hematoxylin dye solution containing the composite enzyme fixing agent, 130 g / L hematoxylin dye solution containing the composite enzyme fixing agent, 200 g / L hematoxylin dye solution containing the composite enzyme fixing agent, and 300 g / L hematoxylin dye solution containing the composite enzyme fixing agent;

[0040] The composite enzyme color fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid, and the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:1.25:0.25;

[0041] The dyed cotton fabrics were placed in the corresponding hematoxylin dye solution containing a composite enzyme fixing agent for fixation treatment, that is, the cotton fabrics dyed in 30g / L hematoxylin dye solution were placed in 30g / L hematoxylin dye solution containing a composite enzyme fixing agent, the cotton fabrics dyed in 50g / L hematoxylin dye solution were placed in 50g / L hematoxylin dye solution containing a composite enzyme fixing agent, the cotton fabrics dyed in 70g / L hematoxylin dye solution were placed in 70g / L hematoxylin dye solution containing a composite enzyme fixing agent, and the cotton fabrics dyed in 90g / L hematoxylin dye solution were placed in 90g / L hematoxylin dye solution containing a composite enzyme fixing agent. The cotton fabric dyed in 130 g / L hematoxylin dye solution was placed in 130 g / L hematoxylin dye solution containing a composite enzyme fixing agent, the cotton fabric dyed in 200 g / L hematoxylin dye solution was placed in 200 g / L hematoxylin dye solution containing a composite enzyme fixing agent, and the cotton fabric dyed in 300 g / L hematoxylin dye solution was placed in 300 g / L hematoxylin dye solution containing a composite enzyme fixing agent, and fixed the color at 50°C for 30 minutes. After the color fixing treatment was completed, the fabric was taken out, washed with water, and dried to obtain 7 groups of dyed and fixed cotton fabrics;

[0042] The 7 groups of cotton fabrics after dyeing and fixing were recorded as 30 g / L hematoxylin dye solution dyed-fixed cotton fabric, 50 g / L hematoxylin dye solution dyed-fixed cotton fabric, 70 g / L hematoxylin dye solution dyed-fixed cotton fabric, 90 g / L hematoxylin dye solution dyed-fixed cotton fabric, 130 g / L hematoxylin dye solution dyed-fixed cotton fabric, 200 g / L hematoxylin dye solution dyed-fixed cotton fabric, and 300 g / L hematoxylin dye solution dyed-fixed cotton fabric;

[0043] The K / S curves of 7 groups of cotton fabrics dyed and fixed with hematoxylin dye solution were measured and recorded respectively as the absorption wavelength changed.

[0044] Depend on Figure 1 It can be seen that the K / S value of the dyed fixed cotton fabric reaches the maximum at 460nm, the fabric appears yellow, and the K / S value curve increases continuously with the increase of the hematoxylin dye concentration.

[0045] Example 2

[0046] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0047] Weigh 4 groups of hematoxylin heartwood, add them into distilled water, the mass volume ratio of hematoxylin heartwood to distilled water is 20g / L, 20g / L, 50g / L, 50g / L respectively, extract at 95℃ for 30min, after the extraction, separate the solid and liquid to obtain 4 groups of hematoxylin dye solution;

[0048] When the mass volume ratio of hematoxylin heartwood to distilled water is 20 g / L, the obtained hematoxylin dye solution is recorded as 20 g / L hematoxylin dye solution-1 and 20 g / L hematoxylin dye solution-2; when the mass volume ratio of hematoxylin heartwood to distilled water is 50 g / L, the obtained hematoxylin dye solution is recorded as 50 g / L hematoxylin dye solution-1 and 50 g / L hematoxylin dye solution-2;

[0049] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0050] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0051] Adding a composite enzyme fixing agent to the four groups of hematoxylin dye solutions of the dyed cotton fabrics respectively, the mass volume ratio of the composite enzyme fixing agent to the hematoxylin dye solution is 1 g / L, and after mixing and dissolving, four groups of hematoxylin dye solutions containing the composite enzyme fixing agent are obtained, namely, 20 g / L hematoxylin dye solution-1 containing the composite enzyme fixing agent, 20 g / L hematoxylin dye solution-2 containing the composite enzyme fixing agent, 50 g / L hematoxylin dye solution-1 containing the composite enzyme fixing agent, and 50 g / L hematoxylin dye solution-2 containing the composite enzyme fixing agent;

[0052] The composite enzyme color fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid, and the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:1.25:0.25;

[0053] The dyed cotton fabrics are placed in the corresponding hematoxylin dye solutions containing a composite enzyme color fixing agent for color fixing treatment, that is, the cotton fabric dyed in 20g / L hematoxylin dye solution-1 is placed in 20g / L hematoxylin dye solution-1 containing a composite enzyme color fixing agent, the cotton fabric dyed in 50g / L hematoxylin dye solution-1 is placed in 50g / L hematoxylin dye solution-1 containing a composite enzyme color fixing agent, and the color is fixed at 50°C for 60min, the cotton fabric dyed in 20g / L hematoxylin dye solution-2 is placed in 20g / L hematoxylin dye solution-2 containing a composite enzyme color fixing agent, and the cotton fabric dyed in 50g / L hematoxylin dye solution-2 is placed in 50g / L hematoxylin dye solution-2 containing a composite enzyme color fixing agent, first at 50°C for 30min, and then at 90°C for 30min, after the color fixing treatment is completed, the cotton fabrics are taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics;

[0054] The four groups of dyed and fixed cotton fabrics were recorded as 20g / L hematoxylin dye solution dyed and fixed cotton fabric at 50℃ for 60min; 20g / L hematoxylin dye solution dyed and fixed cotton fabric at 50℃ for 30min and then at 90℃ for 30min; 50g / L hematoxylin dye solution dyed and fixed cotton fabric at 50℃ for 60min; 50g / L hematoxylin dye solution dyed and fixed cotton fabric at 50℃ for 30min and then at 90℃ for 30min;

[0055] The K / S curves of 4 groups of cotton fabrics dyed and fixed with hematoxylin dye solution were measured and recorded respectively as the absorption wavelength changed.

[0056] Depend on Figure 2 It can be seen that the fixing effect at 50°C is better than that at 90°C. This may be because the increase in temperature accelerates the adsorption and desorption of dyes, and the dyeing rate decreases instead.

[0057] Example 3

[0058] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0059] Step 1: Extraction of plant dye solution

[0060] Weigh 4 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 20 g / L, extract at 95°C for 30 min, after the extraction treatment, perform solid-liquid separation, and obtain 4 groups of hematoxylin dye solution with a concentration of 20 g / L, which are respectively recorded as 20 g / L hematoxylin dye solution-1, 20 g / L hematoxylin dye solution-2, 20 g / L hematoxylin dye solution-3, and 20 g / L hematoxylin dye solution-4;

[0061] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0062] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0063] Adding a composite enzyme color-fixing agent to the four groups of hematoxylin dyeing solutions of the dyed cotton fabrics respectively, the mass volume ratio of the composite enzyme color-fixing agent to the hematoxylin dyeing solution is 1 g / L, and after mixing and dissolving, four groups of hematoxylin dyeing solutions containing the composite enzyme color-fixing agent are obtained, namely, 20 g / L hematoxylin dyeing solution-1 containing the composite enzyme color-fixing agent, 20 g / L hematoxylin dyeing solution-2 containing the composite enzyme color-fixing agent, 20 g / L hematoxylin dyeing solution-3 containing the composite enzyme color-fixing agent, and 20 g / L hematoxylin dyeing solution-4 containing the composite enzyme color-fixing agent;

[0064] The composite enzyme color fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid, and the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:1.25:0.25;

[0065] The dyed cotton fabrics were placed in the corresponding hematoxylin dye solution containing a composite enzyme fixing agent for fixing treatment, that is, the cotton fabrics dyed in 20g / L hematoxylin dye solution-1 were placed in 20g / L hematoxylin dye solution-1 containing a composite enzyme fixing agent and fixed at 50°C for 30min, and the cotton fabrics dyed in 20g / L hematoxylin dye solution-2 were placed in 20g / L hematoxylin dye solution-2 containing a composite enzyme fixing agent and fixed at 50°C. After treatment for 1 hour, the cotton fabric dyed in 20 g / L hematoxylin dye solution-3 was placed in 20 g / L hematoxylin dye solution-3 containing a composite enzyme fixing agent and subjected to a fixing treatment at 50°C for 2 hours. The cotton fabric dyed in 20 g / L hematoxylin dye solution-4 was placed in 20 g / L hematoxylin dye solution-4 containing a composite enzyme fixing agent and subjected to a fixing treatment at 50°C for 4 hours. After the fixing treatment was completed, the fabric was taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics.

[0066] The maximum K / S value at 460nm of the four groups of dyed and fixed cotton fabrics as a function of fixation time was measured and recorded respectively.

[0067] Example 4

[0068] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0069] Step 1: Extraction of plant dye solution

[0070] Weigh three groups of hematoxylin heartwood, add them into distilled water, the mass volume ratio of hematoxylin heartwood to distilled water is 50 g / L, extract at 95°C for 30 min, after the extraction, perform solid-liquid separation, and obtain three groups of hematoxylin dye solution with a concentration of 50 g / L, which are respectively recorded as 50 g / L hematoxylin dye solution-1, 50 g / L hematoxylin dye solution-2, and 50 g / L hematoxylin dye solution-3;

[0071] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0072] The cotton fabrics were placed in three groups of hematoxylin dyeing solutions respectively, with the bath ratio of the cotton fabric to the hematoxylin dyeing solution being 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0073] Adding a composite enzyme fixing agent to the three groups of hematoxylin dyeing solutions of the dyed cotton fabrics respectively, the mass volume ratio of the composite enzyme fixing agent to the hematoxylin dyeing solution is 1 g / L, and after mixing and dissolving, three groups of hematoxylin dyeing solutions containing the composite enzyme fixing agent are obtained, namely, 50 g / L hematoxylin dyeing solution-1 containing the composite enzyme fixing agent, 50 g / L hematoxylin dyeing solution-2 containing the composite enzyme fixing agent, and 50 g / L hematoxylin dyeing solution-3 containing the composite enzyme fixing agent;

[0074] The composite enzyme color fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid, and the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:1.25:0.25;

[0075] The dyed cotton fabrics are placed in the corresponding hematoxylin dye solutions containing a composite enzyme color fixing agent for color fixing treatment, that is, the cotton fabrics dyed in 50 g / L hematoxylin dye solution-1 are placed in 50 g / L hematoxylin dye solution-1 containing a composite enzyme color fixing agent, and color fixing treatment is performed at 50°C for 30 minutes, the cotton fabrics dyed in 50 g / L hematoxylin dye solution-2 are placed in 50 g / L hematoxylin dye solution-2 containing a composite enzyme color fixing agent, and color fixing treatment is performed at 50°C for 1 hour, and the cotton fabrics dyed in 50 g / L hematoxylin dye solution-3 are placed in 50 g / L hematoxylin dye solution-3 containing a composite enzyme color fixing agent, and color fixing treatment is performed at 50°C for 2 hours. After the color fixing treatment is completed, the cotton fabrics are taken out, washed with water, and dried to obtain 3 groups of dyed and fixed cotton fabrics;

[0076] The maximum K / S value of the three groups of cotton fabrics after dyeing and fixing at 460nm was measured and recorded along with the fixing time.

[0077] Example 5

[0078] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0079] Step 1: Extraction of plant dye solution

[0080] Weigh 4 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 150 g / L, extract at 95°C for 30 min, after the extraction treatment, perform solid-liquid separation, and obtain 4 groups of hematoxylin dye solution with a concentration of 150 g / L, which are respectively recorded as 150 g / L hematoxylin dye solution-1, 150 g / L hematoxylin dye solution-2, 150 g / L hematoxylin dye solution-3, and 150 g / L hematoxylin dye solution-4;

[0081] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0082] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0083] Adding a composite enzyme fixing agent to the four groups of hematoxylin dye solutions of the dyed cotton fabrics respectively, the mass volume ratio of the composite enzyme fixing agent to the hematoxylin dye solution is 1 g / L, and after mixing and dissolving, four groups of hematoxylin dye solutions containing the composite enzyme fixing agent are obtained, namely, 150 g / L hematoxylin dye solution-1 containing the composite enzyme fixing agent, 150 g / L hematoxylin dye solution-2 containing the composite enzyme fixing agent, 150 g / L hematoxylin dye solution-3 containing the composite enzyme fixing agent, and 150 g / L hematoxylin dye solution-4 containing the composite enzyme fixing agent;

[0084] The composite enzyme color fixing agent is a complex of laccase, tetramethylpiperidine nitrogen oxide and citric acid, and the mass ratio of laccase, tetramethylpiperidine nitrogen oxide and citric acid is 1:1.25:0.25; the dyed cotton fabrics are respectively placed in the corresponding hematoxylin dye solutions containing the composite enzyme color fixing agent for color fixing treatment, that is, the cotton fabrics dyed in 150g / L hematoxylin dye solution-1 are placed in 150g / L hematoxylin dye solution-1 containing the composite enzyme color fixing agent, and the color fixing treatment is carried out at a temperature of 50°C for 30min; the cotton fabrics dyed in 150g / L hematoxylin dye solution-2 are placed in The cotton fabric dyed in 150 g / L hematoxylin dye solution-2 containing a composite enzyme color fixing agent is subjected to a color fixing treatment at 50°C for 1 hour. The cotton fabric dyed in 150 g / L hematoxylin dye solution-3 is subjected to a color fixing treatment at 50°C for 2 hours. The cotton fabric dyed in 150 g / L hematoxylin dye solution-4 is subjected to a color fixing treatment at 50°C for 4 hours. After the color fixing treatment is completed, the cotton fabric is taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics.

[0085] The maximum K / S value at 460nm of the four groups of dyed and fixed cotton fabrics as a function of fixation time was measured and recorded respectively.

[0086] Example 6

[0087] A color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis comprises the following steps:

[0088] Step 1: Extraction of plant dye solution

[0089] Weigh 4 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 200 g / L, extract at 95°C for 30 min, after the extraction treatment is completed, perform solid-liquid separation, and obtain 4 groups of hematoxylin dye solution with a concentration of 200 g / L, which are respectively recorded as 200 g / L hematoxylin dye solution-1, 200 g / L hematoxylin dye solution-2, 200 g / L hematoxylin dye solution-3, and 200 g / L hematoxylin dye solution-4;

[0090] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0091] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0092] Adding a composite enzyme fixing agent to the four groups of hematoxylin dye solutions of the dyed cotton fabrics respectively, the mass volume ratio of the composite enzyme fixing agent to the hematoxylin dye solution is 1 g / L, and after mixing and dissolving, four groups of hematoxylin dye solutions containing the composite enzyme fixing agent are obtained, namely, 200 g / L hematoxylin dye solution-1 containing the composite enzyme fixing agent, 200 g / L hematoxylin dye solution-2 containing the composite enzyme fixing agent, 200 g / L hematoxylin dye solution-3 containing the composite enzyme fixing agent, and 200 g / L hematoxylin dye solution-4 containing the composite enzyme fixing agent;

[0093] The complex enzyme color fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid, and the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:1.25:0.25;

[0094] The dyed cotton fabrics were placed in the corresponding hematoxylin dye solution containing a composite enzyme fixing agent for fixation treatment, that is, the cotton fabrics dyed in 200 g / L hematoxylin dye solution-1 were placed in 200 g / L hematoxylin dye solution-1 containing a composite enzyme fixing agent and fixed at 50°C for 30 min, and the cotton fabrics dyed in 200 g / L hematoxylin dye solution-2 were placed in 200 g / L hematoxylin dye solution-2 containing a composite enzyme fixing agent and fixed at 50°C for 30 min. The cotton fabric dyed in 200 g / L hematoxylin dye solution-3 was placed in 200 g / L hematoxylin dye solution-3 containing a composite enzyme color fixing agent and subjected to color fixing treatment at 50°C for 2 hours. The cotton fabric dyed in 200 g / L hematoxylin dye solution-4 was placed in 200 g / L hematoxylin dye solution-4 containing a composite enzyme color fixing agent and subjected to color fixing treatment at 50°C for 4 hours. After the color fixing treatment was completed, the fabric was taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics.

[0095] The maximum K / S value at 460nm of the four groups of dyed and fixed cotton fabrics as a function of fixation time was measured and recorded respectively.

[0096] Comparative Example 1

[0097] A method for fixing the color of cotton fabric dyed with plant dye liquor comprises the following steps:

[0098] Step 1: Extraction of plant dye solution

[0099] Weigh 4 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 20 g / L, extract at 95°C for 30 min, after the extraction treatment, perform solid-liquid separation, and obtain 4 groups of hematoxylin dye solution with a concentration of 20 g / L, which are respectively recorded as 20 g / L hematoxylin dye solution-1, 20 g / L hematoxylin dye solution-2, 20 g / L hematoxylin dye solution-3, and 20 g / L hematoxylin dye solution-4;

[0100] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0101] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0102] The dyed cotton fabrics are respectively placed in their respective corresponding hematoxylin dye solutions for dyeing treatment, that is, the cotton fabrics dyed in 20g / L hematoxylin dye solution-1 are placed in 20g / L hematoxylin dye solution-1 again, and a color fixation treatment is performed at 50°C for 30min, the cotton fabrics dyed in 20g / L hematoxylin dye solution-2 are placed in 20g / L hematoxylin dye solution-2 again, and a color fixation treatment is performed at 50°C for 1h, the cotton fabrics dyed in 20g / L hematoxylin dye solution-3 are placed in 20g / L hematoxylin dye solution-3 again, and a color fixation treatment is performed at 50°C for 2h, the cotton fabrics dyed in 20g / L hematoxylin dye solution-4 are placed in 20g / L hematoxylin dye solution-4 again, and a color fixation treatment is performed at 50°C for 4h, after the color fixation treatment is completed, the cotton fabrics are taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics;

[0103] The maximum K / S value at 460nm of the four groups of dyed and fixed cotton fabrics as a function of fixation time was measured and recorded respectively.

[0104] Comparative Example 2

[0105] A method for fixing the color of cotton fabric dyed with plant dye liquor comprises the following steps:

[0106] Step 1: Extraction of plant dye solution

[0107] Weigh three groups of hematoxylin heartwood, add them into distilled water, the mass volume ratio of hematoxylin heartwood to distilled water is 50 g / L, extract at 95°C for 30 min, after the extraction, perform solid-liquid separation, and obtain three groups of hematoxylin dye solution with a concentration of 50 g / L, which are respectively recorded as 50 g / L hematoxylin dye solution-1, 50 g / L hematoxylin dye solution-2, and 50 g / L hematoxylin dye solution-3;

[0108] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0109] The cotton fabrics were placed in three groups of hematoxylin dyeing solutions respectively, with the bath ratio of the cotton fabric to the hematoxylin dyeing solution being 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0110] The dyed cotton fabrics are respectively placed in their respective corresponding hematoxylin dye solutions for fixation treatment, that is, the cotton fabrics dyed in 50 g / L hematoxylin dye solution-1 are placed in 50 g / L hematoxylin dye solution-1 for fixation treatment at 50°C for 30 min, the cotton fabrics dyed in 50 g / L hematoxylin dye solution-2 are placed in 50 g / L hematoxylin dye solution-2 for fixation treatment at 50°C for 1 h, and the cotton fabrics dyed in 50 g / L hematoxylin dye solution-3 are placed in 50 g / L hematoxylin dye solution-3 for fixation treatment at 50°C for 2 h. After the fixation treatment is completed, the cotton fabrics are taken out, washed with water, and dried to obtain 3 groups of dyed and fixed cotton fabrics;

[0111] The maximum K / S value of the three groups of cotton fabrics after dyeing and fixing at 460nm was measured and recorded along with the fixing time.

[0112] Comparative Example 3

[0113] A method for fixing the color of cotton fabric dyed with plant dye liquor comprises the following steps:

[0114] Step 1: Extraction of plant dye solution

[0115] Weigh 4 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 150 g / L, extract at 95°C for 30 min, after the extraction treatment, perform solid-liquid separation, and obtain 4 groups of hematoxylin dye solution with a concentration of 150 g / L, which are respectively recorded as 150 g / L hematoxylin dye solution-1, 150 g / L hematoxylin dye solution-2, 150 g / L hematoxylin dye solution-3, and 150 g / L hematoxylin dye solution-4;

[0116] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0117] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0118] The dyed cotton fabrics are respectively placed in their corresponding hematoxylin dye solutions for fixation treatment, that is, the cotton fabrics dyed in 150g / L hematoxylin dye solution-1 are placed in 150g / L hematoxylin dye solution-1 for fixation treatment at 50°C for 30min, the cotton fabrics dyed in 150g / L hematoxylin dye solution-2 are placed in 150g / L hematoxylin dye solution-2 for fixation treatment at 50°C for 1h, the cotton fabrics dyed in 150g / L hematoxylin dye solution-3 are placed in 150g / L hematoxylin dye solution-3 for fixation treatment at 50°C for 2h, the cotton fabrics dyed in 150g / L hematoxylin dye solution-4 are placed in 150g / L hematoxylin dye solution-4 for fixation treatment at 50°C for 4h, and after the fixation treatment is completed, the cotton fabrics are taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics;

[0119] The maximum K / S value at 460nm of the four groups of dyed and fixed cotton fabrics as a function of fixation time was measured and recorded respectively.

[0120] Comparative Example 4

[0121] A method for fixing the color of cotton fabric dyed with plant dye liquor comprises the following steps:

[0122] Step 1: Extraction of plant dye solution

[0123] Weigh 4 groups of hematoxylin heartwood, add them into distilled water respectively, the mass volume ratio of hematoxylin heartwood to distilled water is 200 g / L, extract at 95°C for 30 min, after the extraction treatment is completed, perform solid-liquid separation, and obtain 4 groups of hematoxylin dye solution with a concentration of 200 g / L, which are respectively recorded as 200 g / L hematoxylin dye solution-1, 200 g / L hematoxylin dye solution-2, 200 g / L hematoxylin dye solution-3, and 200 g / L hematoxylin dye solution-4;

[0124] Step 2: Dyeing and fixing of cotton fabrics with plant dyes

[0125] The cotton fabrics were placed in four groups of hematoxylin dyeing solutions, the bath ratio of the cotton fabrics to the hematoxylin dyeing solution was 1:50, and dyed at 50°C for 30 minutes. After the dyeing process was completed, the dyed cotton fabrics were taken out;

[0126] The dyed cotton fabrics are respectively placed in the corresponding hematoxylin dye solution for fixation treatment, that is, the cotton fabrics dyed in 200g / L hematoxylin dye solution-1 are placed in 200g / L hematoxylin dye solution-1 for fixation treatment at 50°C for 30min, the cotton fabrics dyed in 200g / L hematoxylin dye solution-2 are placed in 200g / L hematoxylin dye solution-2 for fixation treatment at 50°C for 1h, the cotton fabrics dyed in 200g / L hematoxylin dye solution-3 are placed in 200g / L hematoxylin dye solution-3 for fixation treatment at 50°C for 2h, the cotton fabrics dyed in 200g / L hematoxylin dye solution-4 are placed in 200g / L hematoxylin dye solution-4 for fixation treatment at 50°C for 4h, and after the fixation treatment is completed, the cotton fabrics are taken out, washed with water, and dried to obtain 4 groups of dyed and fixed cotton fabrics;

[0127] The maximum K / S value at 460nm of the four groups of dyed and fixed cotton fabrics as a function of fixation time was measured and recorded respectively.

[0128] The maximum K / S value of the cotton fabric in Example 3 and Comparative Example 1 varies with the fixation time. Figure 3 As shown by Figure 3 It can be seen that when the concentration of hematoxylin dye solution is 20g / L and the fixing time is 30min, the fixing effect is the best. The K / S value of the control cotton fabric is 0.953, and the K / S value of the cotton fabric with the addition of complex enzyme fixing reaches 1.542. When the fixing time exceeds 30min, the fixing effect decreases.

[0129] The maximum K / S value of the cotton fabric in Example 4 and Comparative Example 2 varies with the fixation time. Figure 4 As shown by Figure 4 It can be seen that after adding composite enzyme to fix the color for 1 hour, the K / S value reaches 2.432, and the fixation effect is the best. When the fixation time exceeds 1 hour, the K / S value of the dyed cotton fabric decreases, and the fixation effect becomes worse.

[0130] The maximum K / S value of the cotton fabric in Example 5 and Comparative Example 3 varies with the fixation time. Figure 5 As shown by Figure 5 It can be seen that after adding complex enzyme to fix the color for 2 hours, the K / S value of the dyed cotton fabric reaches 5.401, and the color depth reaches the highest. As the fixation time increases, the K / S value of the cotton fabric decreases, and the fixation effect decreases.

[0131] The maximum K / S value of the cotton fabric in Example 6 and Comparative Example 4 varies with the fixation time. Figure 6 As shown by Figure 6 It can be seen that after adding the composite enzyme for 2 hours of color fixation, the K / S value of the dyed fabric reached 3.755 and the color depth reached the highest. As the color fixation time increased, the K / S value of the cotton fabric decreased and the color fixation effect decreased.

[0132] According to the above test results, the color fixation effect of cotton fabric dyed with plant dye is best when the concentration of hematoxylin dye is 150g / L and the compound enzyme fixation time is 2h.

[0133] The actual picture of the cotton fabric sample after dyeing and fixing prepared by the present invention is as follows: Figure 7 As shown, Figure 7 In the figure, the upper left is the cotton fabric sample obtained by fixing for 30 min in Comparative Example 1, the upper right is the cotton fabric sample obtained by fixing for 30 min in Example 3, the lower left is the cotton fabric sample obtained by fixing for 2 h in Comparative Example 3, and the lower right is the cotton fabric sample obtained by fixing for 2 h in Example 5. It can be seen that compared with not using the composite enzyme fixing agent, the cotton fabric dyeing effect obtained by using the composite enzyme fixing agent is good, and compared with 20 g / L hematoxylin dye solution, the cotton fabric dyeing effect obtained by using 150 g / L hematoxylin dye solution is good.

[0134] Test example

[0135] Determine the color fastness of the cotton fabric dyed and fixed for 2 hours in Example 5 and Comparative Example 3 (i.e., using 150 g / L hematoxylin dye solution):

[0136] The grading index of colorfastness to fading, color staining grade and light fastness were measured respectively. The results are shown in Table 1:

[0137] Table 1

[0138] Rating Index Color staining level Light fastness / grade Example 5 0.13 4-5 1-2 Comparative Example 3 0.02 4-5 1

[0139] As shown in Table 1, the dyed cotton fabric treated with composite enzyme fixation has good dyeing fastness, improved fading fastness, high staining grade, and improved light fastness.

[0140] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for fixing the color of cotton fabric dyed with plant dye liquor based on composite enzyme catalysis, characterized in that: The following steps are involved: Step 1: Extraction of plant dye solution Weighing the plant dye material, adding it into distilled water, and performing extraction treatment, after the extraction treatment is completed, performing solid-liquid separation to obtain the plant dye solution; Step 2: Dyeing and fixing of cotton fabrics with plant dyes placing the cotton fabric in the plant dye solution for dyeing, and taking out the dyed cotton fabric after the dyeing is completed; Adding a composite enzyme color-fixing agent to the plant dyeing solution of the dyed cotton fabric, mixing and dissolving, and obtaining a plant dyeing solution containing the composite enzyme color-fixing agent; The dyed cotton fabric is placed in a plant dye solution containing a composite enzyme color-fixing agent to perform a color-fixing treatment. After the color-fixing treatment is completed, the fabric is taken out, washed with water, and dried to obtain the dyed and color-fixed cotton fabric.

2. The color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 1, characterized in that: In the step 1, the plant dyes include hematoxylin, madder, sophora japonica, gardenia, turmeric, and lithospermum.

3. The color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 1, characterized in that: In the step 1, the mass volume of the plant dye and distilled water is 20-300 g / L, and the extraction treatment condition is to extract at a temperature of 80-100° C. for 20-60 min.

4. The color fixing method for cotton fabric dyed with plant dye liquor based on composite enzyme catalysis according to claim 1, characterized in that: In the step 2, the bath ratio of the cotton fabric to the plant dye solution is 1:(20-50).

5. The color fixing method of cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 1, characterized in that: In the step 2, the dyeing treatment condition is dyeing at a temperature of 30-100° C. for 20-60 minutes.

6. The color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 1, characterized in that: In the step 2, the mass volume of the complex enzyme fixing agent and the plant dye solution is 1-5 g / L.

7. The color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 1, characterized in that: In the step 2, the complex enzyme color fixing agent is a complex of laccase, tetramethylpiperidinium nitrogen oxide and citric acid.

8. The color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 7, characterized in that: In the composite enzyme color-fixing agent, the mass ratio of laccase, tetramethylpiperidinium nitrogen oxide and citric acid is 1:(1-1.5):(0.05-0.25).

9. The color fixing method for cotton fabric dyed with plant dye solution based on composite enzyme catalysis according to claim 1, characterized in that: In the step 2, the color fixing treatment is carried out at a temperature of 30-90° C. for 0.5-4 hours.

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