Yellow Lyocell fabric prepared by dyeing with plant dye and sweet osmanthus and preparation method thereof
阅读说明：本技术 植物染料桂花染色制得的黄色莱赛尔面料及其制备方法 (Yellow Lyocell fabric prepared by dyeing with plant dye and sweet osmanthus and preparation method thereof ) 是由 周凡雨 彭雄义 邓健 董雄伟 李强 蔡亚军 刘仰硕 蔡映杰 于 2020-10-13 设计创作，主要内容包括：本发明涉及植物染料桂花染色制得的黄色莱赛尔面料及其染色方法。通过水蒸汽蒸馏从桂花中提取黄色植物染料原液,然后再将原液中黄色色素接枝1-氨基-2-硫酸酯乙基砜乙烷,制得黄色植物染料改性液；最后,将莱赛尔面料在黄色植物染料改性液中进行染色,制得黄色莱赛尔面料。本发明使反应活性低的桂花中的黄色色素变成具有高反应活性天然染料,此外,染色过程不需要加其它媒染剂和促染剂等染料助剂,简化了染色流程,节约了成本,同时减少了染色造成的环境污染；本发明染色后的黄色莱赛尔面料具有较高的K/S值,耐皂洗变色牢度和耐干摩擦色牢度均较高。(The invention relates to a yellow lyocell fabric prepared by dyeing with a plant dye, namely osmanthus fragrans, and a dyeing method thereof. Extracting yellow plant dye stock solution from sweet osmanthus through steam distillation, and grafting 1-amino-2-sulfate ethyl sulfone ethane to yellow pigment in the stock solution to prepare yellow plant dye modified solution; and finally, dyeing the lyocell fabric in a yellow plant dye modification solution to obtain the yellow lyocell fabric. The invention changes yellow pigment in the sweet osmanthus with low reaction activity into natural dye with high reaction activity, in addition, dye auxiliaries such as other mordants, accelerating agents and the like are not needed in the dyeing process, the dyeing process is simplified, the cost is saved, and meanwhile, the environmental pollution caused by dyeing is reduced; the dyed yellow lyocell fabric has higher K/S value, higher soaping color change fastness and dry friction color fastness.)
1. The preparation method of the yellow lyocell fabric prepared by dyeing with the plant dye osmanthus fragrans is characterized by comprising the following steps:
(1) preparation of a dyeing solution: diluting the modified yellow plant dye solution with water to prepare a dyeing solution, wherein the amount of the water is 10-20 times that of the modified yellow plant dye solution, and regulating the pH value of the dyeing solution to 10-11 by using 30wt% NaOH alkali liquor;
(2) dyeing: putting the lyocell fabric and dyeing liquid into a dyeing machine for dyeing, wherein the bath ratio is 1: 20-30, the dyeing time is 30-50 minutes, the dyeing temperature is 50-60 ℃, and taking out the lyocell fabric after dyeing is finished;
(3) and (3) post-treatment: and (3) washing the dyed lyocell fabric obtained in the step (2) with cold water, soap boiling, water washing and drying to obtain a yellow lyocell fabric.
2. The preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus according to claim 1, wherein the preparation method of the modified yellow plant dye solution in the step (1) comprises the following steps: adding 5wt% of formaldehyde aqueous solution and 1-amino-2-sulfuric ester ethyl sulfone ethane into yellow plant dye stock solution, adjusting the pH of the reaction solution to 10-11 by using 30wt% of NaOH alkali solution, continuously stirring, reacting for 80-100 minutes, and reacting at the temperature of 80-90 ℃ to obtain the modified yellow plant dye solution.
3. The preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus flower according to claim 2, wherein the preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring 2-chloroethanol and chlorosulfonic acid in a three-neck flask for reaction for 1-3 hours at the temperature of 50-60 ℃; after the reaction is finished, cooling and crystallizing the reacted solution, wherein the cooling temperature is-5-0 ℃, and crystallizing the product to obtain 2-chloroethanol sulfate; the ratio of the 2-chloroethanol to the chlorosulfonic acid is 1mL to (1-2) mL;
step 002, preparation of 1-amino-2-sulfate ethyl thioether ethane: dissolving 2-chloroethanol sulfate and 2-aminoethanethiol in 10wt% sodium hydroxide aqueous solution, and reacting at room temperature for 1-3 hours to obtain reaction liquid containing 1-amino-2-sulfuric ester ethyl thioether ethane; the proportion of the 2-chloroethanol sulfate, the 2-aminoethanethiol and the 10wt% sodium hydroxide aqueous solution is 1g to (1-1.2) g to (20-40) mL;
step 003, preparation of 1-amino-2-sulfate ethyl sulfone ethane: at room temperature, dropwise adding 30wt% of aqueous hydrogen peroxide solution into the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, wherein the dropwise adding time is 30-60 minutes, reacting for 1-3 hours after the dropwise adding is completed, and distilling under reduced pressure after the reaction is completed to prepare 1-amino-2-sulfuric ester ethyl sulfone ethane; the ratio of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane to 30wt% of hydrogen peroxide water solution is 1mL to (0.1-0.3) mL.
4. The preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus flower is characterized in that the dosage ratio of the 1-amino-2-sulfate ethyl sulfone ethane (g), 5wt% formaldehyde water solution (mL) to yellow plant dye stock solution (mL) is as follows: 1: 4-6: 400-600.
5. The preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus according to claim 2, wherein the preparation method of the yellow plant dye stock solution comprises the following steps: cleaning and mashing sweet osmanthus, distilling with steam at 200-260 ℃ for 100-150 min, and collecting filtrate after distillation to obtain yellow vegetable dye stock solution.
6. The preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus flower is characterized in that the dosage ratio of the osmanthus flower (g) to the water vapor (mL/min) is as follows: 1: 10-20.
7. The preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus according to claim 1, wherein the soaping condition in the step (3) is as follows: 1-3 g/L of soap flakes, 1-3 g/L of sodium carbonate, 65 ℃, 15min and a bath ratio of 1: 30-50.
8. The yellow lyocell fabric dyed by the plant dye osmanthus is characterized by being prepared by the preparation method of the yellow lyocell fabric dyed by the plant dye osmanthus according to any one of claims 1 to 7.
Technical Field
The invention belongs to the technical field of fabric preparation, and particularly relates to a yellow lyocell fabric prepared by dyeing with a plant dye, namely osmanthus fragrans, and a preparation method of the yellow lyocell fabric.
Background
From the moment of the generation of human society, human beings have been aware of various colors obtained from plants of nature to decorate their own clothes. They squeeze juice from weeds or branches and use the obtained colors for dyeing or drawing other patterns, but due to the influence of weather, the change of seasons and the difference of plant dyeing methods, the obtained colors are more different and different, and the colors are more like natural to give the incredible interest to the plant dyes of our.
Before the 19 th century, most of dyes for textile printing and dyeing are plant dyes, and after the 19 th century, synthetic dyes gradually replace the plant dyes in the printing and dyeing field due to the characteristics of colorful colors, complete chromatograms, good dyeing fastness, low price and the like. The large and small dye houses begin to use chemical dyes to dye fabrics, and only in remote minority areas, plant dyes are continuously used for dyeing, and slowly quit the historical stage. In recent years, with the enhancement of environmental protection, health and ecological consciousness, the dyeing concept of health and environmental protection returns to the visual field of people again, and the development of application type plant dyes has become a hot research direction in the world. In the textile printing and dyeing industry, in the research process of plant dye extraction and dyeing process, most plant dyes are widely applied in the fields of high-grade textile fabrics, clothing articles and the like because of the advantages of innocuity, no anaphylaxis and no carcinogenicity of most plant dyes and the biodegradability of printing and dyeing wastewater after the plant dyes are dyed and the compatibility with the environment.
The natural plant dye is mainly derived from the roots, stems, leaves and other parts of plants, the pigment of the natural plant dye can be naturally degraded generally, most of the natural plant dye has no toxicity or other side effects and is harmless to the environment, and various advantages of the natural plant dye make the natural plant dye gradually become the key point of novel dye development. The history of plant dye dyeing can be traced back to the yellow emperor period in ancient times, and people know that the juice of plants is used for dyeing dressed clothes so as to achieve the effect of improving the appearance.
Osmanthus fragrans is a commonly known name of a plurality of Chinese lutes, represents a species of Olea, also called cinnamomum japonicum, is evergreen shrub or arborescent in the family of Oleaceae, is thin in hard mass and skin, long and elliptical in leaf, sharp in end, opposite and not withered in winter. The peanut leaves have large gardening varieties, and the most representative ones are Jingui, Yingui, Dangui and laurel, etc. The species of osmanthus fragrans is yellow and has good potential for yellow plant dyes. However, the yellow pigment of osmanthus has low color fastness, especially low color fastness to washing and weather when applied to natural dyes. Aiming at the limitation of the application of the yellow pigment of the cinnamomum japonicum in natural dyes, the performance of the yellow pigment needs to be further improved.
The lyocell fiber is a novel regenerated cellulose fiber produced by a solvent method, wherein the lyocell fiber prepared by taking an N-methylmorpholine-N-oxide aqueous solution as a solvent is the only variety industrially produced at present. The lyocell fiber has many advantages in the aspects of raw materials, production flow, product quality, environmental friendliness and the like, so that the lyocell fiber is commonly concerned by various countries in the industry. Lyocell fibres have a number of advantages, such as: good drapability, high strength, easy dyeing, thick hand feeling, simple production process, renewable raw material sources, no environmental pollution in the production process and the like. Lyocell fabric is a fabric woven by lyocell fibers, and currently, the fabric is mainly dyed by chemically synthesized dyes. Literature research and market research find that lyocell fabric dyed by natural dye is only reported and needs to be further developed.
Disclosure of Invention
The chemically synthesized dye has strong reactivity, is combined with the lyocell fabric through chemical bonds, is relatively stable in yellow pigment of the osmanthus fragrans as the plant dye without chemical modification, is poor in reactivity, is relatively weak in binding force with the lyocell fabric, and is low in dyeing fastness, washing resistance and weather fastness of the yellow pigment dyed by the osmanthus fragrans without chemical modification. The invention aims to overcome the defects of the prior art and provides yellow lyocell fabric prepared by dyeing with plant dye osmanthus fragrans and a preparation method thereof.
The invention aims to provide a blue lyocell fabric for dyeing plant dye hyacinth, which has high K/S value, soaping-resistant color-changing fastness level and dry-rubbing-resistant color fastness level and has good application prospect.
The invention aims to provide a yellow lyocell fabric prepared by dyeing with a plant dye, namely osmanthus fragrans, and the fabric can be prepared by the following preparation method: extracting yellow plant dye stock solution from sweet osmanthus through steam distillation, and grafting 1-amino-2-sulfate ethyl sulfone ethane to the extract; preparing yellow plant dye modified liquid; and finally, dyeing the lyocell fabric in yellow plant dye modified liquid.
The invention also aims to provide a preparation method of the yellow lyocell fabric prepared by dyeing with the plant dye osmanthus fragrans, which comprises the following steps:
(1) preparing a yellow plant dye stock solution: cleaning and mashing sweet osmanthus, distilling with steam at 200-260 ℃ for 100-150 min, and collecting filtrate after distillation to obtain yellow vegetable dye stock solution.
Preferably, the dosage ratio of the sweet osmanthus flower (g) to the water vapor (mL/min) is as follows: 1: 10-20.
(2) Chemical modification: adding 5wt% of formaldehyde aqueous solution and 1-amino-2-sulfuric ester ethyl sulfone ethane into the yellow plant dye stock solution prepared in the step (1), adjusting the pH of the reaction solution to 10-11 by using 30wt% of NaOH alkali solution, continuously stirring, reacting for 80-100 minutes, and reacting at the temperature of 80-90 ℃ to obtain the modified yellow plant dye solution.
Preferably, the dosage ratio of the 1-amino-2-sulfate ethyl sulfone ethane (g), 5wt% formaldehyde aqueous solution (mL) and yellow plant dye stock solution (mL) is as follows: 1: 4-6: 400-600.
Preferably, the preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring 2-chloroethanol and chlorosulfonic acid in a three-neck flask for reaction for 1-3 hours at the temperature of 50-60 ℃; after the reaction is finished, cooling and crystallizing the reacted solution, wherein the cooling temperature is-5-0 ℃, and crystallizing the product to obtain 2-chloroethanol sulfate; the ratio of the 2-chloroethanol to the chlorosulfonic acid is 1mL to (1-2) mL; the main chemical reaction equations involved in this step are shown below.
Step 002, preparation of 1-amino-2-sulfate ethyl thioether ethane: dissolving 2-chloroethanol sulfate and 2-aminoethanethiol in 10wt% sodium hydroxide aqueous solution, and reacting at room temperature for 1-3 hours to obtain reaction liquid containing 1-amino-2-sulfuric ester ethyl thioether ethane; the proportion of the 2-chloroethanol sulfate, the 2-aminoethanethiol and the 10wt% sodium hydroxide aqueous solution is 1g to (1-1.2) g to (20-40) mL; the main chemical reaction equations involved in this step are shown below.
Step 003, preparation of 1-amino-2-sulfate ethyl sulfone ethane: at room temperature, dropwise adding 30wt% of aqueous hydrogen peroxide solution into the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, wherein the dropwise adding time is 30-60 minutes, reacting for 1-3 hours after the dropwise adding is completed, and distilling under reduced pressure after the reaction is completed to prepare 1-amino-2-sulfuric ester ethyl sulfone ethane; the ratio of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane to 30wt% of aqueous hydrogen peroxide solution is 1mL to (0.1-0.3) mL; the main chemical reaction equations involved in this step are shown below.
The chemical reaction equation involved in the step (2) is as follows, wherein R-C6H4OH represents the molecular structure of yellow pigment in the yellow plant dye stock solution.
(3) Dyeing: diluting the modified yellow plant dye solution obtained in the step (2) with water to obtain a dyeing solution, wherein the amount of the water is 10-20 times that of the modified yellow plant dye solution, and regulating the pH value of the dyeing solution to 10-11 by using 30wt% of NaOH alkali liquor; and (3) putting the Lyocell fabric and dyeing liquid into a dyeing machine for dyeing, wherein the bath ratio is 1 to (20-30), the dyeing time is 30-50 minutes, the dyeing temperature is 50-60 ℃, and the Lyocell fabric is taken out after dyeing is finished.
(4) Post-treatment of the lyocell fabric: and (4) washing the dyed lyocell fabric obtained in the step (3) with cold water, soap boiling, water washing and drying to obtain a yellow lyocell fabric.
Preferably, the soaping conditions are: 1-3 g/L of soap flakes, 1-3 g/L of sodium carbonate, 65 ℃, 15min and a bath ratio of 1: 30-50.
The chemical modification and dyeing mechanism analysis of the invention:
the molecular structure of the yellow pigment extracted from the osmanthus fragrans contains a large number of phenolic hydroxyl groups, and active hydrogen atoms at the ortho-position of the phenolic hydroxyl groups are easy to perform condensation reaction, so that 1-amino-2-sulfate ethyl sulfone ethane is introduced at the ortho-position of the phenolic hydroxyl groups.
The chemically modified yellow pigment molecule contains beta-ethyl sulfone sulfate which is a characteristic group of the reactive dye, which is equivalent to modifying the yellow pigment extracted from the sweet osmanthus into the reactive dye; the lyocell fabric mainly comprises cellulose, and the dyeing of the cellulose fiber is mainly realized by adopting reactive dye. Therefore, the chemically modified yellow pigment can be well chemically reacted with the lyocell fabric, so that the two are firmly combined.
The invention has the following remarkable advantages:
(1) through chemical modification, a characteristic group beta-ethyl sulfone sulfate of an active dye is grafted on yellow pigment molecules in the osmanthus fragrans, and the active dye is converted into a vinyl sulfone group in an alkaline medium to have high reactivity and form stable covalent bond combination with cellulose fibers; thereby changing yellow pigment in the sweet osmanthus with low reaction activity into natural dye with high reaction activity.
(2) Aiming at the problem that a large amount of printing and dyeing auxiliary agents are needed in the dyeing process of the synthetic dye, in the dyeing process of the invention, because the affinity between the yellow pigment molecules in the modified sweet osmanthus and the fabric is better, the yellow pigment molecules are easy to be close to the surface of the fabric, so that other dye auxiliary agents such as mordants, accelerating agents and the like are not needed to be added, the dyeing process is simplified, the cost is saved, and the environmental pollution caused by dyeing is reduced.
(3) Aiming at the problem of high extraction difficulty of the yellow pigment in the sweet osmanthus, the invention adopts a steam distillation method to extract the yellow pigment in the sweet osmanthus, and the extraction method has the characteristics of simplicity, practicability, high efficiency and the like.
(4) Aiming at the problem that the synthetic route of the modifier 1-amino-2-sulfate ethyl sulfone ethane is complex, the invention obtains a simple synthetic route by refining a synthetic scheme.
(5) The dyed yellow lyocell fabric has higher K/S value, higher soaping color change fastness and dry friction color fastness.
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
The preparation method of the yellow lyocell fabric prepared by dyeing with the plant dye osmanthus fragrans comprises the following steps:
(1) preparing a yellow plant dye stock solution: cleaning and mashing 10g of sweet osmanthus, distilling with steam at 240 ℃ for 120 min, wherein the amount of the steam is 150mL/min, and collecting filtrate after distillation to obtain yellow plant dye stock solution.
(2) Chemical modification: adding 1.5mL of 5wt% formaldehyde aqueous solution and 0.3g of 1-amino-2-sulfuric ester ethyl sulfone ethane into 150mL of the yellow plant dye stock solution prepared in the step (1), adjusting the pH of the reaction solution to 10.5 by using 30wt% NaOH alkali liquor, continuously stirring, reacting for 90 minutes at 85 ℃, and preparing the modified yellow plant dye solution.
(3) Dyeing: diluting the modified yellow plant dye solution obtained in the step (2) with water to prepare a dyeing solution, wherein the amount of the water is 15 times that of the modified yellow plant dye solution, and regulating the pH value of the dyeing solution to 10.5 by using 30wt% of NaOH alkali liquor; placing the lyocell fabric and the dyeing liquid into a dyeing machine for dyeing; the bath ratio is 1: 25, the dyeing time is 40 minutes, the dyeing temperature is 55 ℃, and the lyocell fabric is taken out after dyeing is finished.
The preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring 10mL of 2-chloroethanol and 15mL of chlorosulfonic acid in a three-neck flask for reaction, wherein the reaction time is 2 hours and the reaction temperature is 55 ℃; after the reaction is finished, cooling and crystallizing the reacted solution at-3 ℃ to obtain a crystallized product, namely 2-chloroethanol sulfate;
step 002, preparation of 1-amino-2-sulfate ethyl thioether ethane: dissolving 5g of 2-chloroethanol sulfate and 5g of 2-aminoethanethiol in 150mL of 10wt% sodium hydroxide aqueous solution, and reacting at room temperature for 2 hours to obtain a reaction solution containing 1-amino-2-sulfate ethyl thioether ethane;
step 003, preparation of 1-amino-2-sulfate ethyl sulfone ethane: at room temperature, 2mL of 30wt% aqueous hydrogen peroxide solution is dropwise added into 10mL of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, the dropwise adding time is 5 minutes, the reaction is carried out for 2 hours after the dropwise adding is finished, and reduced pressure distillation is carried out after the reaction is finished, so as to prepare the 1-amino-2-sulfuric ester ethyl sulfone ethane.
(4) Post-treatment of the lyocell fabric: washing the dyed lyocell fabric obtained in the step (3) with cold water, soap boiling, water washing and drying to obtain a yellow lyocell fabric; the soap boiling conditions are as follows: 2g/L of soap flakes, 2g/L of sodium carbonate, 65 ℃, 15min and a bath ratio of 1: 40.
Example 2
The preparation method of the yellow lyocell fabric prepared by dyeing with the plant dye osmanthus fragrans comprises the following steps:
(1) preparing a yellow plant dye stock solution: cleaning and mashing 10g of sweet osmanthus, distilling with steam at 240 ℃ for 120 min, wherein the amount of the steam is 150mL/min, and collecting filtrate after distillation to obtain yellow plant dye stock solution.
(2) Chemical modification: adding 1.5mL of 5wt% formaldehyde aqueous solution and 0.375g of 1-amino-2-sulfuric ester ethyl sulfone ethane into 150mL of the yellow plant dye stock solution prepared in the step (1), adjusting the pH of the reaction solution to 10.3 by using 30wt% NaOH alkali liquor, continuously stirring, reacting for 80 minutes at the reaction temperature of 80 ℃, and preparing the modified yellow plant dye solution.
(3) Dyeing: diluting the modified yellow plant dye solution obtained in the step (2) with water to prepare a dyeing solution, wherein the amount of the water is 15 times that of the modified yellow plant dye solution, and regulating the pH value of the dyeing solution to 10.3 by using 30wt% of NaOH alkali liquor; and putting the lyocell fabric and the dyeing liquid into a dyeing machine for dyeing, wherein the bath ratio is 1: 20, the dyeing time is 40 minutes, the dyeing temperature is 50 ℃, and the lyocell fabric is taken out after dyeing is finished.
The preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring 10mL of 2-chloroethanol and 15mL of chlorosulfonic acid in a three-neck flask for reaction, wherein the reaction time is 2 hours and the reaction temperature is 55 ℃; after the reaction is finished, cooling and crystallizing the reacted solution at-3 ℃ to obtain a crystallized product, namely 2-chloroethanol sulfate;
step 002, preparation of 1-amino-2-sulfate ethyl thioether ethane: dissolving 5g of 2-chloroethanol sulfate and 5g of 2-aminoethanethiol in 150mL of 10wt% sodium hydroxide aqueous solution, and reacting at room temperature for 2 hours to obtain a reaction solution containing 1-amino-2-sulfate ethyl thioether ethane;
step 003, preparation of 1-amino-2-sulfate ethyl sulfone ethane: at room temperature, 2mL of 30wt% aqueous hydrogen peroxide solution is dropwise added into 10mL of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, the dropwise adding time is 5 minutes, the reaction is carried out for 2 hours after the dropwise adding is finished, and reduced pressure distillation is carried out after the reaction is finished, so as to prepare the 1-amino-2-sulfuric ester ethyl sulfone ethane.
(4) Post-treatment of the lyocell fabric: washing the dyed lyocell fabric obtained in the step (3) with cold water, soap boiling, water washing and drying to obtain a yellow lyocell fabric; the soap boiling conditions are as follows: soap flakes 1g/L, soda 1g/L, 65 deg.C, 15min, bath ratio 1: 30.
Example 3
The preparation method of the yellow lyocell fabric prepared by dyeing with the plant dye osmanthus fragrans comprises the following steps:
(1) preparing a yellow plant dye stock solution: cleaning and mashing 10g of sweet osmanthus, distilling with steam at 240 ℃ for 120 min, wherein the amount of the steam is 150mL/min, and collecting filtrate after distillation to obtain yellow plant dye stock solution.
(2) Chemical modification: adding 1.5mL of 5wt% formaldehyde aqueous solution and 0.25g of 1-amino-2-sulfuric ester ethyl sulfone ethane into 150mL of the yellow plant dye stock solution prepared in the step (1), adjusting the pH of the reaction solution to 10.8 by using 30wt% NaOH alkali liquor, continuously stirring, reacting for 100 minutes at the reaction temperature of 90 ℃, and preparing the modified yellow plant dye solution.
(3) Dyeing: diluting the modified yellow plant dye solution obtained in the step (2) with water to prepare a dyeing solution, wherein the amount of the water is 15 times that of the modified yellow plant dye solution, and regulating the pH value of the dyeing solution to 10.8 by using 30wt% of NaOH alkali liquor; and putting the lyocell fabric and the dyeing liquid into a dyeing machine for dyeing, wherein the bath ratio is 1: 30, the dyeing time is 40 minutes, the dyeing temperature is 60 ℃, and the lyocell fabric is taken out after dyeing is finished.
The preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring 10mL of 2-chloroethanol and 15mL of chlorosulfonic acid in a three-neck flask for reaction, wherein the reaction time is 2 hours and the reaction temperature is 55 ℃; after the reaction is finished, cooling and crystallizing the reacted solution at-3 ℃ to obtain a crystallized product, namely 2-chloroethanol sulfate;
step 002, preparation of 1-amino-2-sulfate ethyl thioether ethane: dissolving 5g of 2-chloroethanol sulfate and 5g of 2-aminoethanethiol in 150mL of 10wt% sodium hydroxide aqueous solution, and reacting at room temperature for 2 hours to obtain a reaction solution containing 1-amino-2-sulfate ethyl thioether ethane;
step 003, preparation of 1-amino-2-sulfate ethyl sulfone ethane: at room temperature, 2mL of 30wt% aqueous hydrogen peroxide solution is dropwise added into 10mL of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, the dropwise adding time is 5 minutes, the reaction is carried out for 2 hours after the dropwise adding is finished, and reduced pressure distillation is carried out after the reaction is finished, so as to prepare the 1-amino-2-sulfuric ester ethyl sulfone ethane.
(4) Post-treatment of the lyocell fabric: washing the dyed lyocell fabric obtained in the step (3) with cold water, soap boiling, water washing and drying to obtain a yellow lyocell fabric; the soap boiling conditions are as follows: 3g/L of soap flakes, 3g/L of soda ash, 65 ℃, 15min and a bath ratio of 1: 50.
Comparative example 1
In this comparative example, 1-amino-2-sulfate ethylsulfone ethane was not prepared and the crude yellow vegetable dye solution was used for dyeing, and the other preparation method was carried out in the same manner as in example 1.
Comparative example 2
In this comparative example, the dyeing process was changed and the other preparation was carried out as in example 1, with example 1 as a comparison, the dyeing process after the change being:
diluting the modified yellow plant dye solution with water to prepare a dyeing solution, wherein the amount of the water is 15 times of that of the modified yellow plant dye solution, and regulating the pH value of the dyeing solution to be 10.5 by using 30wt% NaOH alkali liquor; and putting the lyocell fabric and dyeing liquor into a dyeing machine for dyeing, wherein the bath ratio is 1: 25, dyeing is carried out for 15min at 60 ℃, then sodium chloride is added, dyeing is carried out for 15min at 60 ℃, soda is added after the temperature is raised to 90 ℃, color fixing is carried out for 30min at 90 ℃, wherein the concentration of sodium chloride is 40 g/L, the concentration of soda is 10 g/L, and the lyocell fabric is taken out after dyeing is finished.
Comparative example 3
In this comparative example, reactive dye reactive yellow 145 on the market was purchased, and the dyeing method employed a conventional dyeing method. The preparation method of the yellow lyocell fabric dyed by the reactive dye reactive yellow 145 comprises the following steps:
selecting a Lyocell fabric and reactive dye reactive yellow 145, dyeing the Lyocell fabric and the reactive dye reactive yellow 145 by a conventional method, adding salt after dyeing for 15min at 60 ℃, continuing dyeing for 15min at 60 ℃, heating to 90 ℃, adding soda ash, fixing color for 30min at 90 ℃, wherein the experimental formula is as follows: the using amount of the reactive dye reactive yellow 145 is 2 percent (owf), the salt is 40 g/L, the soda is 10 g/L, and the bath ratio is 1: 50; and cooling after dyeing is finished, taking out a sample, washing with cold water, soap boiling (1.5 g/L of soap flakes and 1.5g/L of soda at 55 ℃, 15min, bath ratio of 1: 30), washing with water, and drying to obtain the yellow lyocell fabric.
Performance evaluation:
the yellow lyocell fabrics obtained in the above examples 1 to 3 and comparative examples 1 to 3 were subjected to performance evaluation. The K/S value is measured by adopting a color measuring and matching instrument SF600X of DataColor company in America; the soaping-resistant color change fastness value test refers to GB/T3921-2008 'textile color fastness test soaping-resistant color fastness'; the dry rubbing resistance color fastness value test refers to GB/T3920-2008 'textile color fastness test rubbing color fastness', and specific data are shown in Table 1.
TABLE 1
K/S value
Fastness to soaping change/grade
Color fastness to dry rubbing/grade
Example 1
14.48
4-5
5
Example 2
14.23
5
5
Example 3
14.79
5
4-5
Comparative example 1
7.37
3
3
Comparative example 2
11.81
4
4-5
Comparative example 3
11.65
4-5
4-5
As can be seen from Table 1, the K/S values, the soaping discoloration resistance fastnesses and the dry rubbing fastness of examples 1 to 3 were all better than those of comparative examples 1 to 3.