CN112482052B - Green Lyocell fabric prepared by dyeing with plant dye rosemary and preparation method thereof - Google Patents
Green Lyocell fabric prepared by dyeing with plant dye rosemary and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/02—Preparation of sulfones; Preparation of sulfoxides by formation of sulfone or sulfoxide groups by oxidation of sulfides, or by formation of sulfone groups by oxidation of sulfoxides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/04—Preparation of sulfones; Preparation of sulfoxides by reactions not involving the formation of sulfone or sulfoxide groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B57/00—Other synthetic dyes of known constitution
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
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- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
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- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/10—After-treatment with compounds containing metal
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- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention relates to a green Lyocell fabric prepared by dyeing a plant dye rosemary and a preparation method thereof. The invention extracts green plant dye stock solution and green toner precipitate from rosemary leaves by ethanol-water mixed solution distillation, and then grafts 1-amino-2-sulfate ethyl sulfone ethane to the extract to prepare modified green plant dye powder; and finally, dyeing the lyocell fabric in the modified green plant dye to obtain the green lyocell fabric. The invention changes the green pigment in the rosemary leaves with low reactivity into natural dye with high reactivity, 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 green lyocell fabric has a high K/S value, and has high soaping color change fastness and dry friction color fastness.
Description
Technical Field
The invention belongs to the technical field of fabric preparation, and particularly relates to a green Lyocell fabric prepared by dyeing with a vegetable dye rosemary and a preparation method thereof.
Background
Natural dyes generally refer to dyes that have not been synthesized, have been chemically processed to a very small extent, and are generally obtained from animal or plant sources or from mineral sources. Since 1856, aniline violet appears, and the synthetic dye rapidly occupies the market and replaces the natural dye due to the advantages of rich color, high dyeing efficiency, complete chromatogram, low price and the like. However, synthetic dyes are increasingly problematic in production and use, for example, water pollution, soil pollution, air quality deterioration, and generation of carcinogenic substances, which are serious concerns. The natural dye prepared from nature is not only green and environment-friendly, non-toxic and biodegradable, but also has the functions of disinsection and antibiosis, good health care performance and the like, and is a popular research object in the modern times. The natural dyes can be classified into four types, namely plant dyes, animal dyes, microbial dyes and mineral dyes according to the acquisition source. The vegetable dye not only enables the dyed fabric to have bright and natural color, but also has the effects of antibiosis, antiphlogosis and the like. The plant dye is obtained by extracting pigment from natural flowers, grasses, trees, stems, leaves, fruits, seeds, barks and roots. The utilization of plant dyes is the mainstream of ancient dyeing technology in China.
There are two main types of chlorophyll in higher plants: chlorophyll a, b, chlorophyll a being typically blue-green in color, while chlorophyll b is yellow-green, chlorophyll b being a locally oxidized derivative of chlorophyll a. Chlorophyll a is three times as chlorophyll b, the molecular structure of chlorophyll is known in the 30's of the twentieth century, and in the later 50's, chlorophyll a is artificially synthesized, and other pigments are almost simultaneously found. The carotenoid in chloroplast mainly comprises two kinds of carotene and lutein, wherein the carotenoid is orange yellow, and the lutein is yellow. Lutein is twice as much as carotene. Plant chlorophyll is typically three to four times as much as carotenoids; the two main classes of four pigments are insoluble in water and soluble in organic solvents such as ethanol, acetone, etc. Chemically, chlorophyll is an ester of chlorophyllin, which is saponified in the ester linkage under the action of alkali to give a salt of chlorophyllin, which is soluble in water but remains green as it retains the Mg core structure.
Rosemary is a rare natural spice plant, can emit a faint scent in growing seasons, and has the effects of clearing away the heart-fire and refreshing. Its stem, leaf and flower have pleasant fragrance, and the aromatic oil extracted from flower and twig can be used for preparing cosmetic raw materials such as air cleaner, perfume, soap, etc., and the best-known cosmetic water is made of rosemary, and can be used in beverage, skin care oil, pilatory, and washing cream.
The leaves of rosemary contain a large amount of chlorophyll, and the leaves are green, and in addition, the main ingredients in the leaves can be used as the main raw material of astringent. From this it can be analyzed that the leaves of rosemary have a good potential for natural dyes. However, when the green pigment in rosemary leaves is applied to natural dyes, the color fastness is low, and particularly, the color fastness to washing and weather is low. Aiming at the defects of the application of the rosemary leaves in natural dyes, the performance of the rosemary leaves needs to be further improved.
Lyocell is one of the regenerated cellulose fibers. The fiber takes wood pulp of plant source as raw material, is made into cellulose fiber by a solvent spinning method, and is woven into textile so as to enter the consumer market, the product can be completely decomposed in soil, the amine oxide solvent used in the production is nontoxic, pollution-free and recyclable, the whole fiber production flow is environment-friendly, and the solvent recovery rate can reach more than 99 percent, so the lyocell fiber is called as '21 st century green fiber'. In addition, lyocell is a new type of renewable cellulose fiber that has many 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. The lyocell fabric is a fabric woven by lyocell fibers, and currently, the fabric is mainly dyed by chemically synthesized dyes. The literature research and the market survey find that the lyocell fabric dyed by the natural dye is only reported and needs to be further developed.
Disclosure of Invention
The chemical synthetic dye has strong reactivity, is combined with the lyocell fabric through chemical bonds, is relatively stable in green pigment of rosemary which is a plant dye not subjected to chemical modification, is poor in reactivity, is relatively weak in binding force with the lyocell fabric, is low in dyeing fastness, and is low in washing resistance and weather fastness. The invention aims to overcome the defects of the prior art and provides a green Lyocell fabric prepared by dyeing with a plant dye rosemary and a preparation method thereof.
The invention aims to provide the green lyocell fabric prepared by the rosemary dyeing of the vegetable dye, the fabric has high K/S value, soaping-resistant color-changing fastness grade and dry-rubbing color fastness grade, and the fabric has good application prospect.
The invention aims to provide a green lyocell fabric prepared by dyeing a plant dye rosemary, and the fabric can be prepared by the following preparation method: distilling the mixed solution of ethanol and water to extract green plant dye stock solution and green toner precipitate from herba Rosmarini officinalis, and grafting the extract with 1-amino-2-sulfate ethyl sulfone ethane; preparing modified green plant dye powder; and finally, dyeing the lyocell fabric in the modified green plant dye.
The invention also aims to provide a preparation method of the green lyocell fabric prepared by dyeing the plant dye rosemary, wherein the preparation method comprises the following steps:
(1) Preparation of green plant dye stock solution and toner precipitate: weighing cleaned leaves of rosemary, mashing the leaves, and dissolving the leaves in a mixed solution of ethanol and water, wherein the material-liquid ratio of the leaves to the solution is 1g to (10-20) mL; heating at 50-60 deg.c for 6-8 hr, cooling the extracted liquid and filtering; heating the filtrate at 95-100 deg.c for 3-5 hr, eliminating alcohol solvent, filtering to obtain green plant dye liquid and green color precipitate.
Preferably, the volume fraction of ethanol in the ethanol-water mixed solution is 30-40%.
(2) Chemical modification: adding the green plant dye stock solution prepared in the step (1), a green toner precipitate, 5wt% of formaldehyde aqueous solution and 1-amino-2-sulfuric ester ethyl sulfone ethane into the aqueous solution, adjusting the pH of the reaction solution to 10-11 by using 30wt% of NaOH alkali liquor, continuously stirring, reacting for 30-60 minutes at 50-60 ℃, and spray drying after the reaction is finished to obtain the modified green plant dye powder.
Preferably, the ratio of the green plant dye stock solution, the green toner educt, the 1-amino-2-sulfuric ester ethyl sulfone ethane and the 5wt% formaldehyde water solution to the water is (10-20) mL: 1g, (0.1-0.3) g, (3-5) mL: 30-50) mL.
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 at the temperature of-5-0 ℃ to obtain 2-chloroethanol sulfate as a crystallization product; 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 finished, and distilling under reduced pressure after the reaction is finished to prepare 1-amino-2-sulfuric ester ethyl sulfone ethane; the proportion of the reaction liquid containing the 1-amino-2-sulfuric ester ethyl thioether ethane to the 30wt% 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-C 6 H 4 -OH represents the molecular structure of the green pigment.
(3) Dyeing: dissolving a proper amount of modified green plant dye in an aqueous solution to prepare a dyeing solution, and regulating the pH value of the dyeing solution to 10-11 by using 30wt% NaOH alkali liquor; and (2) putting the Lyocell fabric and the dyeing solution into a dyeing machine for dyeing, wherein the bath ratio is 1 to (20-30), the dyeing time is 60-80 minutes, the dyeing temperature is 70-80 ℃, and the Lyocell fabric is taken out after dyeing is finished.
Preferably, the ratio of the modified green plant dye (g) to water (mL) is 1: (50-60).
(4) And (3) post-treatment: and (4) washing the dyed lyocell fabric obtained in the step (3) with cold water, soap boiling, water washing and drying to obtain the green lyocell fabric.
Preferably, the soaping conditions are: 1g/L of soap flakes, 1g/L of soda ash, 65 ℃,15min and 1: 30 of bath ratio.
The chemical modification and dyeing mechanism analysis of the invention:
the molecular structure of the green pigment extracted from rosemary contains a large amount of phenolic hydroxyl, and active hydrogen atoms at the ortho-position of the phenolic hydroxyl are easy to generate condensation reaction, so that 1-amino-2-sulfate ethyl sulfone ethane is introduced at the ortho-position of the phenolic hydroxyl.
The chemically modified green pigment molecule contains beta-ethyl sulfone sulfate which is a characteristic group of the reactive dye, and the modification is equivalent to the modification of the green pigment extracted from rosemary 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 green 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 reactive dye characteristic group beta-ethyl sulfone sulfate is grafted on a green pigment molecule in the leaves of rosemary, and is converted into a vinyl sulfone group in an alkaline medium to have high reactivity and form stable covalent bond combination with cellulose fibers; so that the green pigment in the leaves of rosemary with low reactivity is changed into natural dye with high reactivity.
(2) Aiming at the problem that a large amount of printing and dyeing auxiliaries are needed in the dyeing process of the synthetic dye, in the dyeing process of the invention, because the affinity between the green pigment molecules in the modified rosemary leaves and the fabric is good, the green pigment molecules are easy to approach the surface of the fabric, so that dye auxiliaries such as other mordants, accelerating agents and the like are not needed, 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 difficulty in extracting the green pigment in the rosemary leaves, the invention adopts a method of dissolving the green pigment in the rosemary leaves by using an ethanol-water mixed solvent, 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 green lyocell fabric has higher K/S value, higher soaping color change fastness and dry rubbing color fastness.
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
The preparation method of the green lyocell fabric prepared by dyeing with the plant dye rosemary comprises the following steps:
(1) Preparation of green plant dye stock solution and toner precipitate: weighing 50g of cleaned leaves of rosemary, mashing the leaves, and dissolving the leaves in a mixed solution of ethanol and water containing 35% of ethanol, wherein the ratio of materials to liquid is 1: 15; heating at 55 deg.C for 7 hr, cooling the extractive solution, and filtering; heating the filtrate at 97 deg.C for 4 hr, removing ethanol solvent, and filtering to obtain green plant dye stock solution and green toner precipitate.
(2) Chemical modification: and (2) adding 15mL of the green plant dye stock solution prepared in the step (1), 1g of green toner precipitate, 4mL of a 5wt% aqueous solution of formaldehyde and 0.2g of 1-amino-2-sulfuric ester ethyl sulfone ethane into 40mL of an aqueous solution, adjusting the pH of the reaction solution to 10.7 by using 30wt% of NaOH alkaline solution, continuously stirring, reacting for 50 minutes at the reaction temperature of 55 ℃, and spray drying after the reaction is finished to obtain the modified green plant dye powder.
The preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring and reacting 10mL of 2-chloroethanol and 15mL of chlorosulfonic acid in a three-neck flask for 2 hours at the reaction temperature of 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 reaction liquid 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 added dropwise into 10mL of 1-amino-2-sulfate ethyl thioether ethane-containing reaction solution prepared in the step 002, the dropwise addition time is 5 minutes, the reaction is carried out for 2 hours after the dropwise addition is finished, and reduced pressure distillation is carried out after the reaction is finished, so as to prepare 1-amino-2-sulfate ethyl sulfone ethane.
(3) Dyeing: dissolving 2g of modified green plant dye in 110mL of aqueous solution to prepare a dyeing solution, and regulating the pH value of the dyeing solution to 10.3 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: 15, the dyeing time is 70 minutes, the dyeing temperature is 75 ℃, and the lyocell fabric is taken out after dyeing is finished.
(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 green lyocell fabric; the soap boiling conditions are as follows: 1g/L of soap flakes, 1g/L of soda ash, 65 ℃,15min and 1: 30 of bath ratio.
Example 2
The preparation method of the green lyocell fabric prepared by the rosemary dyeing through the vegetable dye comprises the following steps:
(1) Preparation of green plant dye stock solution and toner precipitate: weighing 50g of cleaned leaves of rosemary, mashing the leaves, and dissolving the leaves in a mixed solution of ethanol and water containing 30% of ethanol, wherein the ratio of materials to liquid is 1: 10; heating at 55 deg.C for 7 hr, cooling the extractive solution, and filtering; heating the filtrate at 97 deg.C for 4 hr, removing ethanol solvent, and filtering to obtain green plant dye stock solution and green toner precipitate.
(2) Chemical modification: and (2) adding 10mL of the green plant dye stock solution prepared in the step (1), 1g of green toner precipitate, 3mL of a 5wt% formaldehyde aqueous solution and 0.1g of 1-amino-2-sulfate ethyl sulfone ethane into 30mL of the aqueous solution, adjusting the pH of the reaction solution to 10.8 by using a 30wt% NaOH alkaline solution, continuously stirring, reacting for 50 minutes at the reaction temperature of 55 ℃, and spray drying after the reaction is finished to obtain the modified green plant dye powder.
The preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring and reacting 10mL of 2-chloroethanol and 15mL of chlorosulfonic acid in a three-neck flask for 2 hours at the reaction temperature of 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% aqueous solution of sodium hydroxide, and reacting at room temperature for 2 hours to prepare reaction liquid containing 1-amino-2-sulfuric ester 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 dripped into 10mL of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, the dripping time is 5 minutes, the reaction is carried out for 2 hours after the dripping is finished, and the reduced pressure distillation is carried out after the reaction is finished, so as to prepare the 1-amino-2-sulfuric ester ethyl sulfone ethane.
(3) Dyeing: dissolving 2g of modified green plant dye in 100mL of aqueous solution to prepare a dyeing 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: 10, the dyeing time is 70 minutes, the dyeing temperature is 75 ℃, and the lyocell fabric is taken out after dyeing is finished.
(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 green 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 green lyocell fabric prepared by dyeing with the plant dye rosemary comprises the following steps:
(1) Preparation of green plant dye stock solution and toner precipitate: weighing 50g of cleaned rosemary leaves, mashing the rosemary leaves and dissolving the mashed rosemary leaves in 40% ethanol-water mixed solution, wherein the material-liquid ratio is 1: 20; heating at 55 deg.C for 7 hr, cooling the extractive solution, and filtering; heating the filtrate at 97 deg.C for 4 hr, removing ethanol solvent, and filtering to obtain green plant dye stock solution and green toner precipitate.
(2) Chemical modification: and (2) adding 20mL of the green plant dye stock solution prepared in the step (1), 1g of green toner precipitate, 5mL of 5wt% aqueous formaldehyde solution and 0.3g of 1-amino-2-sulfuric ester ethyl sulfone ethane into 50mL of aqueous solution, adjusting the pH of the reaction solution to 10.5 by using 30wt% NaOH alkali solution, continuously stirring, reacting for 50 minutes at the reaction temperature of 55 ℃, and spray drying after the reaction is finished to obtain the modified green plant dye powder.
The preparation method of the 1-amino-2-sulfate ethyl sulfone ethane comprises the following steps:
step 001, preparation of 2-chloroethanol sulfate: stirring and reacting 10mL of 2-chloroethanol and 15mL of chlorosulfonic acid in a three-neck flask for 2 hours at the reaction temperature of 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% aqueous solution of sodium hydroxide, and reacting at room temperature for 2 hours to prepare reaction liquid containing 1-amino-2-sulfuric ester 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 dripped into 10mL of the reaction solution containing 1-amino-2-sulfuric ester ethyl thioether ethane prepared in the step 002, the dripping time is 5 minutes, the reaction is carried out for 2 hours after the dripping is finished, and the reduced pressure distillation is carried out after the reaction is finished, so as to prepare the 1-amino-2-sulfuric ester ethyl sulfone ethane.
(3) Dyeing: dissolving 2g of modified green plant dye in 120mL of aqueous solution to prepare a dyeing solution, and regulating the pH value of the dyeing solution to 10.7 by using 30wt% NaOH alkali liquor; placing the lyocell fabric and the dyeing liquid into a dyeing machine for dyeing; the bath ratio is 1: 20, the dyeing time is 70 minutes, the dyeing temperature is 75 ℃, and the lyocell fabric is taken out after dyeing is finished.
(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 green lyocell fabric; the soap boiling conditions are as follows: soap flakes 1g/L, soda 1g/L,65 deg.C, 15min, bath ratio 1: 30.
Comparative example 1
In this comparative example, 1-amino-2-sulfate ethylsulfone ethane was not prepared and the extracted green vegetable dye stock solution and the toner precipitate were directly dyed, and the other preparation methods were performed as in example 1, by way of comparison with 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:
dissolving 2g of modified green plant dye in 110mL to prepare a dyeing solution, and regulating the pH value of the dyeing solution to 10.3 by using 30wt% NaOH alkali liquor; placing the Lyocell fabric and a dyeing solution into a dyeing machine for dyeing, wherein the bath ratio is 1: 15, adding sodium chloride after dyeing for 15min at 60 ℃, continuing dyeing for 15min at 60 ℃, heating to 90 ℃, adding soda, and fixing color at 90 ℃ for 30min, wherein the concentration of the sodium chloride is 40 g/L, and the concentration of the soda is 10 g/L; and taking out the lyocell fabric after dyeing is finished.
Comparative example 3
In this comparative example, a conventional dyeing method and a reactive dye reactive green 19 purchased from the market were used. The preparation method of the green lyocell fabric dyed by the reactive dye reactive green 19 comprises the following steps:
selecting a Lyocell fabric and reactive dye reactive green 19, dyeing the Lyocell fabric by adopting a conventional dyeing method, adding salt after dyeing for 15min at 60 ℃, continuously dyeing for 15min at 60 ℃, adding soda ash after heating to 90 ℃, fixing color for 30min at 90 ℃, wherein the experimental prescription is as follows: the dosage of the reactive dye reactive green 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, boiling with soap (1 g/L of soap flakes and 1g/L of soda at 65 ℃ for 15min, wherein the bath ratio is 1: 30), washing with water, and drying to obtain the green lyocell fabric.
Performance evaluation:
the green lyocell fabrics obtained in examples 1 to 3 and comparative examples 1 to 3 were evaluated for their properties. The K/S value is measured by adopting an SF600X color measuring and matching instrument of the American DataColor company; the soaping-resistant color change fastness value test refers to GB/T3921-2008 'textile color fastness test soaping-resistant color fastness'; the dry rubbing fastness value test refers to GB/T3920-2008 'color fastness to rubbing' of textile color fastness test, and the 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 | 15.43 | 4-5 | 5 |
| Example 2 | 16.23 | 5 | 5 |
| Example 3 | 15.19 | 5 | 5 |
| Comparative example 1 | 10.44 | 3-4 | 3-4 |
| Comparative example 2 | 11.62 | 3 | 3-4 |
| Comparative example 3 | 10.32 | 4 | 4 |
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.
Claims (6)
1. The preparation method of the green lyocell fabric prepared by dyeing with the plant dye rosemary is characterized by comprising the following steps:
(1) Preparation of a dyeing solution: dissolving the modified green plant dye in an aqueous solution to prepare a dyeing 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 liquor into a dyeing machine for dyeing, wherein the bath ratio is 1: 20-30, the dyeing time is 60-80 minutes, the dyeing temperature is 70-80 ℃, and the lyocell fabric is taken out after dyeing is finished;
(3) And (3) post-treatment: washing the dyed lyocell fabric obtained in the step (2) with cold water, soap boiling, water washing and drying to obtain a green lyocell fabric;
wherein, the preparation method of the modified green plant dye in the step (1) comprises the following steps: adding green plant dye stock solution, green toner precipitate, 5wt% of formaldehyde aqueous solution and 1-amino-2-sulfuric ester ethyl sulfone ethane into the aqueous solution, adjusting the pH of the reaction solution to 10-11 by using 30wt% of NaOH alkali liquor, continuously stirring, reacting for 30-60 minutes at the reaction temperature of 50-60 ℃, and preparing modified green plant dye powder by adopting spray drying after the reaction is finished;
the preparation method of the green plant dye stock solution and the toner educt comprises the following steps: weighing cleaned rosemary leaves, mashing the rosemary leaves and dissolving the rosemary leaves in a mixed solution of ethanol and water, wherein the material-liquid ratio of the leaves to the solution is 1g to (10-20) mL; heating at 50-60 deg.c for 6-8 hr, cooling the extracted liquid and filtering; heating the filtrate at 95-100 ℃ for 3-5 hours, removing the ethanol solvent, and filtering to respectively prepare green plant dye stock solution and green toner educt;
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 50-60 ℃; after the reaction is finished, cooling and crystallizing the reacted solution at the temperature of-5-0 ℃ to obtain 2-chloroethanol sulfate as a crystallization product; 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 finished, and distilling under reduced pressure after the reaction is finished to prepare 1-amino-2-sulfuric ester ethyl sulfone ethane; the proportion of the reaction liquid containing the 1-amino-2-sulfuric ester ethyl thioether ethane to the 30wt% aqueous hydrogen peroxide solution is 1mL to (0.1-0.3) mL.
2. The method for preparing the green lyocell fabric dyed by the rosemary plant dye according to claim 1, wherein the ratio of the modified green plant dye to the water in the step (1) is 1g to (50-60) mL.
3. The method for preparing a green lyocell fabric dyed with rosemary as a vegetable dye according to claim 1, wherein the ratio of the raw liquid of the green vegetable dye, the precipitate of the green toner, 1-amino-2-sulfate ethyl sulfone ethane and 5wt% of formaldehyde aqueous solution to water is (10 to 20) mL: 1g, (0.1 to 0.3) g, (3 to 5) mL: 30 to 50 mL.
4. The method for preparing a green lyocell fabric dyed with rosemary as a plant dye of claim 1, wherein the volume fraction of ethanol in the ethanol-water mixed solution is 30-40%.
5. The method for preparing the green lyocell fabric dyed by the rosemary serving as the plant dye according to the claim 1, wherein the soaping condition in the step (3) is as follows: soap flakes 1g/L, soda 1g/L,65 deg.C, 15min, bath ratio 1: 30.
6. A green Lyocell fabric dyed with rosemary which is a vegetable dye, characterized in that the fabric is prepared by the method for preparing the green Lyocell fabric dyed with rosemary which is a vegetable dye according to any one of claims 1 to 5.
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