CN113832744A - Environment-friendly clothing dye and application thereof in clothing printing and dyeing - Google Patents
Environment-friendly clothing dye and application thereof in clothing printing and dyeing 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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- 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
- D06P1/22—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 vat dyestuffs including indigo
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- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/5214—Polymers of unsaturated compounds containing no COOH groups or functional derivatives thereof
- D06P1/5221—Polymers of unsaturated hydrocarbons, e.g. polystyrene polyalkylene
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- D06P1/52—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
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- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
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- D06P1/62—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
- D06P1/621—Compounds without nitrogen
- D06P1/622—Sulfonic acids or their salts
- D06P1/623—Aliphatic, aralophatic or cycloaliphatic
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- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
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- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
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- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
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Abstract
The invention discloses an environment-friendly garment dye and application thereof in garment printing and dyeing, wherein the environment-friendly garment dye is prepared from the following raw materials: water, vegetable dye, sodium chlorophenol, polyethylene, citric acid, oleate, polyoxyethylene sorbitan monooleate, ethylene glycol, phosphate, 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, 2, 6-di-tert-butylphenol, a penetrating agent, a dispersing agent, an anti-wrinkling agent and an auxiliary agent. The auxiliary agent is green and environment-friendly, and meanwhile, the dye prepared by the method has good dye uptake and color fastness, and printed clothes have good drapability and crease resistance.
Description
Technical Field
The invention belongs to the technical field of dyes, and particularly relates to an environment-friendly garment dye and application thereof in garment printing and dyeing.
Background
With the gradual appearance of the problems of environmental pollution, health influence and the like of chemical dyes, the plant dyes become hot spots and research directions concerned by researchers due to the unique green environmental protection performance of the plant dyes. The natural plant dyeing is from leaves, stems, flowers, roots, fruits and the like of plants, and mainly has the following advantages: the environment-friendly color-changing dye is harmless to human bodies, good in environmental compatibility, biodegradable, and has a dyeing and decorating function, harm caused by a plurality of chemical dyes is avoided, and the environment compatibility is good. And a plurality of vegetable dyes are Chinese medicinal herbs, so that the vegetable dyes have the effects of diminishing inflammation, preventing insects, resisting bacteria, resisting oxidation, protecting health and the like. The development of healthy and environment-friendly products by utilizing vegetable dyes has become a necessary trend of developing textile printing and dyeing products to health, environment protection, ecology, comfort and functionality.
The most common problem of the plant dyed textile fabric in the prior art is that the color fastness is not ideal enough, and the main reason is that the washing fastness and the light fastness of the fabric are reduced by the unstable chromophoric group of the plant dye; on the other hand, the pigments of the vegetable dyes come from different plants, and the stability of the color fastness of dyed fabrics and the color reproducibility are influenced according to different environments, geographies and seasons.
Chinese patent ZL201811401548.1 discloses a clothing dye and a preparation method thereof, and the clothing dye mainly comprises 5-10 parts of magnesium stearate, 20-30 parts of polyamide resin, 10-15 parts of acridine fused cyclic hydrocarbon, 15-20 parts of organic carboxylic acid compound, 10-20 parts of polyether modified siloxane, 5-15 parts of fatty alcohol-polyoxyethylene ether, 12-20 parts of light stabilizer and 5-15 parts of antioxidant. The garment dye disclosed by the invention has the beneficial effects of difficulty in decoloring, strong oxidation resistance, difficulty in color change, simple process and low cost. However, the wrinkle resistance and drape property affect the beauty of the fabric, and the invention aims to further improve the drape property and wrinkle resistance of the fabric, thereby expanding the application thereof.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an environment-friendly garment dye and application thereof in garment printing and dyeing.
In order to solve the technical problems, the invention adopts the technical scheme that:
an environment-friendly clothing dye is composed of the following raw materials in parts by weight: 50-200 parts of water, 40-150 parts of plant dye, 2-6 parts of sodium pentachlorophenate, 18-25 parts of polyethylene, 5-10 parts of citric acid, 2-5 parts of oleate, 3-10 parts of polyoxyethylene sorbitan monooleate, 4-10 parts of ethylene glycol, 2-8 parts of phosphate, 8-14 parts of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, 1-4 parts of 2, 6-di-tert-butylphenol, 5-12 parts of penetrating agent, 5-12 parts of dispersing agent, 1-5 parts of crease-resistant agent and 1-5 parts of auxiliary agent.
The adopted vegetable dye is nontoxic, harmless and pollution-free, is environment-friendly and healthy, reduces the pollution to the environment in the using process, and the oleate can be used as a dustproof agent, reduces the pollution to other dyes and fabrics and has a certain effect on protecting the environment; the polyethylene dye has the effects of environmental protection and lasting and stable dyeing; the polyethylene has excellent bonding performance, can effectively improve the bonding performance of a finished product, and has excellent weather resistance; the polyoxyethylene sorbitan monooleate can be used as a leveling agent, an emulsifier and a softening agent to improve the comprehensive performance of the dye, the phosphate can improve the wetting effect of the dye on plants, the 2, 6-di-tert-butylphenol can be used as an accelerating agent in the dyeing process to improve the dyeing efficiency and reduce the dyeing time, the penetrating agent can promote the dye to enter the dyed material to improve the color fixing rate, the crease-resist agent can improve the soft, smooth and comfortable hand feeling of dye fabrics, and the auxiliary agent further improves the comprehensive performance of the dye in various aspects.
The vegetable dye is one or more of indigo, gardenia yellow and turmeric.
The penetrating agent is one or more than two of alkyl sodium sulfonate, secondary alkyl sodium sulfate, isooctanol polyoxyethylene ether sodium phosphate, sulfated castor oil and phosphate compounds; the dispersant is sodium lignosulphonate or sodium carboxymethyl cellulose.
In order to improve the application effect of the dye in the fabric, the anti-creasing agent can be added in the dye preparation process to effectively improve the flatness of the fabric, so that the fabric can achieve better effects such as beauty, smoothness, flatness and the like after being dyed, the anti-creasing agent can be added to effectively reduce the friction between the fabric and between the fabric and equipment, reduce scratches or streaks of the fabric in the wet processing process, improve the better smoothness of the fabric in a wet state, improve the smoothness of the fabric in the processing process and prevent the knotting phenomenon, thereby achieving the efficient anti-creasing effect of the anti-creasing agent.
Specifically, ester and ether components with relatively large molecular weights in the components of the anti-wrinkling agent are preferentially added, so that the uniform distribution of the anti-wrinkling agent can be ensured, and if the temperature of the alcohol amine component is relatively high, the structural property is relatively unstable, so that the alcohol amine component needs to be added after being reduced by a certain temperature to ensure the integrity of the structural property, and finally, the uniform dispersion is ensured after the temperature reduction treatment.
The preparation method of the anti-wrinkling agent comprises the following steps: mixing 5-15 parts by weight of water, 2-8 parts by weight of decyl isocyanate, 1-5 parts by weight of polyether modified silicone oil, 1-3 parts by weight of isomeric tridecanol polyoxyethylene ether and 0.1-1 part by weight of isobornyl acetate, and stirring at 70-100 ℃ and 600-ion flow 1000rpm for 5-10min to obtain an anti-wrinkling agent base solution; and cooling to 60-80 ℃, adding 0.5-1 part by weight of N, N-dimethylethanolamine and 0.5-1 part by weight of linoleic acid diethanolamide, continuously stirring for 20-30min, and cooling to room temperature at the speed of 10-18 ℃/min to obtain the anti-wrinkling agent.
The preparation method of the auxiliary agent comprises the following steps: s1, reacting 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane with ethylene glycol methyl ether and 2-methoxyethoxymethyl chloride to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane;
s2, mixing quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane and octamethyl cyclotetrasiloxane in S1, and adding sodium hydroxide and dimethyl sulfoxide to react to obtain epoxy amino silicone oil;
and S3, dissolving the epoxy amino silicone oil and the glucoside in the S2 into N-methyl pyrrolidone, and adding boron trifluoride diethyl etherate to react to obtain the assistant.
In industrial dyeing processes, the effect of dye on the fabric dyeing performance is often determined by the nature of the dye, and the wetting performance, color fastness level, stability and hand feeling experience of the dye on the fabric in the dyeing process are often the most concerned, and the appearance and use effect of the dyed fabric are also influenced.
Aiming at the technical problems of high cost, poor chemical stability and high temperature resistance, low color fastness, poor hand feeling, easy fading, skin irritation, great harm to the environment, large use amount, single function and the like of the dye in the prior art, the invention has the advantages of obvious dyeing and color homogenizing effect, good acid and alkali resistance, high color fastness, good hand feeling, difficult fading, no stimulation to human skin, safe use, environmental protection and the like.
Specifically, in the implementation process, S1, silazane and 2-methoxyethoxymethyl chloride are used as main quaternized raw materials, and the quaternized silazane is generated by heating and stirring in the presence of ethylene glycol methyl ether serving as a solvent; s1, mixing quaternized silazane and octamethylcyclotetrasiloxane, and generating epoxy amino silicone oil under the protection of dimethyl sulfoxide serving as an accelerator and nitrogen; s3, epoxy amino silicone oil and glucoside generate functional groups with amino groups, alkoxy silane groups, sulfonic acid and the like under the action of boron trifluoride ether serving as a catalyst, the stability of the product is strengthened from molecular functional groups, and amino groups and sulfonic acid groups of organic silicon functional groups and hydrophilic groups with adhesive force effects are introduced, so that the glucoside modified by the multifunctional groups has good adhesive force and lubricating property, and the auxiliary agent is obtained.
The method for preparing the modified glucoside is simple in process and convenient to operate, and particularly the obtained glucoside salt modified by amino groups, alkyl groups and sulfonic acid groups not only has the relevant properties of nonionic surfactant alkyl glucoside, but also improves the water solubility of the product due to the introduction of sulfonate ions, so that the problems of poor water solubility, easy precipitation at low temperature and the like of alkyl glucoside with a long carbon chain are solved.
Preferably, the preparation method of the auxiliary agent comprises the following steps: s1, mixing 10-50 parts by weight of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane with 100 parts by weight of ethylene glycol methyl ether and 40-80 parts by weight of 2-methoxyethoxymethyl chloride, stirring and reacting at 60-70 ℃ and 400-600rpm for 4-8h, evaporating and concentrating at 80-100 ℃ to the original volume of 1/5-1/8, and drying to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane;
s2, taking 10-30 parts by weight of quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane in S2, adding 10-30 parts by weight of octamethylcyclotetrasiloxane, mixing, heating to 80-100 ℃ under the protection of nitrogen, adding 0.5-3 parts by weight of sodium hydroxide and 0.4-2 parts by weight of dimethyl sulfoxide, reacting at 80-120 ℃ and 200-400rpm for 3-6h, adding 0.5-3 parts by weight of 1, 3-bis (3-aminopropyl) -tetramethyldisiloxane, continuing to react for 1-3h, and distilling at 60-80 ℃ under reduced pressure for 0.5-2h to obtain epoxy amino silicone oil;
s3, dissolving 5-15 parts by weight of epoxy amino silicone oil and 0.1-1 part by weight of glucoside in 10-30 parts by weight of N-methylpyrrolidone, adding 1-4 parts by weight of 1-5 wt% boron trifluoride diethyl etherate solution, reacting for 4-8h at 70-90 ℃ and 300-500rpm, and distilling under reduced pressure at 60-80 ℃ until the solvent N-methylpyrrolidone is completely removed to obtain the assistant.
The glucoside is alkyl glucoside or modified glucoside.
The alkyl glycoside is one or more than two of methyl glycoside, ethyl glycoside, propyl glycoside, butyl glycoside, hexyl glycoside, octyl glycoside, decyl glycoside, dodecyl glycoside and tetradecyl glycoside.
The preparation method of the modified glucoside comprises the following steps: reacting alkyl glycoside, propylene oxide, sulfuryl chloride and phosphotungstic acid, adding a modifier and stirring; adjusting the pH value of the reaction solution, and adding ammonium ceric nitrate to react to obtain the modified glucoside.
Preferably, the preparation method of the modified glycoside is as follows: mixing 5-10 parts by weight of butyl glucoside, 2-8 parts by weight of propylene oxide, 5-15 parts by weight of water, 2-8 parts by weight of sulfuryl chloride and 3-10 parts by weight of phosphotungstic acid, reacting for 2-6h at 80-110 ℃ and 1200rpm, adding 5-10 parts by weight of modifier, 3-8 parts by weight of acrylamide and 0.5-3 parts by weight of 20-40 wt% sodium hydroxide ethanol solution, and stirring for 10-30min at 600-1200 rpm; adjusting pH to 9-11 with 1-3mol/L sodium hydroxide water solution, adding 0.1-1 weight part of ammonium ceric nitrate, and reacting at 90-130 deg.C for 4-7h to obtain modified glycoside.
The modifier is sodium 3-chloro-2-hydroxypropyl sulfonate and/or vinyl tri (2-methoxyethoxy) silane; preferably, the modifier is prepared by mixing 3-chloro-2-hydroxypropyl sodium sulfonate and vinyl tri (2-methoxyethoxy) silane according to the mass ratio of (1-3): (1-5).
The application of the environment-friendly clothing dye in clothing printing and dyeing.
The invention has the beneficial effects that:
1. the anti-creasing agent prepared by the invention has the advantages of effectively reducing the friction between fabrics and equipment, reducing the scratches or streaks of the fabrics in the wet processing process, improving the better smoothness of the fabrics in a wet state, improving the smoothness of the fabrics in the processing process, preventing the knotting phenomenon and achieving the efficient anti-creasing effect of the anti-creasing agent.
2. The method has simple process and convenient operation, particularly the obtained modified glucoside sulfonate not only has the relevant properties of the nonionic surfactant alkyl glucoside, but also has good lubricating property, and simultaneously the water solubility of the product is improved due to the introduction of the sulfonate ions, so that the problems of poor water solubility, easy precipitation at low temperature and the like of the alkyl glucoside with a long carbon chain are solved, and meanwhile, the auxiliary agent is green and environment-friendly.
3. The dye prepared by the invention has good dye uptake and color fastness, and also has good drapability and wrinkle resistance.
Detailed Description
The above summary of the present invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following examples.
Introduction of some raw materials in this application:
the indigo in the examples was purchased from Gi chemical products, Inc. of Texas.
In the examples, polyoxyethylene sorbitan monooleate was purchased from denna navigation chemical technology ltd, model: t-80, cargo number: 383.
in the embodiment, polyethylene is purchased from Jiuding chemical materials Co, Yuyao, model number: U-PE350, density: 0.947g/cm3。
Polyether modified silicone oil in examples, CAS No.: 67674-67-3, available from Jinanhao chemical technology Ltd, viscosity: (25 ℃)2000 mpa.S.
Examples isomeric tridecanol polyoxyethylene ethers, CAS number: 9043-30-5.
Examples isobornyl acetate, CAS No.: 125-12-2.
Example 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinylcyclotetrasilazane, CAS number: 5162-63-0.
Example 3-chloro-2-hydroxypropyl sodium sulfonate, CAS No.: 126-83-0.
Examples vinyl tris (2-methoxyethoxy) silane, CAS number: 1067-53-4.
In the examples, the commercially available anti-wrinkling agent is purchased from Jiahong organosilicon science and technology Limited, Dongguan city, and the model is as follows: goon906, cat #: 906, type: non-ionic.
Example 1
An environment-friendly clothing dye is composed of the following raw materials in parts by weight: 100 parts by weight of water, 80 parts by weight of indigo, 4 parts by weight of sodium pentachlorophenate, 20 parts by weight of polyethylene, 6 parts by weight of citric acid, 3 parts by weight of oleate, 5 parts by weight of polyoxyethylene sorbitan monooleate, 6 parts by weight of ethylene glycol, 5 parts by weight of phosphate ester, 10 parts by weight of 3-chloro-2-hydroxypropyltrimethylammonium chloride, 2 parts by weight of 2, 6-di-tert-butylphenol, 8 parts by weight of sulfated castor oil, 6 parts by weight of sodium carboxymethylcellulose, and 3 parts by weight of an anti-wrinkling agent. The anti-wrinkling agent is a commercially available anti-wrinkling agent.
Example 2
An environment-friendly clothing dye is composed of the following raw materials in parts by weight: 100 parts by weight of water, 80 parts by weight of indigo, 4 parts by weight of sodium pentachlorophenate, 20 parts by weight of polyethylene, 6 parts by weight of citric acid, 3 parts by weight of oleate, 5 parts by weight of polyoxyethylene sorbitan monooleate, 6 parts by weight of ethylene glycol, 5 parts by weight of phosphate ester, 10 parts by weight of 3-chloro-2-hydroxypropyltrimethylammonium chloride, 2 parts by weight of 2, 6-di-tert-butylphenol, 8 parts by weight of sulfated castor oil, 6 parts by weight of sodium carboxymethylcellulose, and 3 parts by weight of an anti-wrinkling agent.
The preparation method of the anti-wrinkling agent comprises the following steps: mixing 8 parts by weight of water, 4 parts by weight of decyl isocyanate, 3 parts by weight of polyether modified silicone oil, 2 parts by weight of isomeric tridecanol polyoxyethylene ether and 0.4 part by weight of isobornyl acetate, and stirring at 90 ℃ and 800rpm for 6min to obtain an anti-wrinkling agent base solution; and cooling to 80 ℃, adding 0.6 weight part of N, N-dimethylethanolamine and 0.8 weight part of linoleic acid diethanolamide, continuously stirring for 25min, and cooling to room temperature at the speed of 15 ℃/min to obtain the anti-wrinkling agent.
Example 3
An environment-friendly clothing dye is composed of the following raw materials in parts by weight: 100 parts by weight of water, 80 parts by weight of indigo, 4 parts by weight of sodium pentachlorophenate, 20 parts by weight of polyethylene, 6 parts by weight of citric acid, 3 parts by weight of oleate, 5 parts by weight of polyoxyethylene sorbitan monooleate, 6 parts by weight of ethylene glycol, 5 parts by weight of phosphate ester, 10 parts by weight of 3-chloro-2-hydroxypropyltrimethylammonium chloride, 2 parts by weight of 2, 6-di-tert-butylphenol, 8 parts by weight of sulfated castor oil, 6 parts by weight of sodium carboxymethylcellulose, 3 parts by weight of an anti-wrinkling agent and 3 parts by weight of an auxiliary agent.
The preparation method of the anti-wrinkling agent comprises the following steps: mixing 8 parts by weight of water, 4 parts by weight of decyl isocyanate, 3 parts by weight of polyether modified silicone oil, 2 parts by weight of isomeric tridecanol polyoxyethylene ether and 0.4 part by weight of isobornyl acetate, and stirring at 90 ℃ and 800rpm for 6min to obtain an anti-wrinkling agent base solution; and cooling to 80 ℃, adding 0.6 weight part of N, N-dimethylethanolamine and 0.8 weight part of linoleic acid diethanolamide, continuously stirring for 25min, and cooling to room temperature at the speed of 15 ℃/min to obtain the anti-wrinkling agent.
The preparation method of the auxiliary agent comprises the following steps: s1, mixing 30 parts by weight of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane, 150 parts by weight of ethylene glycol methyl ether and 60 parts by weight of 2-methoxyethoxymethyl chloride, stirring and reacting at 65 ℃ and 500rpm for 6 hours, evaporating and concentrating at 90 ℃ to an original volume of 1/6, and drying to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane;
s2, taking 20 parts by weight of quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane, adding 20 parts by weight of octamethylcyclotetrasiloxane, heating to 95 ℃ under the protection of nitrogen, adding 1 part by weight of sodium hydroxide and 0.6 part by weight of dimethyl sulfoxide, reacting for 5 hours at 100 ℃ and 300rpm, adding 1 part by weight of 1, 3-bis (3-aminopropyl) -tetramethyldisiloxane, continuing to react for 2 hours, and distilling at 70 ℃ under reduced pressure for 1 hour to obtain epoxy amino silicone oil;
s3, dissolving 10 parts by weight of epoxy amino silicone oil and 0.2 part by weight of glucoside in 20 parts by weight of N-methylpyrrolidone, adding 2 parts by weight of 2 wt% boron trifluoride diethyl etherate solution, reacting at 80 ℃ and 400rpm for 6 hours, and distilling at 70 ℃ under reduced pressure until the solvent N-methylpyrrolidone is completely removed to obtain an assistant; the glucoside is butyl glucoside.
Comparative example 1
Essentially the same as example 3, except that the preparation of the adjuvant is as follows:
s1, mixing 30 parts by weight of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane, 150 parts by weight of ethylene glycol methyl ether and 60 parts by weight of 2-methoxyethoxymethyl chloride, stirring and reacting at 65 ℃ and 500rpm for 6 hours, evaporating and concentrating at 90 ℃ to an original volume of 1/6, and drying to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane;
s2, taking 20 parts by weight of quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane, adding 20 parts by weight of octamethylcyclotetrasiloxane, heating to 95 ℃ under the protection of nitrogen, adding 1 part by weight of sodium hydroxide and 0.6 part by weight of dimethyl sulfoxide, reacting for 5 hours at 100 ℃ and 300rpm, adding 1 part by weight of 1, 3-bis (3-aminopropyl) -tetramethyldisiloxane, continuing to react for 2 hours, and distilling under reduced pressure for 1 hour at 70 ℃ to obtain the assistant.
Example 4
An environment-friendly clothing dye is composed of the following raw materials in parts by weight: 100 parts by weight of water, 80 parts by weight of indigo, 4 parts by weight of sodium pentachlorophenate, 20 parts by weight of polyethylene, 6 parts by weight of citric acid, 3 parts by weight of oleate, 5 parts by weight of polyoxyethylene sorbitan monooleate, 6 parts by weight of ethylene glycol, 5 parts by weight of phosphate ester, 10 parts by weight of 3-chloro-2-hydroxypropyltrimethylammonium chloride, 2 parts by weight of 2, 6-di-tert-butylphenol, 8 parts by weight of sulfated castor oil, 6 parts by weight of sodium carboxymethylcellulose, 3 parts by weight of an anti-wrinkling agent and 3 parts by weight of an auxiliary agent.
The preparation method of the anti-wrinkling agent comprises the following steps: mixing 8 parts by weight of water, 4 parts by weight of decyl isocyanate, 3 parts by weight of polyether modified silicone oil, 2 parts by weight of isomeric tridecanol polyoxyethylene ether and 0.4 part by weight of isobornyl acetate, and stirring at 90 ℃ and 800rpm for 6min to obtain an anti-wrinkling agent base solution; and cooling to 80 ℃, adding 0.6 weight part of N, N-dimethylethanolamine and 0.8 weight part of linoleic acid diethanolamide, continuously stirring for 25min, and cooling to room temperature at the speed of 15 ℃/min to obtain the anti-wrinkling agent.
The preparation method of the auxiliary agent comprises the following steps:
s1, mixing 30 parts by weight of 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane, 150 parts by weight of ethylene glycol methyl ether and 60 parts by weight of 2-methoxyethoxymethyl chloride, stirring at 65 ℃ and 500rpm for reaction for 6 hours, evaporating and concentrating at 90 ℃ to 1/6 of original volume, and drying to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane;
s2, taking 20 parts by weight of quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane, adding 20 parts by weight of octamethylcyclotetrasiloxane, heating to 95 ℃ under the protection of nitrogen, adding 1 part by weight of sodium hydroxide and 0.6 part by weight of dimethyl sulfoxide, reacting for 5 hours at 100 ℃ and 300rpm, adding 1 part by weight of 1, 3-bis (3-aminopropyl) -tetramethyldisiloxane, continuing to react for 2 hours, and distilling at 70 ℃ under reduced pressure for 1 hour to obtain epoxy amino silicone oil;
s3, dissolving 10 parts by weight of epoxy amino silicone oil and 0.2 part by weight of glucoside in 20 parts by weight of N-methylpyrrolidone, adding 2 parts by weight of 2 wt% boron trifluoride diethyl etherate solution, reacting at 80 ℃ and 400rpm for 6h, and distilling at 70 ℃ under reduced pressure until the solvent N-methylpyrrolidone is completely removed to obtain the assistant.
The glucoside is modified glucoside; the preparation method of the modified glucoside comprises the following steps: mixing 7 parts by weight of butyl glucoside, 4 parts by weight of propylene oxide, 8 parts by weight of water, 4 parts by weight of sulfuryl chloride and 5 parts by weight of phosphotungstic acid, reacting for 4 hours at 100 ℃ and 1000rpm, adding 8 parts by weight of modifier, 6 parts by weight of acrylamide and 1 part by weight of 30 wt% sodium hydroxide ethanol solution, and stirring for 20 minutes at 1000 rpm; adjusting the pH value to 10 by using 2mol/L aqueous solution of sodium hydroxide, adding 0.2 part by weight of ammonium ceric nitrate, and reacting for 5 hours at 110 ℃ to obtain modified glucoside; the modifier is 3-chloro-2-hydroxypropyl sodium sulfonate.
Example 5
Essentially the same as example 4 except that the modifier is vinyltris (2-methoxyethoxy) silane.
Example 6
Essentially the same as example 4, except that the modifier consists of sodium 3-chloro-2-hydroxypropyl sulfonate and vinyltris (2-methoxyethoxy) silane in a mass ratio of 2: 3.
Test example 1
The environmentally friendly garment dye prepared in examples 1-6 was used for a fabric (100% nylon fabric, gram weight 160 g/m)2) And (6) dyeing. Soaking the fabric into an environment-friendly clothing dye at a bath ratio of 1g to 30mL, heating to 60 ℃ at a speed of 2 ℃/min, heating to 80 ℃ at a speed of 1 ℃/min, heating to 100 ℃ at a speed of 0.8 ℃/min, keeping the temperature for 50min, taking out, rolling and drying, wherein the rolling residue rate is 45%, and thus obtaining the dyed fabric; soaking the dyed fabric into water at 35 ℃ for washing, wherein the bath ratio is 1g to 20mL, and keeping the temperature for 10 min; taking out and drying to obtain a finished fabric, and testing the finished fabric as follows.
1. And (3) friction color fastness test: the test is carried out by referring to the national standard GB/T3920-.
2. Testing water color fastness: the fabric is tested by referring to the national standard GB/T5713 and 2013 ' color fastness to Water ' of textile color fastness test ', before the test, the finished fabric is subjected to humidity adjustment for 6 hours under the conditions that the temperature is 20 ℃ and the relative humidity is 65%, the test is carried out for 4 times in parallel, and the average value is taken.
3. And (3) testing the coloring rate: the test is carried out by referring to national standard GB/T9337-2009 determination of dyeing rate of disperse dye at high temperature, the test is carried out for 4 times in parallel, and the average value is taken.
TABLE 1 test results of crocking fastness, water fastness and dyeing degree
From the results in table 1, it can be seen that the dye added with the self-made anti-creasing agent of the present invention can improve the dyeing degree and color fastness of the fabric to a certain extent, because the anti-creasing agent can effectively reduce the friction between the fabric and between the fabric and equipment, and reduce the scratches or streaks of the fabric in the wet processing process, thereby improving the tight connection between the fabric and the fabric, and further improving the dyeing degree of the fabric. The color fastness and the dyeing degree of the fabric can be further improved by adding the auxiliary agent into the dye, because the prepared auxiliary agent has functional groups such as amino groups, alkoxy silane groups, sulfonic acid and the like, the stability of the product is enhanced from the molecular functional groups, and the amino groups and the sulfonic acid groups of the organic silicon functional groups and the hydrophilic groups with adhesive force effects are introduced, so that the glucoside modified by the multifunctional groups has good adhesive force and lubricating property, and the color fixing rate and the dyeing degree of the fabric are improved. Example 6 adopts a modifier compounded by 3-chloro-2-hydroxypropyl sodium sulfonate and vinyl tris (2-methoxyethoxy) silane, which can further improve the color fixation rate and color fastness of the fabric, because the 3-chloro-2-hydroxypropyl sodium sulfonate can improve the water solubility of the dye, and the vinyl tris (2-methoxyethoxy) silane can improve the oil solubility of the dye, and the two can be used simultaneously to synergize, and the amino and sulfonic acid groups of the organosilicon functional group and the hydrophilic group with adhesive force effect are introduced, so that the glycoside modified by the multifunctional group has good adhesive force and lubricating property, and finally the comprehensive performance of the dye is improved.
Test example 2
And (3) testing the coefficient of draping: the finished fabric of test example 1 was tested with reference to national standard GB/T23329-.
TABLE 2 drape coefficient test results
From the results in table 2, it can be seen that the dye added with the self-made anti-creasing agent can improve the drapability of the fabric to a certain extent, because the anti-creasing agent can effectively reduce the friction between the fabric and between the fabric and equipment, and reduce scratches or streaks of the fabric in the wet processing process, so that the tight connection between the fabric and the fabric is improved, the drapability of the fabric is improved, and the addition of the auxiliary agent can further improve the drapability of the fabric.
Test example 3
And (3) testing the recovery performance of the wrinkles: the finished fabric of test example 1 was tested with reference to the national standard GB/T3819 and 1997 "recovery angle method for measuring crease recovery of textile fabric", before the test, the finished fabric was conditioned for 6 hours at a temperature of 20 ℃ and a relative humidity of 65%, the test temperature was 35 ℃, the test relative humidity was 90%, the test load: 10N, stress event 5min, parallel 4 tests, and average.
Table 3 wrinkle recovery test results
From the test data in table 3, it can be seen that compared with the fabric treated by adding the commercially available anti-creasing agent dye, the fabric treated by adding the self-made anti-creasing agent dye of the invention has significantly improved crease recovery angle, and the crease resistance performance is still good without much influence on the crease recovery angle of the fabric after adding the auxiliary agent.
Claims (10)
1. The environment-friendly clothing dye is characterized by comprising the following raw materials in parts by weight: 50-200 parts of water, 40-150 parts of plant dye, 2-6 parts of sodium pentachlorophenate, 18-25 parts of polyethylene, 5-10 parts of citric acid, 2-5 parts of oleate, 3-10 parts of polyoxyethylene sorbitan monooleate, 4-10 parts of ethylene glycol, 2-8 parts of phosphate, 8-14 parts of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, 1-4 parts of 2, 6-di-tert-butylphenol, 5-12 parts of penetrating agent, 5-12 parts of dispersing agent, 1-5 parts of crease-resistant agent and 1-5 parts of auxiliary agent.
2. The eco-friendly garment dye according to claim 1, wherein the vegetable dye is one or more of indigo, gardenia yellow and turmeric.
3. The environmentally friendly garment dye according to claim 1, wherein the penetrant is one or more of alkyl sodium sulfonate, secondary alkyl sodium sulfate, isooctanol polyoxyethylene ether phosphate sodium salt, sulfated castor oil and phosphate ester compounds; the dispersant is sodium lignosulphonate or sodium carboxymethyl cellulose.
4. The environmentally friendly garment dye according to claim 1, wherein the anti-wrinkling agent is prepared by the following method: mixing 5-15 parts by weight of water, 2-8 parts by weight of decyl isocyanate, 1-5 parts by weight of polyether modified silicone oil, 1-3 parts by weight of isomeric tridecanol polyoxyethylene ether and 0.1-1 part by weight of isobornyl acetate, and stirring at 70-100 ℃ and 600-ion flow 1000rpm for 5-10min to obtain an anti-wrinkling agent base solution; and cooling to 60-80 ℃, adding 0.5-1 part by weight of N, N-dimethylethanolamine and 0.5-1 part by weight of linoleic acid diethanolamide, continuously stirring for 20-30min, and cooling to room temperature at the speed of 10-18 ℃/min to obtain the anti-wrinkling agent.
5. The environmentally friendly garment dye of claim 1, wherein the preparation method of the auxiliary agent is as follows: s1, reacting 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane with ethylene glycol methyl ether and 2-methoxyethoxymethyl chloride to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane;
s2, mixing quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane and octamethyl cyclotetrasiloxane in S1, and adding sodium hydroxide and dimethyl sulfoxide to react to obtain epoxy amino silicone oil;
and S3, dissolving the epoxy amino silicone oil and the glucoside in the S2 into N-methyl pyrrolidone, and adding boron trifluoride diethyl etherate to react to obtain the assistant.
6. The environmentally friendly garment dye of claim 5, wherein the glycoside is an alkyl glycoside or a modified glycoside.
7. The environmentally friendly garment dye according to claim 6, wherein the alkyl glycoside is one or more of methyl glycoside, ethyl glycoside, propyl glycoside, butyl glycoside, hexyl glycoside, octyl glycoside, decyl glycoside, dodecyl glycoside, and tetradecyl glycoside.
8. The environmentally friendly garment dye of claim 6, wherein the modified glycoside is prepared by the following method: reacting alkyl glycoside, propylene oxide, sulfuryl chloride and phosphotungstic acid, adding a modifier and stirring; adjusting the pH value of the reaction solution, and adding ammonium ceric nitrate to react to obtain the modified glucoside.
9. The environmentally friendly garment dye according to claim 8, wherein the modifier is sodium 3-chloro-2-hydroxypropyl sulfonate and/or vinyl tris (2-methoxyethoxy) silane.
10. Use of an environmentally friendly garment dye as claimed in any one of claims 1 to 9 in garment printing.
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