CN113832744B - 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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- CN113832744B CN113832744B CN202111185010.3A CN202111185010A CN113832744B CN 113832744 B CN113832744 B CN 113832744B CN 202111185010 A CN202111185010 A CN 202111185010A CN 113832744 B CN113832744 B CN 113832744B
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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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- D06P1/52—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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- D06P1/00—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
- D06P1/44—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
- D06P1/642—Compounds containing nitrogen
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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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- D06P1/00—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
- D06P1/44—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 application discloses an environment-friendly clothing dye and application thereof in clothing printing and dyeing, wherein the environment-friendly clothing dye comprises 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, penetrating agent, dispersing agent, crease-resist agent and auxiliary agent. The auxiliary agent is green and environment-friendly, and meanwhile, the dye prepared by the application has good dye uptake and color fastness, and the dyed clothing has good draping property and crease resistance.
Description
Technical Field
The application 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
Along 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 of researchers due to the special green environment-friendly performance. The natural plant dyeing is derived from leaves, stems, flowers, roots, fruits and the like of plants, and has the following advantages: harmless to human body, good environmental compatibility, biodegradability, dyeing and decoration functions, avoiding harm caused by a plurality of chemical dyes, and good environmental compatibility. In addition, because the plant dye is the Chinese herbal medicine, the plant dye has the effects of diminishing inflammation, preventing insect, resisting bacteria, resisting oxidation, protecting health and the like. The development of healthy and environment-friendly products by using vegetable dyes has become a necessary trend of the development of textile printing and dyeing products to health, environment protection, ecology, comfort and functionality.
The most common problem in the prior art of vegetable dyeing textile fabrics is that the color fastness is not ideal, and the main reason is that on one hand, the unstable chromophores of vegetable dyes reduce the washing fastness and the light fastness; on the other hand, the pigment of the vegetable dye comes from different plants, and the stability of the vegetable dye to the color fastness of the dyed fabric and the color reproducibility are affected according to different environments, geographies and seasons.
The 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 thick 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 clothing dye has the advantages of difficult decolorization, strong oxidation resistance, difficult discoloration, simple process and low cost. However, the anti-wrinkle performance and the draping performance affect the beauty of the fabric, and the application aims to further improve the draping performance and the anti-wrinkle performance of the fabric, thereby expanding the application of the fabric.
Disclosure of Invention
Aiming at the defects in the prior art, the application provides an environment-friendly clothing dye and application thereof in clothing printing and dyeing.
In order to solve the technical problems, the application adopts the following technical scheme:
an environment-friendly clothing dye is prepared from the following raw materials in parts by weight: 50-200 parts of water, 40-150 parts of vegetable 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-resist agent and 1-5 parts of auxiliary agent.
The vegetable dye adopted in the application is nontoxic, harmless, pollution-free, environment-friendly and healthy, reduces the pollution to the environment in the use process, and the oleate can be used as a dustproof agent to reduce the pollution to other dyes and fabrics and has a certain effect on environmental protection; the polyethylene has the effects of environmental protection and durable and stable dyeing; polyethylene has excellent adhesive property, can effectively improve the adhesive property of a finished product, and has excellent weather resistance; the polyoxyethylene sorbitan monooleate can be used as a leveling agent and an emulsifying agent, and also can be used as a softening agent, so that the comprehensive performance of the dye is improved, 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, the dyeing efficiency is improved, the dyeing time is reduced, the penetrating agent can promote the dye to enter the dyed substances, the fixation rate is improved, 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 multiple aspects.
The vegetable dye is one or more of indigo, gardenia yellow and turmeric.
The penetrating agent is one or more than two of sodium alkyl sulfonate, sodium secondary alkyl sulfate, isooctyl alcohol polyoxyethylene ether phosphate sodium salt, sulfated castor oil and phosphate compounds; the dispersing agent is sodium lignin sulfonate or sodium carboxymethyl cellulose.
In order to improve the application effect of the dye in the fabric, the application can effectively improve the flatness of the fabric in the dye preparation process, so that the fabric can also achieve better effects of beautiful appearance, smoothness, flatness and the like after being dyed, the crease-resist agent can be added to effectively reduce friction among the fabric, the fabric and equipment, reduce scratches or streaks of the fabric in the wet processing process, improve the smoothness of the fabric in the wet state, and simultaneously the crease-resist agent can also improve the fluency of the fabric in the processing process, prevent knotting and achieve the high-efficiency crease-resist effect of the crease-resist agent.
Specifically, the ester and ether components with relatively large molecular weight are preferentially added in the composition of the crease-resist agent, so that the distribution of the crease-resist agent is uniform, and if the alcohol amine component is relatively high in temperature, the structural property is relatively unstable, so that the crease-resist agent needs to be added after a certain temperature is reduced to ensure the integrity of the structural property, and the uniform dispersion is finally ensured through cooling treatment.
The preparation method of the crease-resist 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 600-1000rpm for 5-10min to obtain a base solution of the crease-resist agent; cooling to 60-80deg.C, adding 0.5-1 weight parts of N, N-dimethylethanolamine and 0.5-1 weight parts of linoleic acid diethanolamide, stirring for 20-30min, and cooling to room temperature at a speed of 10-18deg.C/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 the S1, and adding sodium hydroxide and dimethyl sulfoxide for reaction to obtain epoxy amino silicone oil;
s3, dissolving epoxy amino silicone oil and glycoside in the S2 in N-methyl pyrrolidone, and adding boron trifluoride diethyl etherate solution for reaction to obtain the auxiliary agent.
In the industrial dyeing process, the effect of the dye on the dyeing performance of the fabric often depends on the properties of the dye, and in the dyeing process, how the dye wets the fabric, the color fastness level, the stability and the hand feeling experience are often the most concerned, and the appearance and the using effect of the dyed fabric are also affected.
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, large environmental hazard, large usage amount, single function and the like of the dye in the prior art, the application has the characteristics of obvious dyeing color homogenizing effect, good acid and alkali resistance, high color fastness, good hand feeling, difficult fading, no irritation to human skin, safe and environment-friendly use and the like.
Specifically, in the implementation process, S1, using silazane and 2-methoxyethoxymethyl chloride as main raw materials for quaternization, and heating and stirring in the presence of a solvent of ethylene glycol methyl ether to generate quaternized silazane; s1, mixing quaternized silazane and octamethyl cyclotetrasiloxane, and generating epoxy amino silicone oil under the protection of accelerator dimethyl sulfoxide and nitrogen; s3, epoxy amino silicone oil and glycoside generate functional groups with amino groups, alkoxy silane groups, sulfonic acid and the like under the action of boron trifluoride diethyl ether serving as catalysts, stability of products is enhanced from the molecular functional groups, and amino groups and sulfonic acid groups with adhesive force effect and organic silicon functional groups and hydrophilic groups are introduced, so that the multifunctional group modified glycoside has good adhesive force and lubricating property, and the auxiliary agent is obtained.
The method for preparing the modified glycoside has simple process and convenient operation, and particularly the obtained glycoside salt modified by amino, alkyl and sulfonic acid groups not only has the relevant properties of the nonionic surfactant alkyl glycoside, but also improves the water solubility of the product due to the introduction of sulfonate ions, thereby solving the problems of poor water solubility, easy precipitation at low temperature and the like of the long-carbon-chain alkyl glycoside.
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 cyclic tetrasilazane with 100-200 parts by weight of ethylene glycol methyl ether and 40-80 parts by weight of 2-methoxyethoxymethyl chloride, stirring at 60-70 ℃ and 400-600rpm for reaction for 4-8 hours, evaporating and concentrating at 80-100 ℃ to 1/5-1/8 of the original volume, and drying to obtain quaternized 1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclic tetrasilazane;
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 octamethyl cyclotetrasiloxane, 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 for 3-6h at 80-120 ℃ at 200-400rpm, adding 0.5-3 parts by weight of 1, 3-bis (3-aminopropyl) -tetramethyl disiloxane, continuously reacting for 1-3h, and then carrying out reduced pressure distillation for 0.5-2h at 60-80 ℃ to obtain epoxy amino silicone oil;
s3, taking 5-15 parts by weight of epoxy amino silicone oil and 0.1-1 part by weight of glycoside to dissolve in 10-30 parts by weight of N-methyl pyrrolidone, adding 1-4 parts by weight of 1-5wt% boron trifluoride diethyl ether solution into the mixture, reacting for 4-8 hours at 70-90 ℃ and 300-500rpm, and distilling under reduced pressure at 60-80 ℃ until the solvent N-methyl pyrrolidone is completely removed, thus obtaining the auxiliary agent.
The glycoside is alkyl glycoside or modified glycoside.
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.
The preparation method of the modified glycoside comprises the following steps: reacting alkyl glycoside, propylene oxide, sulfuryl chloride and phosphotungstic acid, and then adding a modifier and stirring; and regulating the pH value of the reaction solution, and adding ammonium ceric nitrate to react to obtain the modified glycoside.
Preferably, the preparation method of the modified glycoside comprises the following steps: 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 2-6 hours at 80-110 ℃ and 800-1200rpm, adding 5-10 parts by weight of modifier, 3-8 parts by weight of acrylamide and 0.5-3 parts by weight of 20-40wt% sodium hydroxide ethanol solution, and stirring for 10-30 minutes at 600-1200 rpm; and then adjusting the pH value to be between 9 and 11 by using 1 to 3mol/L sodium hydroxide aqueous solution, adding 0.1 to 1 weight part of ammonium cerium nitrate, and reacting for 4 to 7 hours at the temperature of between 90 and 130 ℃ to obtain the modified glycoside.
The modifier is sodium 3-chloro-2-hydroxypropyl sulfonate and/or vinyl tri (2-methoxyethoxy) silane; preferably, the modifier is prepared from 3-chlorine-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 application has the beneficial effects that:
1. the crease-resist agent prepared by the application has the advantages of effectively reducing friction among fabrics and between fabrics and equipment, reducing scratches or streaks of the fabrics in the wet processing process, improving the smoothness of the fabrics in the wet state, improving the smoothness of the fabrics in the processing process, and preventing knotting phenomenon so as to achieve the high-efficiency crease-resist effect of the crease-resist agent.
2. The method disclosed by the application is simple in process and convenient to operate, and particularly the obtained modified glycoside sulfonate not only has the relevant properties of the nonionic surfactant alkyl glycoside, but also has good lubricating performance, and meanwhile, the water solubility of the product is improved due to the introduction of sulfonate ions, so that the problems that the long-carbon-chain alkyl glycoside is poor in water solubility, easy to separate out at low temperature and the like are solved, and meanwhile, the auxiliary disclosed by the application is environment-friendly.
3. The dye prepared by the application has good dye-uptake and color fastness, and also has good draping property and crease resistance.
Detailed Description
The above summary of the present application is described in further detail below in conjunction with the detailed description, but it should not be understood that the scope of the above-described subject matter of the present application is limited to the following examples.
Introduction of partial raw materials in the application:
the indigo of the examples was purchased from texas gevarious chemical products limited.
In the examples, polyoxyethylene sorbitan monooleate was purchased from Jinan navigation chemical engineering Co., ltd., model: t-80, cargo number: 383.
in the examples, polyethylene is purchased from Yuyao Jioding chemical materials Co., ltd., model: U-PE350, density: 0.947g/cm 3 。
Polyether modified silicone oil in examples, CAS number: 67674-67-3, available from Jinan Haoyan chemical technology Co., ltd., viscosity: 2000mpa.S at 25 ℃.
In the examples, the isomeric tridecanol polyoxyethylene ether, CAS number: 9043-30-5.
Isobornyl acetate, CAS number: 125-12-2.
1,3,5, 7-tetramethyl-1, 3,5, 7-tetravinyl cyclotetrasilazane in the examples, CAS number: 5162-63-0.
Sodium 3-chloro-2-hydroxypropyl sulfonate, CAS number: 126-83-0.
In the examples vinyltris (2-methoxyethoxy) silane, CAS number: 1067-53-4.
The commercially available wrinkle resistant agent in the examples was purchased from the silicone technology Co.Ltd, jia Honda, dongguan, model: goon906, cat number: 906, type: and (3) non-ionic.
Example 1
An environment-friendly clothing dye is prepared from 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, 10 parts by weight of 3-chloro-2-hydroxypropyl trimethyl ammonium 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 carboxymethyl cellulose and 3 parts by weight of a crease-resist agent. The anti-wrinkling agent is a commercially available anti-wrinkling agent.
Example 2
An environment-friendly clothing dye is prepared from 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, 10 parts by weight of 3-chloro-2-hydroxypropyl trimethyl ammonium 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 carboxymethyl cellulose and 3 parts by weight of a crease-resist agent.
The preparation method of the crease-resist agent comprises the following steps: 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 are mixed, and stirred at 90 ℃ and 800rpm for 6 minutes to obtain a base solution of the crease-resist agent; 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 a speed of 15 ℃/min to obtain the crease-resist agent.
Example 3
An environment-friendly clothing dye is prepared from 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, 10 parts by weight of 3-chloro-2-hydroxypropyl trimethyl ammonium 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 carboxymethyl cellulose, 3 parts by weight of an anti-wrinkling agent and 3 parts by weight of an auxiliary agent.
The preparation method of the crease-resist agent comprises the following steps: 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 are mixed, and stirred at 90 ℃ and 800rpm for 6 minutes to obtain a base solution of the crease-resist agent; 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 a speed of 15 ℃/min to obtain the crease-resist 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 the 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 octamethyl cyclotetrasiloxane, 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) -tetramethyl disiloxane, continuously reacting for 2 hours, and then distilling under reduced pressure for 1 hour at 70 ℃ to obtain epoxy amino silicone oil;
s3, dissolving 10 parts by weight of epoxy amino silicone oil and 0.2 part by weight of glycoside into 20 parts by weight of N-methylpyrrolidone, adding 2 parts by weight of 2wt% boron trifluoride diethyl ether solution into the mixture, reacting for 6 hours at 80 ℃ and 400rpm, and distilling under reduced pressure at 70 ℃ until the solvent N-methylpyrrolidone is completely removed to obtain an auxiliary agent; the glycoside is butyl glycoside.
Comparative example 1
Substantially the same as in example 3, except that the auxiliary agent was prepared 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 at 65 ℃ and 500rpm for reaction for 6 hours, evaporating and concentrating at 90 ℃ to 1/6 of the 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 octamethyl cyclotetrasiloxane, 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) -tetramethyl disiloxane, continuously reacting for 2 hours, and then distilling under reduced pressure for 1 hour at 70 ℃ to obtain the auxiliary agent.
Example 4
An environment-friendly clothing dye is prepared from 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, 10 parts by weight of 3-chloro-2-hydroxypropyl trimethyl ammonium 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 carboxymethyl cellulose, 3 parts by weight of an anti-wrinkling agent and 3 parts by weight of an auxiliary agent.
The preparation method of the crease-resist agent comprises the following steps: 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 are mixed, and stirred at 90 ℃ and 800rpm for 6 minutes to obtain a base solution of the crease-resist agent; 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 a speed of 15 ℃/min to obtain the crease-resist 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 the 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 octamethyl cyclotetrasiloxane, 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) -tetramethyl disiloxane, continuously reacting for 2 hours, and then distilling under reduced pressure for 1 hour at 70 ℃ to obtain epoxy amino silicone oil;
s3, 10 parts by weight of epoxy amino silicone oil and 0.2 part by weight of glycoside are taken and dissolved in 20 parts by weight of N-methyl pyrrolidone, 2 parts by weight of 2wt% boron trifluoride diethyl ether solution is added into the mixture to react for 6 hours at 80 ℃ and 400rpm, and the mixture is distilled under reduced pressure at 70 ℃ until the solvent N-methyl pyrrolidone is completely removed, so that the auxiliary agent is obtained.
The glycoside is a modified glycoside; the preparation method of the modified glycoside comprises the following steps: 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 are mixed and reacted for 4 hours at 100 ℃ and 1000rpm, 8 parts by weight of modifier, 6 parts by weight of acrylamide and 1 part by weight of 30wt% sodium hydroxide ethanol solution are added and stirred for 20 minutes at 1000 rpm; adjusting the pH value to be 10 by using a 2mol/L sodium hydroxide aqueous solution, adding 0.2 part by weight of ammonium cerium nitrate, and reacting for 5 hours at 110 ℃ to obtain modified glycoside; the modifier is 3-chlorine-2-hydroxypropyl sodium sulfonate.
Example 5
Substantially the same as in example 4, except that the modifier was vinyltris (2-methoxyethoxy) silane.
Example 6
Substantially the same as in example 4, except that the modifier consisted of sodium 3-chloro-2-hydroxypropyl sulfonate and vinyltris (2-methoxyethoxy) silane in a mass ratio of 2:3.
Test example 1
The environment-friendly garment dye pair fabric prepared in examples 1-6 (100% nylon fabric, gram weight 160g/m 2 ) Dyeing is performed. Immersing the fabric into environment-friendly clothing dye, wherein the bath ratio is 1g:30mL, heating to 60 ℃ at the speed of 2 ℃/min, heating to 80 ℃ at the speed of 1 ℃/min, heating to 100 ℃ at the speed of 0.8 ℃/min, preserving heat for 50min, taking out, and rolling to obtain the dyed fabric, wherein the rolling surplus rate is 45%; immersing the dyed fabric into water at 35 ℃ for washing, wherein the bath ratio is 1g to 20mL, and preserving the heat for 10min; and taking out and drying to obtain a finished fabric, and testing the finished fabric as follows.
1. Rubbing color fastness test: the test is carried out by referring to national standard GB/T3920-2008 "rubbing fastness to textile color fastness test", the finished fabric is subjected to humidity control for 6 hours under the conditions of 20 ℃ and 65% relative humidity before the test, the test is carried out for 4 times in parallel, and the average value is obtained.
2. Water fastness test: the test is carried out by referring to national standard GB/T5713-2013 "textile color fastness test Water fastness", the finished fabric is subjected to humidity control for 6 hours under the condition that the temperature is 20 ℃ and the relative humidity is 65% before the test, the test is carried out for 4 times in parallel, and the average value is obtained.
3. And (3) testing the coloring rate: the test is carried out by referring to the national standard GB/T9337-2009 determination of high-temperature dyeing and coloring rate of disperse dyes, the test is carried out for 4 times in parallel, and the average value is obtained.
TABLE 1 test results of rubbing color fastness, water-fast color fastness and color Rate
From the results of table 1, it is apparent that the dye added with the self-made anti-wrinkling agent of the present application can improve the dyeing degree and color fastness of the fabrics to some extent, because the anti-wrinkling agent can effectively reduce friction between fabrics and equipment, and reduce scratches or streaks of fabrics during wet processing, thereby improving tight connectivity between fabrics and improving the dyeing degree of fabrics. The addition of the auxiliary agent in the dye can further improve the color fastness and the coloring rate of the fabric, 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, thereby improving the color fixing rate and the coloring rate of the fabric. In the embodiment 6, the modifier is compounded by 3-chloro-2-hydroxypropyl sodium sulfonate and vinyl tri (2-methoxyethoxy) silane, so that the fixation rate and color fastness of the fabric can be further improved, the 3-chloro-2-hydroxypropyl sodium sulfonate can improve the water solubility of the dye, the vinyl tri (2-methoxyethoxy) silane can improve the oil solubility of the dye, the two can be synergistically used, and an organosilicon functional group with an adhesive force effect and an amino and sulfonic acid group with a hydrophilic group are introduced, so that the glucoside 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) overhang coefficient test: the finished fabric of test example 1 was tested with reference to national standard GB/T23329-2009 determination of textile fabric drape, and the finished fabric was subjected to parallel testing 4 times under conditions of 20℃and 65% relative humidity for 24 hours before the test, and the average value was obtained.
TABLE 2 results of drape coefficient test
As can be seen from the results in Table 2, the addition of the self-made anti-wrinkling agent of the present application can improve the drape performance of the fabric to a certain extent, because the anti-wrinkling agent can effectively reduce friction between the fabric and the fabric, between the fabric and the equipment, and reduce scratches or streaks of the fabric during wet processing, thereby improving the tight connectivity between the fabric and the fabric, thereby improving the drape performance of the fabric, and the addition of the auxiliary agent can further improve the drape performance of the fabric.
Test example 3
Crease recovery test: the finished fabric of test example 1 was tested with reference to national standard GB/T3819-1997 method for determining recovery angle of fold recovery of textile fabrics, and the finished fabric was subjected to humidity control for 6 hours at a temperature of 20℃and a relative humidity of 65% before the test, a test temperature of 35℃and a test relative humidity of 90% and a test load: 10N, subjected to a pressure event for 5min, tested 4 times in parallel, and averaged.
TABLE 3 results of the crease recovery test
As can be seen from the test data in Table 3, the crease recovery angle of the fabric treated with the self-made crease-resist dye of the application is significantly improved compared with the fabric treated with the commercially available crease-resist dye, and the crease recovery angle of the fabric is not greatly affected after the addition of the auxiliary agent, so that the crease resistance is still good.
Claims (3)
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 vegetable 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 resist and 1-5 parts of auxiliary agent;
the preparation method of the crease-resist 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 600-1000rpm for 5-10min to obtain a base solution of the crease-resist agent; cooling to 60-80deg.C, adding 0.5-1 weight parts of N, N-dimethylethanolamine and 0.5-1 weight parts of linoleic acid diethanolamide, stirring for 20-30min, and cooling to room temperature at a speed of 10-18deg.C/min to obtain crease-resist 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 the S1, and adding sodium hydroxide and dimethyl sulfoxide for reaction to obtain epoxy amino silicone oil;
s3, dissolving epoxy amino silicone oil and glycoside in the S2 in N-methyl pyrrolidone, and adding boron trifluoride diethyl ether solution for reaction to obtain an auxiliary agent;
the glycoside is a modified glycoside; the preparation method of the modified glycoside comprises the following steps: 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 2-6 hours at 80-110 ℃ and 800-1200rpm, adding 5-10 parts by weight of modifier, 3-8 parts by weight of acrylamide and 0.5-3 parts by weight of 20-40wt% sodium hydroxide ethanol solution, and stirring for 10-30 minutes at 600-1200 rpm; regulating the pH to 9-11 by using 1-3mol/L sodium hydroxide aqueous solution, adding 0.1-1 weight part of ammonium cerium nitrate, and reacting for 4-7 hours at 90-130 ℃ to obtain modified glycoside; the modifier is 3-chlorine-2-hydroxypropyl sodium sulfonate and/or vinyl tri (2-methoxyethoxy) silane;
the vegetable dye is one or more of indigo, gardenia yellow and turmeric;
the penetrating agent is one or more than two of sodium alkyl sulfonate, sodium secondary alkyl sulfate, isooctyl alcohol polyoxyethylene ether phosphate sodium salt, sulfated castor oil and phosphate compounds; the dispersing agent is sodium lignin sulfonate or sodium carboxymethyl cellulose.
2. The environment-friendly clothing dye according to claim 1, wherein the modifier is prepared from 3-chlorine-2-hydroxypropyl sodium sulfonate and vinyltris (2-methoxyethoxy) silane according to the mass ratio of (1-3): (1-5).
3. Use of the environmentally friendly garment dye of claim 1 or 2 in garment printing and dyeing.
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