WO2019006940A1 - 一种用于纺织品的人工复合染色剂及其制备方法 - Google Patents

一种用于纺织品的人工复合染色剂及其制备方法 Download PDF

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WO2019006940A1
WO2019006940A1 PCT/CN2017/109633 CN2017109633W WO2019006940A1 WO 2019006940 A1 WO2019006940 A1 WO 2019006940A1 CN 2017109633 W CN2017109633 W CN 2017109633W WO 2019006940 A1 WO2019006940 A1 WO 2019006940A1
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parts
textiles
sodium
artificial composite
agent
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PCT/CN2017/109633
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English (en)
French (fr)
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蔡国强
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苏州市晨彩纺织研发有限公司
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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
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
    • 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
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/006—Preparation of organic pigments
    • 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
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0092—Dyes in solid form

Definitions

  • the invention relates to the field of dyeing agents, in particular to an artificial composite dyeing agent for textiles and a preparation method thereof.
  • Textile dyes are a dye used in textile dyeing. Usually plant extracts such as plant fruits and sap also contain natural chemical extracts such as coal tar. Divided into natural dyes and synthetic dyes, mostly synthetic dyes on the market. The color of the dye and its affinity to the tissue are determined by the molecular structure of the dye itself, and the color-forming chromophore and the color-promoting group that produces affinity with the tissue determine the dyeing properties of the dye. Most of the existing dyes on the market have insufficient dye affinity, and in the high temperature and acid-base environment, the leveling property is poor and fading is likely to occur. At the same time, the dyed fabrics are more fading during long-term washing and drying, and the dyeing is not strong enough to meet the people's requirements for color. Moreover, even after the fixing of the general chemical dye, it is easy to fade after repeated washing. Therefore, the present invention utilizes natural plant stains to develop a composite dye having a more stable and safe performance to cope with market and industry development.
  • the present invention provides an artificial composite coloring agent for textiles and a preparation method thereof, which are obtained by combining specific materials and combining corresponding production processes to obtain an artificial composite coloring agent for textiles. Stable and easy to dye, safe and non-irritating to human body, able to meet the requirements of the industry, with good application prospects.
  • An artificial composite dye for textiles made from the following raw materials: natural dyes 30-50 parts of raw materials, 2-3 parts of organic dyeing raw materials, 5-10 parts of butyl methacrylate, 8-10 parts of hydroxypropylmethylcellulose, 7-10 parts of dimethicone diquaternary ammonium salt 5-8 parts of paraffin, 4-8 parts of coconut oil fatty acid diethanolamide, 1-2 parts of octylphenol polyoxyethylene ether, 2-5 parts of citric acid, 1-3 parts of sodium thiosulfate, phthalic acid 1-4 parts of dibutyl ester, 6-12 parts of ethoxylated alkyl ammonium sulfate, 1-2 parts of vinyl sulfone, 2-3 parts of sodium ascorbate, 1-3 parts of erythritol, disodium edetate 1-3 parts, 1-2 parts of chitosan polysaccharide, 1-2 parts of citronellonitrile, 2-5 parts of coupling agent, and 1-4 parts of auxiliary
  • the natural dye raw material is one or more of indigo, indigo, valerian, turmeric, comfrey, gentian, valerian, impatiens, yam, and gallnut.
  • the coupling agent is ⁇ -aminopropyltrimethoxysilane, vinyltriethoxysilane, vinyltris( ⁇ -methoxyethoxy)silane, 3-aminopropyltrimethoxy Any of silanes.
  • the auxiliary agent is selected from any one or more of citric acid, neopentyl glycol, tartaric acid, and sodium lignosulfonate.
  • the preparation method of the artificial composite coloring agent for textiles comprises the following steps:
  • step (3) Dissolving the powder in step (2) in an equal volume of deionized water, ultrasonically dispersing, ultrasonic time is 50 minutes, ultrasonic frequency is 220-250 KW;
  • butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid diethanolamide, octylphenol polyoxyethylene ether, citric acid, sulfur Sulfur Sodium salt, dibutyl phthalate, coupling agent, auxiliary agent are injected into the reaction kettle, mixed and stirred, the stirring speed is 150-200 rpm, the reaction time is 40 minutes, and the reaction temperature is 185-200 ° C;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • the inert gas is nitrogen.
  • the invention has the following beneficial effects:
  • the artificial composite coloring agent for textiles of the present invention which is a natural dye raw material, butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid Diethanolamide, octylphenol polyoxyethylene ether, citric acid, sodium thiosulfate, dibutyl phthalate as main components, by adding organic dyeing raw materials, ethoxylated alkyl ammonium sulfate, vinyl sulfone, ascorbic acid Sodium, erythritol, disodium edetate, chitosan polysaccharide, citronellonitrile, coupling agent, auxiliary agent, supplemented by grinding, ultrasonic dispersion, pressure distillation, stirring reaction, cooling
  • the process of foaming, compressive spraying and the like makes the prepared artificial composite dyeing agent for textiles stable and easy to dye, safe and non-irritating to the human body,
  • the artificial composite dyeing agent for textiles of the invention is cheap, simple in process, suitable for large-scale industrial application, and has strong practicability.
  • butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid diethanolamide, octylphenol polyoxyethylene ether, citric acid, sulfur Sodium sulfate, dibutyl phthalate, ⁇ -aminopropyltrimethoxysilane, citric acid were injected into the reaction vessel, mixed and stirred, the stirring speed was 150 rpm, the reaction time was 40 minutes, and the reaction temperature was 185. °C;
  • step (7) adding the condensed filtrate of step (4) and the organic dye to the cooled product of step (6)
  • Material ethoxylated ammonium alkyl sulfate, vinyl sulfone, sodium ascorbate, erythritol, disodium edetate, chitosan polysaccharide, citronellin, evenly mixed, injected into the foaming machine, fully bulged Foaming, let stand for 30 minutes;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • step (3) dissolving the powder in step (2) in an equal volume of deionized water, ultrasonically dispersing, ultrasonic time is 50 minutes, ultrasonic frequency is 230 KW;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • step (3) (4) heating the ultrasonic dispersion mixture of step (3) to 45 ° C, and then adding an equal volume of no Water ethanol, pressurized distillation to obtain a condensed filtrate;
  • butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid diethanolamide, octylphenol polyoxyethylene ether, citric acid, sulfur Sodium sulfate, dibutyl phthalate, vinyl tris( ⁇ -methoxyethoxy)silane, and tartaric acid were injected into the reaction vessel, stirred and stirred at a stirring rate of 190 rpm, and the reaction time was 40 minutes.
  • the reaction temperature is 195 ° C;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • step (3) Dissolving the powder in step (2) in an equal volume of deionized water, ultrasonically dispersing, ultrasonic time is 50 minutes, ultrasonic frequency is 250 KW;
  • butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid diethanolamide, octylphenol polyoxyethylene ether, citric acid, sulfur Sodium sulfate, dibutyl phthalate, 3-aminopropyltrimethoxysilane, sodium lignin sulfonate were injected into the reaction vessel, mixed and stirred, the stirring speed was 200 rpm, and the reaction time was 40 minutes.
  • the temperature is 200 ° C;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • step (7) adding the condensed filtrate and the organic dyeing raw material of the step (4), the ethoxylated alkyl ammonium sulfate, sodium ascorbate, erythritol, disodium edetate, and the dehydrated product to the step (6).
  • the acetyl chitosan polysaccharide and the citronella nitrile are uniformly mixed, injected into the foaming machine, fully foamed, and allowed to stand for 30 minutes;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • step (3) Dissolving the powder in step (2) in an equal volume of deionized water, ultrasonically dispersing, ultrasonic time is 50 minutes, ultrasonic frequency is 250 KW;
  • butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid diethanolamide, octylphenol polyoxyethylene ether, citric acid, neighbor Dibutyl phthalate, 3-aminopropyltrimethoxysilane, sodium lignin sulfonate was injected into the reaction vessel, mixed and stirred, the stirring speed was 200 rpm, the reaction time was 40 minutes, and the reaction temperature was 200 ° C;
  • step (7) adding the condensed filtrate of the step (4) and the organic dyeing raw material, the ethoxylated alkyl ammonium sulfate, the vinyl sulfone, the sodium ascorbate, the disodium edetate, and the deacetylation to the cooled product of the step (6).
  • the chitosan polysaccharide and the citronella nitrile are uniformly mixed, injected into the foaming machine, fully foamed, and allowed to stand for 30 minutes;
  • the mixed liquid in the step (7) is filtered, and the spray is compressed to obtain a powdery dye product, which can be dispensed.
  • the artificial composite dyes for textiles prepared in Examples 1-4 and Comparative Examples 1-2 were subjected to several performance tests of soaping fastness, rubbing fastness, perspiration fastness and sensitization reaction.
  • Artificial composite dyeing agent for textiles of the invention using natural dye raw material, butyl methacrylate, hydroxypropyl methylcellulose, polydimethylsiloxane diquaternary ammonium salt, paraffin wax, coconut oil fatty acid diethanolamide , octylphenol ethoxylate, citric acid, sodium thiosulfate, dibutyl phthalate as the main component, by adding organic dyeing raw materials, ethoxylated ammonium alkyl sulfate, vinyl sulfone, sodium ascorbate, red Sterol, disodium edetate, chitosan polysaccharide, citronellonitrile, coupling agent, auxiliary agent, supplemented by grinding, ultrasonic dispersion, pressure distillation, stirring reaction, cooling foaming, compression Spray and other processes make the artificial composite dyeing agent for textiles stable, easy to dye, safe and non-irritating to human body, able to meet the requirements of the industry, and have a good application

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Coloring (AREA)

Abstract

提供一种用于纺织品的人工复合染色剂及其制备方法，由下列重量份的原料制成：天然染料原材料30-50份、有机染色原料2-3份、甲基丙烯酸丁酯5-10份、羟丙基甲基纤维素8-10份、聚二甲基硅氧烷二季胺盐7-10份、石蜡5-8份、椰子油脂肪酸二乙醇酰胺4-8份、辛基酚聚氧乙烯醚1-2份、鞣酸2-5份、硫代硫酸钠1-3份、邻苯二甲酸二丁酯1-4份、乙氧基化烷基硫酸铵6-12份、乙烯砜1-2份、抗坏血酸钠2-3份、赤藓醇1-3份、乙二胺四乙酸二钠1-3份、脱乙酰壳聚糖多糖1-2份、香茅腈1-2份、偶联剂2-5份、助剂1-4份。制备而成的用于纺织品的人工复合染色剂，其性能稳定易于染色、对人体安全无刺激。

Description

一种用于纺织品的人工复合染色剂及其制备方法 技术领域
本发明涉及染色剂领域，特别涉及到一种用于纺织品的人工复合染色剂及其制备方法。
背景技术
纺织染料是用于纺织品染色的一种染剂。多为植物果实，树液等植物提取物，也含有煤焦油等天然化学物质提取物。分为天然染料和合成染料，市面上多为合成染料。染料的颜色和它与组织间的亲和力是由染料本身的分子结构决定的，产生颜色的发色基团和与组织间产生亲和力的助色基团共同决定了染色剂的染色性质。现有的市场上的大部分的染料亲和力不够，在高温和酸碱的环境下，造成匀染性差同时容易发生褪色现象。同时染色出来的织物在长期的洗涤日晒过程中，褪色较为明显，染色不牢固，适应不了人们对色彩的要求。而且一般的化工染料即使经过固色后，经多次水洗仍容易褪色。所以本发明利用天然的植物染色剂研制出性能更加稳定安全的复合染色剂来应对市场和行业的发展。
发明内容
为解决上述技术问题，本发明提供一种用于纺织品的人工复合染色剂及其制备方法，通过采用特定原料进行组合，配合相应的生产工艺，得到的用于纺织品的人工复合染色剂，其性能稳定易于染色、对人体安全无刺激，能够满足行业的要求，具有较好的应用前景。
本发明的目的可以通过以下技术方案实现：
用于纺织品的人工复合染色剂，由下列重量份的原料制成：天然染料 原材料30-50份、有机染色原料2-3份、甲基丙烯酸丁酯5-10份、羟丙基甲基纤维素8-10份、聚二甲基硅氧烷二季胺盐7-10份、石蜡5-8份、椰子油脂肪酸二乙醇酰胺4-8份、辛基酚聚氧乙烯醚1-2份、鞣酸2-5份、硫代硫酸钠1-3份、邻苯二甲酸二丁酯1-4份、乙氧基化烷基硫酸铵6-12份、乙烯砜1-2份、抗坏血酸钠2-3份、赤藓醇1-3份、乙二胺四乙酸二钠1-3份、脱乙酰壳聚糖多糖1-2份、香茅腈1-2份、偶联剂2-5份、助剂1-4份。
优选地，所述天然染料原材料为蓼蓝、菘蓝、荩草、姜黄、紫草、龙胆、茜草、凤仙花、薯莨、五倍子中的一种或几种。
优选地，所述偶联剂为γ-氨丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷、3-氨丙基三甲氧基硅烷中的任意一种。
优选地，所述助剂选自柠檬酸、新戊二醇、酒石酸、木质素磺酸钠中的任意一种或几种。
所述的用于纺织品的人工复合染色剂的制备方法，包括以下步骤：
(1)按照重量份称取各原料；
(2)将天然染料原材料洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为220-250KW；
(4)将步骤(3)的超声分散混合物加热至30-50℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫 酸钠、邻苯二甲酸二丁酯、偶联剂、助剂注入反应釜中，混合搅拌，搅拌速度为150-200转/分钟，反应时间为40分钟，反应温度为185-200℃；
(6)将步骤(5)中的反应物至于惰性气体环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
优选地，所述惰性气体为氮气。
本发明与现有技术相比，其有益效果为：
(1)本发明的用于纺织品的人工复合染色剂，以天然染料原材料、甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯为主要成分，通过加入有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈、偶联剂、助剂，辅以研磨过筛、超声分散、加压蒸馏、搅拌反应、冷却发泡、压缩喷雾等工艺，使得制备而成的用于纺织品的人工复合染色剂，其性能稳定易于染色、对人体安全无刺激，能够满足行业的要求，具有较好的应用前景。
(2)本发明的用于纺织品的人工复合染色剂原料廉价、工艺简单，适于大规模工业化运用，实用性强。
具体实施方式
下面结合具体实施例对发明的技术方案进行详细说明。
实施例1
(1)按照重量份称取蓼蓝10份、菘蓝35份、有机染色原料2份、甲基丙烯酸丁酯5份、羟丙基甲基纤维素8份、聚二甲基硅氧烷二季胺盐7份、石蜡5份、椰子油脂肪酸二乙醇酰胺4份、辛基酚聚氧乙烯醚1份、鞣酸2份、硫代硫酸钠1份、邻苯二甲酸二丁酯1份、乙氧基化烷基硫酸铵6份、乙烯砜1份、抗坏血酸钠2份、赤藓醇1份、乙二胺四乙酸二钠1份、脱乙酰壳聚糖多糖1份、香茅腈1份、γ-氨丙基三甲氧基硅烷2份、柠檬酸1份；
(2)将蓼蓝、菘蓝洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为220KW；
(4)将步骤(3)的超声分散混合物加热至30℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯、γ-氨丙基三甲氧基硅烷、柠檬酸注入反应釜中，混合搅拌，搅拌速度为150转/分钟，反应时间为40分钟，反应温度为185℃；
(6)将步骤(5)中的反应物至于氮气环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原 料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
制得的用于纺织品的人工复合染色剂的性能测试结果如表1所示。
实施例2
(1)按照重量份称取荩草20份、姜黄20份、有机染色原料2份、甲基丙烯酸丁酯7份、羟丙基甲基纤维素9份、聚二甲基硅氧烷二季胺盐8份、石蜡6份、椰子油脂肪酸二乙醇酰胺5份、辛基酚聚氧乙烯醚1份、鞣酸3份、硫代硫酸钠2份、邻苯二甲酸二丁酯2份、乙氧基化烷基硫酸铵8份、乙烯砜1份、抗坏血酸钠2份、赤藓醇2份、乙二胺四乙酸二钠2份、脱乙酰壳聚糖多糖1份、香茅腈1份、乙烯基三乙氧基硅烷3份、新戊二醇2份；
(2)将荩草、姜黄洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为230KW；
(4)将步骤(3)的超声分散混合物加热至35℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯、乙烯基三乙氧基硅烷、新戊二醇注入反应釜中， 混合搅拌，搅拌速度为160转/分钟，反应时间为40分钟，反应温度为190℃；
(6)将步骤(5)中的反应物至于氮气环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
制得的用于纺织品的人工复合染色剂的性能测试结果如表1所示。
实施例3
(1)按照重量份称取紫草30份、龙胆15份、有机染色原料3份、甲基丙烯酸丁酯9份、羟丙基甲基纤维素9份、聚二甲基硅氧烷二季胺盐9份、石蜡7份、椰子油脂肪酸二乙醇酰胺7份、辛基酚聚氧乙烯醚2份、鞣酸4份、硫代硫酸钠2份、邻苯二甲酸二丁酯3份、乙氧基化烷基硫酸铵10份、乙烯砜2份、抗坏血酸钠3份、赤藓醇3份、乙二胺四乙酸二钠3份、脱乙酰壳聚糖多糖2份、香茅腈1份、乙烯基三(β-甲氧基乙氧基)硅烷4份、酒石酸3份；
(2)将紫草、龙胆洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为240KW；
(4)将步骤(3)的超声分散混合物加热至45℃，再加入等体积的无 水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯、乙烯基三(β-甲氧基乙氧基)硅烷、酒石酸注入反应釜中，混合搅拌，搅拌速度为190转/分钟，反应时间为40分钟，反应温度为195℃；
(6)将步骤(5)中的反应物至于氮气环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
制得的用于纺织品的人工复合染色剂的性能测试结果如表1所示。
实施例4
(1)按照重量份称取茜草10份、凤仙花10份、薯莨15份、五倍子15份、有机染色原料3份、甲基丙烯酸丁酯10份、羟丙基甲基纤维素10份、聚二甲基硅氧烷二季胺盐10份、石蜡8份、椰子油脂肪酸二乙醇酰胺8份、辛基酚聚氧乙烯醚2份、鞣酸5份、硫代硫酸钠3份、邻苯二甲酸二丁酯4份、乙氧基化烷基硫酸铵12份、乙烯砜2份、抗坏血酸钠3份、赤藓醇3份、乙二胺四乙酸二钠3份、脱乙酰壳聚糖多糖2份、香茅腈2份、3-氨丙基三甲氧基硅烷5份、木质素磺酸钠4份；
(2)将茜草、凤仙花、薯莨、五倍子洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为250KW；
(4)将步骤(3)的超声分散混合物加热至50℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯、3-氨丙基三甲氧基硅烷、木质素磺酸钠注入反应釜中，混合搅拌，搅拌速度为200转/分钟，反应时间为40分钟，反应温度为200℃；
(6)将步骤(5)中的反应物至于氮气环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
制得的用于纺织品的人工复合染色剂的性能测试结果如表1所示。
对比例1
(1)按照重量份称取蓼蓝10份、菘蓝35份、有机染色原料2份、甲基丙烯酸丁酯5份、羟丙基甲基纤维素8份、聚二甲基硅氧烷二季胺盐7 份、石蜡5份、椰子油脂肪酸二乙醇酰胺4份、鞣酸2份、硫代硫酸钠1份、邻苯二甲酸二丁酯1份、乙氧基化烷基硫酸铵6份、抗坏血酸钠2份、赤藓醇1份、乙二胺四乙酸二钠1份、脱乙酰壳聚糖多糖1份、香茅腈1份、γ-氨丙基三甲氧基硅烷2份、柠檬酸1份；
(2)将蓼蓝、菘蓝洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为220KW；
(4)将步骤(3)的超声分散混合物加热至30℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯、γ-氨丙基三甲氧基硅烷、柠檬酸注入反应釜中，混合搅拌，搅拌速度为150转/分钟，反应时间为40分钟，反应温度为185℃；
(6)将步骤(5)中的反应物至于氮气环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
制得的用于纺织品的人工复合染色剂的性能测试结果如表1所示。
对比例2
(1)按照重量份称取茜草10份、凤仙花10份、薯莨15份、五倍子15份、有机染色原料3份、甲基丙烯酸丁酯10份、羟丙基甲基纤维素10份、聚二甲基硅氧烷二季胺盐10份、石蜡8份、椰子油脂肪酸二乙醇酰胺8份、辛基酚聚氧乙烯醚2份、鞣酸5份、邻苯二甲酸二丁酯4份、乙氧基化烷基硫酸铵12份、乙烯砜2份、抗坏血酸钠3份、乙二胺四乙酸二钠3份、脱乙酰壳聚糖多糖2份、香茅腈2份、3-氨丙基三甲氧基硅烷5份、木质素磺酸钠4份；
(2)将茜草、凤仙花、薯莨、五倍子洗净、干燥、研磨至粉末，过300目筛；
(3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为250KW；
(4)将步骤(3)的超声分散混合物加热至50℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
(5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、邻苯二甲酸二丁酯、3-氨丙基三甲氧基硅烷、木质素磺酸钠注入反应釜中，混合搅拌，搅拌速度为200转/分钟，反应时间为40分钟，反应温度为200℃；
(6)将步骤(5)中的反应物至于氮气环境下冷却至室温；
(7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
(8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
制得的用于纺织品的人工复合染色剂的性能测试结果如表1所示。
将实施例1-4和对比例1-2的制得的用于纺织品的人工复合染色剂进行皂洗牢度、摩擦牢度、汗渍牢度和致敏反应这几项性能测试。
表1
Figure PCTCN2017109633-appb-000001
本发明的用于纺织品的人工复合染色剂，以天然染料原材料、甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯为主要成分，通过加入有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈、偶联剂、助剂，辅以研磨过筛、超声分散、加压蒸馏、搅拌反应、冷却发泡、压缩喷雾等工艺，使得制备而成的用于纺织品的人工复合染色剂，其性能稳定易于染色、对人体安全无刺激，能够满足行业的要求，具有较好的应用前景。本发明的用于纺织品的人工复合染色剂原料廉价、工艺简单，适于大规模工业化运用，实用性强。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (6)

  1. 一种用于纺织品的人工复合染色剂，其特征在于：由下列重量份的原料制成：天然染料原材料30-50份、有机染色原料2-3份、甲基丙烯酸丁酯5-10份、羟丙基甲基纤维素8-10份、聚二甲基硅氧烷二季胺盐7-10份、石蜡5-8份、椰子油脂肪酸二乙醇酰胺4-8份、辛基酚聚氧乙烯醚1-2份、鞣酸2-5份、硫代硫酸钠1-3份、邻苯二甲酸二丁酯1-4份、乙氧基化烷基硫酸铵6-12份、乙烯砜1-2份、抗坏血酸钠2-3份、赤藓醇1-3份、乙二胺四乙酸二钠1-3份、脱乙酰壳聚糖多糖1-2份、香茅腈1-2份、偶联剂2-5份、助剂1-4份。
  2. 根据权利要求1所述的用于纺织品的人工复合染色剂，其特征在于：所述天然染料原材料为蓼蓝、菘蓝、荩草、姜黄、紫草、龙胆、茜草、凤仙花、薯莨、五倍子中的一种或几种。
  3. 根据权利要求1所述的用于纺织品的人工复合染色剂，其特征在于：所述偶联剂为γ-氨丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷、3-氨丙基三甲氧基硅烷中的任意一种。
  4. 根据权利要求1所述的用于纺织品的人工复合染色剂，其特征在于：所述助剂选自柠檬酸、新戊二醇、酒石酸、木质素磺酸钠中的任意一种或几种。
  5. 根据权利要求1～4任一所述的用于纺织品的人工复合染色剂的制备方法，其特征在于，包括以下步骤：
    (1)按照重量份称取各原料；
    (2)将天然染料原材料洗净、干燥、研磨至粉末，过300目筛；
    (3)将步骤(2)中的粉末溶于等体积的去离子水中，超声分散，超声时间为50分钟，超声频率为220-250KW；
    (4)将步骤(3)的超声分散混合物加热至30-50℃，再加入等体积的无水乙醇，加压蒸馏，得到冷凝的滤液；
    (5)将甲基丙烯酸丁酯、羟丙基甲基纤维素、聚二甲基硅氧烷二季胺盐、石蜡、椰子油脂肪酸二乙醇酰胺、辛基酚聚氧乙烯醚、鞣酸、硫代硫酸钠、邻苯二甲酸二丁酯、偶联剂、助剂注入反应釜中，混合搅拌，搅拌速度为150-200转/分钟，反应时间为40分钟，反应温度为185-200℃；
    (6)将步骤(5)中的反应物至于惰性气体环境下冷却至室温；
    (7)往步骤(6)的冷却物中加入步骤(4)的冷凝滤液和有机染色原料、乙氧基化烷基硫酸铵、乙烯砜、抗坏血酸钠、赤藓醇、乙二胺四乙酸二钠、脱乙酰壳聚糖多糖、香茅腈混合均匀，注入发泡机，充分鼓起发泡，静置30分钟；
    (8)将步骤(7)中的混合液过滤，压缩喷雾，得到粉末状的染料成品，分装即可。
  6. 根据权利要求5所述的用于纺织品的人工复合染色剂的制备方法，其特征在于：所述惰性气体为氮气。
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