CN107044055B - A method for dyeing cotton fabric with carmine with less water - Google Patents
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Abstract
本发明属于天然染料染色方法技术领域，具体涉及一种胭脂虫红素少水染色棉织物的方法。本发明方法包括：a、配制整理液：取壳聚糖，加冰醋酸，搅拌，得到壳聚糖稀释整理液；b、棉织物整理：将棉织物按1:30浴比浸入壳聚糖整理液中，加交联剂，采用二浸二轧处理，在酸中和环境中放置，水洗，烘焙，得到壳聚糖改性棉织物；c、配制染液：将胭脂虫红素溶解于有机溶剂和水的混合溶液中，搅拌，得到染液；d、染色：将壳聚糖改性棉织物按1：30浴比置于染液中，水洗，干燥，即得。本发明通过对棉织物进行壳聚糖改性处理，采用有机溶剂体系进行染色，减少了染色废水的排放，提高了棉织物的拒水性能，提高了胭脂虫红素对棉织物的上染率和色牢度。The invention belongs to the technical field of dyeing methods of natural dyes, and in particular relates to a method for dyeing cotton fabrics with cochineal with less water. The method of the present invention comprises: a, preparation finishing liquid: take chitosan, add glacial acetic acid, stir, obtain chitosan dilution finishing liquid; b, cotton fabric finishing: immerse cotton fabric by 1:30 liquor ratio chitosan finishing In the solution, add a crosslinking agent, adopt two dipping and two rolling treatments, place in an acid neutral environment, wash with water, and bake to obtain a chitosan modified cotton fabric; c, preparation of dyeing liquor: dissolving carmine in organic Stir in a mixed solution of solvent and water to obtain a dye solution; d. Dyeing: put the chitosan-modified cotton fabric in the dye solution at a liquor ratio of 1:30, wash with water, and dry to obtain the product. In the invention, the cotton fabric is modified with chitosan and dyed with an organic solvent system, thereby reducing the discharge of dyeing wastewater, improving the water repellency of the cotton fabric, and increasing the dyeing rate of cochineal red on the cotton fabric and color fastness.
Description
技术领域technical field
本发明属于天然染料染色方法技术领域，具体涉及一种胭脂虫红素少水染色棉织物的方法。The invention belongs to the technical field of dyeing methods of natural dyes, and in particular relates to a method for dyeing cotton fabrics with cochineal with less water.
背景技术Background technique
天然染料是染料行业里比较特殊的一种，主要来自于大自然中，天然染料是指从植物、动物或矿产资源中获得的、不经人工合成，很少或没有经过化学加工的染料。天然染料根据来源可分为植物染料、动物染料和矿物染料，其中以植物染料为主。胭脂虫红色素是从寄生在仙人掌上的胭脂虫雌虫体内提取的一种天然蒽醌类色素，与其他天然色素不同，其理化性质非常稳定，色调呈粉红至紫红，被视作最安全的天然色素而用于食品、化妆品、药品及纺织品等生产。Natural dyes are a special kind in the dye industry. They mainly come from nature. Natural dyes refer to dyes obtained from plants, animals or mineral resources without artificial synthesis and little or no chemical processing. Natural dyes can be divided into plant dyes, animal dyes and mineral dyes according to the source, among which plant dyes are the main ones. Carmine is a natural anthraquinone pigment extracted from the cochineal female parasitic on the cactus. Unlike other natural pigments, its physical and chemical properties are very stable, and its color is pink to purple. It is regarded as the safest Natural pigments are used in the production of food, cosmetics, pharmaceuticals and textiles.
胭脂虫红素溶于水后，染料母体带负电荷，对蚕丝和羊毛类蛋白质纤维的可及性较好，而棉等纤维素类纤维因电负性，对胭脂虫红素的上染性能普遍较差，可通过一些方法来改善其染色性能。After cochineal is dissolved in water, the dye matrix is negatively charged, and the accessibility to silk and wool protein fibers is better, while cotton and other cellulosic fibers are negatively affected by the dyeing performance of cochineal. Generally poor, some methods can be used to improve its dyeing performance.
如中国专利201510661513.1，一种棉织物的无媒染色方法采用阳离子改性剂LD8202等对棉织物进行表面改性，提高了胭脂虫红在棉织物上的上染率和色牢度，但改善的效果有限。Such as Chinese patent 201510661513.1, a kind of non-corresponding dyeing method of cotton fabric adopts cationic modifier LD8202 etc. to carry out surface modification to cotton fabric, has improved the dyeing rate and color fastness of cochineal red on cotton fabric, but the improved The effect is limited.
目前无水或少水染色方法一般包括超临界二氧化碳染色、溶剂染色、真空染料升华染色。但超临界二氧化碳染色设备要求高，成本大，投资高，不符合实际，真空染料升华染色局限大，只有少量染料才能完成升华，而溶剂染色的操作则相对简单。有机溶剂的染色大多集中在分散染料和活性染料等化学染料的染色，如中国专利201510683767.3和201410152912.0等，而天然染料胭脂虫红的有机溶剂染色则未见报道。Current anhydrous or water-less dyeing methods generally include supercritical carbon dioxide dyeing, solvent dyeing, and vacuum dye sublimation dyeing. However, supercritical carbon dioxide dyeing equipment requires high requirements, high cost, and high investment, which is not realistic. Vacuum dye sublimation dyeing has a large limitation, and only a small amount of dye can complete the sublimation, while the operation of solvent dyeing is relatively simple. The dyeing of organic solvents mostly focuses on the dyeing of chemical dyes such as disperse dyes and reactive dyes, such as Chinese patents 201510683767.3 and 201410152912.0, etc., while the organic solvent dyeing of natural dye cochineal has not been reported.
发明内容Contents of the invention
本发明的目的在于克服现有技术的不足，提供一种可以减少染色废水排放，提高棉织物拒水性能，提高胭脂虫红素对棉织物的上染率和色牢度的胭脂虫红素少水染色棉织物的方法。The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a kind of cochineal that can reduce the discharge of dyeing wastewater, improve the water repellency of cotton fabrics, and improve the dyeing rate and color fastness of cochineal to cotton fabrics. A method of water dyeing cotton fabrics.
本发明一种胭脂虫红素少水染色棉织物的方法，其特征在于，包括以下步骤：A kind of method for dyeing cotton fabric with less water of carmine of the present invention, it is characterized in that, comprises the following steps:
a、配制整理液：取壳聚糖，加入冰醋酸，搅拌，得到浓度为5g/L~15g/L的壳聚糖整理液；a, preparation finishing liquid: get chitosan, add glacial acetic acid, stir, obtain the chitosan finishing liquid that concentration is 5g/L～15g/L;
b、棉织物整理：将棉织物按1:30浴比浸入a步骤得到的壳聚糖整理液中，加交联剂，采用二浸二轧处理，处理后纯棉织物的带液率为50％～100％，在酸中和环境中放置2～5min，水洗，烘焙，得到壳聚糖改性棉织物；B, cotton fabric finishing: cotton fabric is immersed in the chitosan finishing liquid that step a obtains by 1:30 bath ratio, adds crosslinking agent, adopts two soaking two rollings to process, and the liquid carrying rate of pure cotton fabric after processing is 50% % to 100%, placed in an acid neutralizing environment for 2 to 5 minutes, washed with water, and baked to obtain chitosan-modified cotton fabrics;
c、配制染液：将胭脂虫红素溶解于有机溶剂和水的混合溶液中，搅拌，得到染液；c, preparation of dyeing solution: dissolving cochineal in the mixed solution of organic solvent and water, stirring to obtain dyeing solution;
d、染色：将b步骤得到的壳聚糖改性棉织物按1:30浴比置于c步骤得到的染液中进行染色，水洗，干燥，得到染色的壳聚糖改性棉织物。d, dyeing: the chitosan modified cotton fabric obtained in step b is placed in the dye solution obtained in step c at a bath ratio of 1:30 for dyeing, washed with water, and dried to obtain dyed chitosan modified cotton fabric.
上述一种胭脂虫红素少水染色棉织物的方法，其中所述壳聚糖相对分子质量为5×105～7×105，冰醋酸质量百分浓度为1%~3%。The above-mentioned method for dyeing cotton fabric with less water by cochineal, wherein the relative molecular mass of chitosan is 5×10 5 to 7×10 5 , and the mass percent concentration of glacial acetic acid is 1% to 3%.
上述一种胭脂虫红素少水染色棉织物的方法，其中所述交联剂的加入量为整理液重量的0.5%~2%。The above-mentioned method for dyeing cotton fabric with less water with carmine, wherein the amount of the crosslinking agent added is 0.5% to 2% of the weight of the finishing solution.
进一步的，上述的一种胭脂虫红素少水染色棉织物的方法，其中所述交联剂为三聚磷酸钠、环氧氯丙烷、柠檬酸中的至少一种。Furthermore, the above-mentioned method for dyeing cotton fabric with less water with carmine, wherein the crosslinking agent is at least one of sodium tripolyphosphate, epichlorohydrin, and citric acid.
上述的一种胭脂虫红素少水染色棉织物的方法，其中所述酸中和环境为氨气环境。The above-mentioned method for dyeing cotton fabric with less water with carmine, wherein the acid neutralizing environment is an ammonia gas environment.
上述的一种胭脂虫红素少水染色棉织物的方法，其中所述烘焙温度为40～80℃，烘焙时间为10～60min。The above-mentioned method for dyeing cotton fabric with less water with carmine, wherein the baking temperature is 40-80° C., and the baking time is 10-60 minutes.
上述的一种胭脂虫红素少水染色棉织物的方法，其中所述有机溶剂中和水的混合溶液中，有机溶剂占混合溶液的体积百分比为90%～95%。The above-mentioned method for dyeing cotton fabric with less water with carmine, wherein in the mixed solution of organic solvent and water, the organic solvent accounts for 90% to 95% by volume of the mixed solution.
进一步的，上述的一种胭脂虫红素少水染色棉织物的方法，其中所述有机溶剂为醇类有机溶剂，醇类有机溶剂为乙醇或异丙醇中的一种。Further, the above-mentioned method for dyeing cotton fabric with less water with carmine, wherein the organic solvent is an alcoholic organic solvent, and the alcoholic organic solvent is one of ethanol or isopropanol.
上述的一种胭脂虫红素少水染色棉织物的方法，其中c步骤中所述胭脂虫红素的加入量为棉织物质量的0.1%～5%。The above method for dyeing cotton fabric with less water with cochineal, wherein the amount of cochineal added in step c is 0.1% to 5% of the mass of the cotton fabric.
上述的一种胭脂虫红素少水染色棉织物的方法，其中d步骤中所述染色温度为40～90℃，染色时间为30～80min。The above-mentioned method for dyeing cotton fabric with less water with carmine, wherein the dyeing temperature in step d is 40-90° C., and the dyeing time is 30-80 minutes.
本发明为提高胭脂虫红素对棉织物的上染性能，以壳聚糖对棉织物进行改性处理后，采用有机溶剂体系进行染色，在减少染色废水排放，提高棉织物拒水性能的同时，提高了胭脂虫红素对棉织物（棉针织物和棉机织物）的上染率和色牢度，这对提高纺织品的附加值，拓宽天然染料在纺织领域的应用范围，减少天然染料染色过程对环境的污染和节约废水处理的成本具有十分重要的意义。In order to improve the dyeing performance of cochineal red on cotton fabrics, the invention uses chitosan to modify the cotton fabrics and dyes them with an organic solvent system, so as to reduce the discharge of dyeing wastewater and improve the water repellency of cotton fabrics. , improve the dyeing rate and color fastness of carmine to cotton fabrics (cotton knitted fabrics and cotton woven fabrics), which can improve the added value of textiles, broaden the application range of natural dyes in the textile field, and reduce the dyeing of natural dyes The process is of great significance to the pollution of the environment and the cost saving of wastewater treatment.
具体实施方式Detailed ways
下面结合具体实施例进一步详细描述本发明的技术方案，但本发明的保护范围不局限于以下所述。The technical solution of the present invention will be further described in detail below in conjunction with specific examples, but the protection scope of the present invention is not limited to the following description.
实施例1Example 1
胭脂虫红素少水染色棉织物的方法，具体染色方法如下：A method for dyeing cotton fabrics with less water content of cochineal, the specific dyeing method is as follows:
a.配制整理液：a. Preparation of finishing solution:
将相对分子质量为6×105的壳聚糖置于质量百分浓度为1%的冰醋酸中，搅拌均匀直至完全溶解，配置成浓度为8g/L的壳聚糖整理液；Place the chitosan with a relative molecular mass of 6×10 5 in glacial acetic acid with a mass percentage concentration of 1%, stir evenly until completely dissolved, and configure a chitosan finishing solution with a concentration of 8g/L;
b.纯棉织物整理：将纯棉织物按1:30浴比置于经a步骤配制的整理液中，加入整理液重量0.5%的三聚磷酸钠，采用二浸二轧处理，处理后纯棉织物的带液率为60％，在氨气氛围中放置2~5min，然后水洗，40℃烘焙60min，得壳聚糖改性棉织物；B. Cotton fabric finishing: pure cotton fabric is placed in the finishing solution prepared through step a by bath ratio of 1:30, adding sodium tripolyphosphate of 0.5% of the finishing solution weight, adopting two dipping and two rolling treatments, after treatment, pure The liquid carrying rate of the cotton fabric is 60%, placed in an ammonia atmosphere for 2-5 minutes, then washed with water, and baked at 40°C for 60 minutes to obtain a chitosan-modified cotton fabric;
c.配制染液：将天然染料胭脂虫红素置于乙醇和水的混合液中，乙醇占混合溶液的体积百分数为93%，搅拌均匀配制染液，天然染料胭脂虫红素的加入量为棉织物质量的1%；c. Prepare dye solution: place natural dye cochineal in the mixed solution of ethanol and water, ethanol accounts for 93% by volume of the mixed solution, stir evenly to prepare dye solution, the addition amount of natural dye cochineal is 1% of the mass of cotton fabrics;
d.染色过程：将壳聚糖改性棉织物按1:30浴比置于c步骤配制的染液中染色，其中，染色温度为80℃，染色时间为30分钟；染色完毕取出布样，水洗，晾干，得染色的壳聚糖改性棉织物。d. Dyeing process: the chitosan modified cotton fabric is dyed in the dye solution prepared in step c by a bath ratio of 1:30, wherein the dyeing temperature is 80 ° C, and the dyeing time is 30 minutes; after dyeing, take out the cloth sample, After washing and drying, the dyed chitosan-modified cotton fabric was obtained.
经电脑测色配色仪测定，上述染色棉织物的K/S值为13.4，按GB/T 3921.1－1997测定皂洗牢度3级，按GB/T 3920－1997测定干摩擦牢度4～5级，湿摩擦牢度4级。经接触角测定仪测得接触角为110°。The K/S value of the above-mentioned dyed cotton fabric is 13.4 by the computer color measuring and matching instrument, the soaping fastness is measured according to GB/T 3921.1-1997, and the dry rubbing fastness is measured according to GB/T 3920-1997 4~5 Grade, wet rubbing fastness grade 4. The contact angle measured by a contact angle meter was 110°.
实施例2Example 2
胭脂虫红素少水染色棉织物的方法，具体染色方法如下：A method for dyeing cotton fabrics with less water content of cochineal, the specific dyeing method is as follows:
a.配制整理液：a. Preparation of finishing solution:
将相对分子质量为7×105的壳聚糖置于质量百分浓度为3%的冰醋酸中，搅拌均匀直至完全溶解，配置成12g/L的壳聚糖整理液；The chitosan with a relative molecular mass of 7×10 5 is placed in glacial acetic acid with a mass percentage concentration of 3%, stirred evenly until completely dissolved, and configured into a 12g/L chitosan finishing solution;
b.纯棉织物整理：将纯棉织物按1:30浴比置于经a步骤配制的整理液中，加入整理液重量1.5%的三聚磷酸钠，采用二浸二轧处理，处理后纯棉织物的带液率为90％，在氨气氛围中放置2~5min，然后水洗，80℃烘焙20min，得壳聚糖改性棉织物；b. Cotton fabric finishing: pure cotton fabric is placed in the finishing solution prepared through a step by a bath ratio of 1:30, adding sodium tripolyphosphate with 1.5% of the finishing solution weight, adopting two dipping and two rolling treatments, and the treated pure The liquid carrying rate of the cotton fabric is 90%, placed in an ammonia atmosphere for 2-5 minutes, then washed with water, and baked at 80°C for 20 minutes to obtain a chitosan-modified cotton fabric;
c.配制染液：将天然染料胭脂虫红素置于异丙醇和水的混合液中，异丙醇占混合溶液的体积百分数为95%，搅拌均匀配制成染液，天然染料胭脂虫红素的加入量为棉织物质量的3%；c. Preparation of dyeing solution: place the natural dye cochineal in a mixture of isopropanol and water, isopropanol accounts for 95% of the volume of the mixed solution, stir evenly to prepare a dyeing solution, natural dye cochineal The amount added is 3% of the cotton fabric quality;
d.染色过程：将壳聚糖改性棉织物按1:30浴比置于c步骤配制的染液中染色，其中，染色温度为90℃，染色时间为80分钟；染色完毕取出布样，水洗，晾干，得染色的壳聚糖改性棉织物。d. Dyeing process: the chitosan modified cotton fabric is dyed in the dye solution prepared in step c by a bath ratio of 1:30, wherein the dyeing temperature is 90 ° C, and the dyeing time is 80 minutes; after dyeing, take out the cloth sample, After washing and drying, the dyed chitosan-modified cotton fabric was obtained.
经电脑测色配色仪测定，上述染色棉织物的K/S值为15.2，按GB/T 3921.1－1997测定皂洗牢度3级，按GB/T 3920－1997测定干摩擦牢度4～5级，湿摩擦牢度4级。经接触角测定仪测得接触角为130°。The K/S value of the above-mentioned dyed cotton fabric is 15.2 by the computer color measuring and matching instrument, the soaping fastness is measured according to GB/T 3921.1-1997, and the dry rubbing fastness is measured according to GB/T 3920-1997 4~5 Grade, wet rubbing fastness grade 4. The contact angle measured by a contact angle meter was 130°.
实施例3Example 3
胭脂虫红素少水染色棉织物的方法，具体染色方法如下：A method for dyeing cotton fabrics with less water content of cochineal, the specific dyeing method is as follows:
a.配制整理液：a. Preparation of finishing solution:
将相对分子质量为5×105的壳聚糖置于质量百分浓度为1%的冰醋酸中，搅拌均匀直至完全溶解，配置成10g/L的壳聚糖整理液；The chitosan with a relative molecular mass of 5×10 5 is placed in glacial acetic acid with a mass percentage concentration of 1%, stirred evenly until completely dissolved, and configured into a 10g/L chitosan finishing solution;
b.纯棉织物整理：将纯棉织物按1:30浴比置于经a步骤配制的整理液中，加入整理液重量1%的环氧氯丙烷，采用二浸二轧处理，处理后纯棉织物的带液率为100％，在氨气氛围中放置2~5min，然后水洗，60℃烘焙30min，得壳聚糖改性棉织物；b. Cotton fabric finishing: the pure cotton fabric is placed in the finishing solution prepared through a step by a bath ratio of 1:30, and 1% epichlorohydrin of the finishing solution weight is added, and two dipping and two rolling treatments are adopted. The liquid carrying rate of the cotton fabric is 100%, placed in an ammonia atmosphere for 2-5 minutes, then washed with water, and baked at 60°C for 30 minutes to obtain a chitosan-modified cotton fabric;
c.配制染液：将天然染料胭脂虫红素置于乙醇和水的混合液中，乙醇占混合溶液的体积百分数为93%，搅拌均匀配制成染液，天然染料胭脂虫红素的加入量为棉织物质量的3%；c. Preparation of dye solution: place natural dye cochineal in the mixed solution of ethanol and water, ethanol accounts for 93% of the volume of the mixed solution, stir evenly to prepare dye solution, the addition amount of natural dye cochineal 3% of the mass of cotton fabric;
d.染色过程：将壳聚糖改性棉织物按1:30浴比置于c步骤配制的染液中染色，其中，染色温度为80℃，染色时间为40分钟；染色完毕取出布样，水洗，晾干，得染色的壳聚糖改性棉织物。d. Dyeing process: the chitosan modified cotton fabric is dyed in the dye solution prepared in step c by a bath ratio of 1:30, wherein the dyeing temperature is 80 ° C, and the dyeing time is 40 minutes; after dyeing, take out the cloth sample, After washing and drying, the dyed chitosan-modified cotton fabric was obtained.
经电脑测色配色仪测定，上述染色棉织物的K/S值为16.7，按GB/T 3921.1－1997测定皂洗牢度3级，按GB/T 3920－1997测定干摩擦牢度4～5级，湿摩擦牢度4级。经接触角测定仪测得接触角为101°。The K/S value of the above-mentioned dyed cotton fabric is 16.7 by computer color measurement and color matching instrument, the soaping fastness is 3 grades according to GB/T 3921.1-1997, and the dry rubbing fastness is 4-5 according to GB/T 3920-1997 Grade, wet rubbing fastness grade 4. The contact angle measured by a contact angle meter was 101°.
实施例4Example 4
胭脂虫红素少水染色棉织物的方法，具体染色方法如下：A method for dyeing cotton fabrics with less water content of cochineal, the specific dyeing method is as follows:
a.配制整理液：a. Preparation of finishing solution:
将相对分子质量为6×105的壳聚糖置于质量百分浓度为2%的冰醋酸中，搅拌均匀直至完全溶解，配置成10g/L的壳聚糖整理液；Put the chitosan with a relative molecular mass of 6×10 5 in glacial acetic acid with a mass percentage concentration of 2%, stir evenly until completely dissolved, and configure a 10g/L chitosan finishing solution;
b.纯棉织物整理：将纯棉织物按1:30浴比置于经a步骤配制的整理液中，加入整理液重量2%的柠檬酸，采用二浸二轧处理，处理后纯棉织物的带液率为50％，在氨气氛围中放置2~5min，然后水洗，50℃烘焙50min，得壳聚糖改性棉织物；b. Cotton fabric finishing: put the pure cotton fabric in the finishing solution prepared in step a by bath ratio of 1:30, add 2% citric acid of the finishing solution weight, adopt two dipping and two rolling treatments, and the pure cotton fabric after treatment The liquid carrying rate was 50%, placed in an ammonia atmosphere for 2-5 minutes, then washed with water, and baked at 50°C for 50 minutes to obtain chitosan-modified cotton fabrics;
c.配制染液：将天然染料胭脂虫红素置于异丙醇和水的混合液中，异丙醇占混合溶液的体积百分数为92%，搅拌均匀配制成染液，天然染料胭脂虫红素的加入量为棉织物质量的2%；c. Preparation of dyeing solution: place the natural dye cochineal in the mixed solution of isopropanol and water, isopropanol accounts for 92% by volume of the mixed solution, stir evenly to prepare the dyeing solution, natural dye cochineal The addition amount is 2% of cotton fabric quality;
d.染色过程：将壳聚糖改性棉织物按1:30浴比置于c步骤配制的染液中染色，其中，染色温度为80℃，染色时间为40分钟；染色完毕取出布样，水洗，晾干，得染色的壳聚糖改性棉织物。d. Dyeing process: the chitosan modified cotton fabric is dyed in the dye solution prepared in step c by a bath ratio of 1:30, wherein the dyeing temperature is 80 ° C, and the dyeing time is 40 minutes; after dyeing, take out the cloth sample, After washing and drying, the dyed chitosan-modified cotton fabric was obtained.
经电脑测色配色仪测定，上述染色棉织物的K/S值为17.3，按GB/T 3921.1－1997测定皂洗牢度3~4级，按GB/T 3920－1997测定干摩擦牢度4～5级，湿摩擦牢度4级。经接触角测定仪测得接触角为145°。The K/S value of the above-mentioned dyed cotton fabric is 17.3 by computer color measuring and matching instrument, the soaping fastness is 3~4 according to GB/T 3921.1-1997, and the dry rubbing fastness is 4 according to GB/T 3920-1997 ~ Grade 5, wet rubbing fastness grade 4. The contact angle measured by a contact angle meter is 145°.
实施例5Example 5
胭脂虫红素少水染色棉织物的方法，具体染色方法如下：A method for dyeing cotton fabrics with less water content of cochineal, the specific dyeing method is as follows:
a.配制整理液：a. Preparation of finishing solution:
将相对分子质量为7×105的壳聚糖置于质量百分浓度为3%的冰醋酸中，搅拌均匀直至完全溶解，配置成15g/L的壳聚糖整理液；The chitosan with a relative molecular mass of 7×10 5 is placed in glacial acetic acid with a mass percentage concentration of 3%, stirred evenly until completely dissolved, and configured into a 15g/L chitosan finishing solution;
b.纯棉织物整理：将纯棉织物按1:30浴比置于经a步骤配制的整理液中，加入整理液重量1.5%的柠檬酸，采用二浸二轧处理，处理后纯棉织物的带液率为80％，在氨气氛围中放置2~5min，然后水洗，60℃烘焙30min，得壳聚糖改性棉织物；b. Cotton fabric finishing: put the pure cotton fabric in the finishing solution prepared in step a by bath ratio of 1:30, add 1.5% citric acid of the finishing solution weight, adopt two dipping and two rolling treatments, and the pure cotton fabric after treatment The liquid carrying rate is 80%, placed in an ammonia atmosphere for 2-5 minutes, then washed with water, and baked at 60°C for 30 minutes to obtain chitosan-modified cotton fabrics;
c.配制染液：将天然染料胭脂虫红素置于乙醇和水的混合液中，乙醇占混合溶液的体积百分数为93%，搅拌均匀配制染液，天然染料胭脂虫红素的加入量为棉织物质量的0.5%；c. Prepare dye solution: place natural dye cochineal in the mixed solution of ethanol and water, ethanol accounts for 93% by volume of the mixed solution, stir evenly to prepare dye solution, the addition amount of natural dye cochineal is 0.5% of the mass of cotton fabric;
d.染色过程：将壳聚糖改性棉织物按1:30浴比置于c步骤配制的染液中染色，其中，染色温度为60℃，染色时间为50分钟；染色完毕取出布样，水洗，晾干，得染色的壳聚糖改性棉织物。d. Dyeing process: the chitosan modified cotton fabric is dyed in the dye solution prepared in step c by a bath ratio of 1:30, wherein the dyeing temperature is 60 ° C, and the dyeing time is 50 minutes; after dyeing, take out the cloth sample, After washing and drying, the dyed chitosan-modified cotton fabric was obtained.
经电脑测色配色仪测定，上述染色棉织物的K/S值为15.5，按GB/T 3921.1－1997测定皂洗牢度3级，按GB/T 3920－1997测定干摩擦牢度4～5级，湿摩擦牢度4级。经接触角测定仪测得接触角为130°。The K/S value of the above-mentioned dyed cotton fabric is 15.5 by the computer color measuring and matching instrument, the soaping fastness is measured according to GB/T 3921.1-1997, and the dry rubbing fastness is measured according to GB/T 3920-1997 4~5 Grade, wet rubbing fastness grade 4. The contact angle measured by a contact angle meter was 130°.
对比例1Comparative example 1
胭脂虫红素染色棉织物的方法，具体方法如下：The method for dyeing cotton fabric with carmine, concrete method is as follows:
a.配制染液：将天然染料胭脂虫红素置于乙醇和水的混合液中，乙醇占混合溶液的体积百分数为93%，搅拌均匀配制染液，天然染料胭脂虫红素的加入量为棉织物质量的5%；a. Prepare dye solution: place natural dye cochineal in the mixed solution of ethanol and water, ethanol accounts for 93% by volume of the mixed solution, stir evenly to prepare dye solution, the addition amount of natural dye cochineal is 5% of the mass of cotton fabric;
b.染色过程：直接将棉织物按1:30浴比置于a步骤配制的染液中染色，其中，染色温度为80℃，染色时间为60分钟；染色完毕取出布样，水洗，晾干，得染色棉织物。b. Dyeing process: directly place the cotton fabric in the dye solution prepared in step a according to the bath ratio of 1:30, wherein the dyeing temperature is 80°C, and the dyeing time is 60 minutes; after dyeing, take out the cloth sample, wash it with water, and dry it in the air , to dye cotton fabrics.
经电脑测色配色仪测定，上述染色棉织物的K/S值为5.6，按GB/T 3921.1－1997测定皂洗牢度2级，按GB/T 3920－1997测定干摩擦牢度4级，湿摩擦牢度3~4级。经接触角测定仪测得接触角为130°。水在织物表面快速铺展，接触角无法读取数值。The K/S value of the above-mentioned dyed cotton fabric is 5.6 by the computer color measuring and matching instrument, the soaping fastness is measured according to GB/T 3921.1-1997, and the dry rubbing fastness is measured according to GB/T 3920-1997, which is grade 4. The wet rubbing fastness is grade 3~4. The contact angle measured by a contact angle meter was 130°. The water spreads rapidly on the surface of the fabric, and the contact angle cannot be read.
对比例2Comparative example 2
胭脂虫红素染色棉织物的方法，具体方法如下：The method for dyeing cotton fabric with carmine, concrete method is as follows:
a.配制染液：将天然染料胭脂虫红素置于纯水中，搅拌均匀配制染液，天然染料胭脂虫红素的加入量为棉织物质量的5%；a. Prepare dye liquor: place natural dye cochineal in pure water, stir evenly to prepare dye liquor, the addition of natural dye cochineal is 5% of cotton fabric quality;
b.染色过程：直接将棉织物按1:30浴比置于a步骤配制的染液中染色，其中，染色温度为90℃，染色时间为60分钟；染色完毕取出布样，水洗，晾干，得染色棉织物。b. Dyeing process: directly place the cotton fabric in the dye solution prepared in step a according to the bath ratio of 1:30, wherein the dyeing temperature is 90°C, and the dyeing time is 60 minutes; after dyeing, take out the cloth sample, wash it with water, and dry it in the air , to dye cotton fabrics.
经电脑测色配色仪测定，上述染色棉织物的K/S值为3.2，按GB/T 3921.1－1997测定皂洗牢度2级，按GB/T 3920－1997测定干摩擦牢度4级，湿摩擦牢度3级。水在织物表面快速铺展，接触角无法读取数值。The K/S value of the above-mentioned dyed cotton fabric is 3.2 by the computer color measuring and matching instrument, the soaping fastness is measured according to GB/T 3921.1-1997, and the dry rubbing fastness is measured according to GB/T 3920-1997, which is grade 4. Wet rubbing fastness level 3. The water spreads rapidly on the surface of the fabric, and the contact angle cannot be read.
对比例3Comparative example 3
胭脂虫红素染色棉织物的方法，具体方法如下：The method for dyeing cotton fabric with carmine, concrete method is as follows:
a.配制整理液：a. Preparation of finishing solution:
将相对分子质量为7×105的壳聚糖置于浓度为3%的冰醋酸中，搅拌均匀直至完全溶解，配置成15g/L的壳聚糖整理液；The chitosan with a relative molecular mass of 7×10 5 is placed in 3% glacial acetic acid, stirred evenly until completely dissolved, and configured into a 15g/L chitosan finishing solution;
b.纯棉织物整理：将纯棉织物按1:30浴比置于经a步骤配制的整理液中，加入1.5%的柠檬酸，采用二浸二轧处理，处理后纯棉织物的带液率为80％，在氨气氛围中放置2~5min，然后水洗，60℃烘焙30min，得壳聚糖改性棉织物；b. Cotton fabric finishing: the pure cotton fabric is placed in the finishing liquid prepared through step a by a bath ratio of 1:30, and 1.5% citric acid is added, and two dipping and two rolling treatments are adopted, and the treated pure cotton fabric is treated with liquid The ratio is 80%, placed in an ammonia atmosphere for 2-5 minutes, then washed with water, and baked at 60°C for 30 minutes to obtain chitosan-modified cotton fabrics;
c.配制染液：将天然染料胭脂虫红素置于纯水中，搅拌均匀配制染液，天然染料胭脂虫红素的加入量为棉织物质量的5%；c. Prepare dye liquor: place natural dye cochineal in pure water, stir evenly to prepare dye liquor, the addition of natural dye cochineal is 5% of cotton fabric quality;
d.染色过程：将壳聚糖改性棉织物按1:30浴比置于c步骤配制的染液中染色，其中，染色温度为60℃，染色时间为50分钟；染色完毕取出布样，水洗，晾干，得染色的壳聚糖改性棉织物。d. Dyeing process: the chitosan modified cotton fabric is dyed in the dye solution prepared in step c by a bath ratio of 1:30, wherein the dyeing temperature is 60 ° C, and the dyeing time is 50 minutes; after dyeing, take out the cloth sample, After washing and drying, the dyed chitosan-modified cotton fabric was obtained.
经电脑测色配色仪测定，上述染色棉织物的K/S值为7.6，按GB/T 3921.1－1997测定皂洗牢度3级，按GB/T 3920－1997测定干摩擦牢度4～5级，湿摩擦牢度4级。经接触角测定仪测得接触角为130°。The K/S value of the above-mentioned dyed cotton fabric is 7.6 according to the computer color measuring and matching instrument, the soaping fastness is determined according to GB/T 3921.1-1997, and the dry rubbing fastness is measured according to GB/T 3920-1997 4~5 Grade, wet rubbing fastness grade 4. The contact angle measured by a contact angle meter was 130°.
综上可知，本发明公开的胭脂虫红素少水染色方法，用含有三聚磷酸钠、柠檬酸或环氧氯丙烷的壳聚糖改性液对棉织物进行预处理，再对壳聚糖改性棉织物进行有机溶剂染色处理。根据溶解度参数理论，胭脂虫红素在有机溶剂体系中对棉织物更易于上染，再加上壳聚糖对棉织物预处理后，棉纤维表面的的阳离子数增加，提高了对胭脂虫红素的固着力，与对比例相比，本发明工艺染色速度快，上染率和色牢度更高，节省了用水量，减少了染色废水的排放，提高了棉织物的拒水性能。In summary, the method for dyeing carmine with less water disclosed by the present invention uses a chitosan modification solution containing sodium tripolyphosphate, citric acid or epichlorohydrin to pretreat the cotton fabric, and then to chitosan Modified cotton fabrics were dyed with organic solvents. According to the solubility parameter theory, cochineal is easier to dye cotton fabric in organic solvent system, and after chitosan is pretreated on cotton fabric, the number of cations on the surface of cotton fiber increases, which improves the dyeing effect of cochineal. Compared with the comparison example, the process of the present invention has faster dyeing speed, higher dye uptake and color fastness, saves water consumption, reduces the discharge of dyeing wastewater, and improves the water repellency of cotton fabrics.
以上所述仅是本发明的优选实施方式，应当理解本发明并非局限于本文所披露的形式，不应看作是对其他实施例的排除，而可用于各种其他组合、修改和环境，并能够在本文所述构想范围内，通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本发明的精神和范围，则都应在本发明所附权利要求的保护范围内。The above descriptions are only preferred embodiments of the present invention, and it should be understood that the present invention is not limited to the forms disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and Modifications can be made within the scope of the ideas described herein, by virtue of the above teachings or skill or knowledge in the relevant art. However, changes and changes made by those skilled in the art do not depart from the spirit and scope of the present invention, and should all be within the protection scope of the appended claims of the present invention.
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