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CN101787643B - A kind of washing process of reactive dye cleaning agent - Google Patents

A kind of washing process of reactive dye cleaning agent Download PDF

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CN101787643B
CN101787643B CN2010101083484A CN201010108348A CN101787643B CN 101787643 B CN101787643 B CN 101787643B CN 2010101083484 A CN2010101083484 A CN 2010101083484A CN 201010108348 A CN201010108348 A CN 201010108348A CN 101787643 B CN101787643 B CN 101787643B
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washing
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water
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CN101787643A (en
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王学川
贺宝元
强涛涛
任龙芳
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Shaanxi University of Science and Technology
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Abstract

本发明提供一种活性染料净洗剂的水洗工艺,将染色后的产品依次经冷水洗、酸性皂洗、碱洗、热水洗、温水洗后烘干;冷水洗采用常温水洗1~3格;酸性皂洗是在40~60℃的皂洗液中皂洗1~2格,且皂洗液的pH值为3~5,皂液中净洗剂的用量为0.6~1.2g/l;碱洗是在40~50℃的pH为8~10的碱性溶液中进行碱洗;热水洗是在90~95℃的热水中洗1~2格;温水洗是在45~60℃的温水中洗1~2格。本发明适合活性染料轧染之后的水洗工艺,其优点在于,酸性条件下皂洗,皂洗温度低,水洗工序少,可节约大量的水和蒸汽。水洗后的纺织品,其摩擦牢度与皂洗牢度均优于常规水洗工艺。The invention provides a washing process of a reactive dye detergent, in which the dyed product is sequentially washed with cold water, acid soaped, alkali washed, hot water washed and warm water washed, and then dried; the cold water washing adopts normal temperature water for 1 to 3 grids; Acidic soaping is soaping 1 to 2 grids in soaping liquid at 40-60°C, and the pH value of the soaping liquid is 3-5, and the amount of detergent in the soaping liquid is 0.6-1.2g/l; Washing is carried out in an alkaline solution with a pH of 8-10 at 40-50°C; washing with hot water is washing 1-2 grids in hot water at 90-95°C; washing with warm water is washing in warm water at 45-60°C Wash 1 to 2 grids in the middle. The invention is suitable for the water washing process after pad dyeing of reactive dyes, and has the advantages of soaping under acidic conditions, low soaping temperature, less water washing process, and can save a lot of water and steam. The rubbing fastness and soaping fastness of the washed textiles are better than the conventional washing process.

Description

一种活性染料净洗剂的水洗工艺A kind of washing process of reactive dye cleaning agent

技术领域 technical field

本发明涉及纺织品染整工艺领域,尤其涉及一种活性染料纯棉机织物染色后的净洗剂的水洗工艺。The invention relates to the field of textile dyeing and finishing technology, in particular to a washing process of a detergent for pure cotton woven fabrics dyed with reactive dyes.

背景技术 Background technique

活性染料自1956年问世以来,其发展一直处于领先地位。目前世界上纤维素纤维用活性染料的年产量占全部染料年产量的20%左右,由于新开发的纤维素产品如Lyocell纤维等产量的增加,棉纤维的稳定增长,活性染料的年产量将继续增长。Since the advent of reactive dyes in 1956, its development has been in a leading position. At present, the annual output of reactive dyes for cellulose fibers in the world accounts for about 20% of the total annual output of dyes. Due to the increase in the output of newly developed cellulose products such as Lyocell fiber and the steady growth of cotton fibers, the annual output of reactive dyes will continue increase.

在活性染料染色工艺过程中,染色后的织物表面沾有大量的浮色染料,其中包括部分水解的染料和已吸附于纤维而未参与共价反应的染料,它们对纤维具有一定的直接性,必须借助外力及助剂的共同作用使其脱离纤维而进入水溶液中,由于浮色染料在纤维和净洗液间存在动态吸附平衡,被洗脱下来后会重新吸附到纤维表面,从而导致了浮色洗除不净,产品的湿摩擦牢度达不到要求等缺点。尽量使浮色染料向净洗液中转移,并稳定地分散在净洗液中,降低二次沾染纤维机率是提高净洗效果的关键。During the dyeing process of reactive dyes, the surface of the dyed fabric is stained with a large number of floating dyes, including partially hydrolyzed dyes and dyes that have been adsorbed on the fibers without participating in the covalent reaction. They have certain directness to the fibers. It must be detached from the fiber and enter the aqueous solution with the help of external force and additives. Since the floating dye has a dynamic adsorption balance between the fiber and the cleaning solution, it will be re-adsorbed to the surface of the fiber after being eluted, resulting in floating dye. The color washing is not clean, and the wet rubbing fastness of the product cannot meet the requirements. The key to improving the cleaning effect is to transfer the floating dye to the cleaning solution as much as possible and disperse it stably in the cleaning solution, reducing the probability of secondary contamination of fibers.

活性染料染色后要去除浮色,必须经过多道水洗才能保证成品的最终质量。水洗过程用水量一般占到整个染整用水的60%以上,染整过程中的蒸汽消耗要占到全部能源的60%以上,因此印染企业的节能减排,实质上是对水和蒸汽的节能减排;而对整个印染加工过程来说,又以水洗工序为重。To remove floating color after dyeing with reactive dyes, multiple washings must be performed to ensure the final quality of the finished product. The water consumption in the washing process generally accounts for more than 60% of the entire dyeing and finishing water, and the steam consumption in the dyeing and finishing process accounts for more than 60% of the total energy. Therefore, the energy saving and emission reduction of printing and dyeing enterprises is essentially the energy saving of water and steam. emission reduction; and for the entire printing and dyeing process, the washing process is the most important.

目前印染厂一般水洗工艺如下:At present, the general washing process of printing and dyeing factories is as follows:

染色→冷水洗3格→酸洗(醋酸1mL/L)→热水洗2格(90℃)→碱性皂洗3格(净洗剂5g/L,95℃)→热水洗3格(95℃)→冷水洗3格→烘干(130℃)。所谓的格是机织纺织品在水洗工艺中,每经过一个水洗槽,称之为一格,相当于洗一次。Dyeing → cold water washing 3 compartments → acid washing (acetic acid 1mL/L) → hot water washing 2 compartments (90°C) → alkaline soaping 3 compartments (detergent 5g/L, 95°C) → hot water washing 3 compartments (95°C ) → Wash 3 compartments in cold water → Dry (130°C). The so-called lattice is that in the washing process of woven textiles, every time a washing tank passes through, it is called a lattice, which is equivalent to washing once.

发明内容 Contents of the invention

本发明的目的在于提供一种能够克服现有基于表面活性剂设计的净洗剂的净洗工艺,洗不净,对环境有影响的活性染料净洗剂的水洗工艺。The purpose of the present invention is to provide a kind of cleaning process that can overcome the existing cleaning agent based on surfactant design, wash not clean, the water washing process of the active dye cleaning agent that has influence on environment.

首先是本发明净洗剂的制备:First be the preparation of cleaning agent of the present invention:

1)水相溶液的制备:首先将壳聚糖溶于醋酸溶液中得到质量百分比浓度为0.5~3%的壳聚糖溶液,然后将明胶溶于水中得到质量浓度为3~7%的明胶溶液,所说的壳聚糖的脱乙酰度为89~96%,醋酸溶液的体积比为2~6%;1) Preparation of aqueous phase solution: first dissolving chitosan in acetic acid solution to obtain a chitosan solution with a mass percent concentration of 0.5 to 3%, then dissolving gelatin in water to obtain a gelatin solution with a mass concentration of 3 to 7% , the deacetylation degree of said chitosan is 89~96%, and the volume ratio of acetic acid solution is 2~6%;

按壳聚糖∶明胶为(1~4)∶1的质量比将壳聚糖溶液与明胶溶液混合得壳聚糖/明胶溶液;By chitosan: gelatin is (1~4): the mass ratio of chitosan solution and gelatin solution are mixed to obtain chitosan/gelatin solution;

2)乳液制备:按乳化剂∶液体石蜡=1∶(100~300)的体积比向液体石蜡中加入乳化剂得液体石蜡与乳化剂的混合溶液,所说的乳化剂为司盘80和吐温80,其中司盘80和吐温80的体积比为(1~6)∶1;再按壳聚糖/明胶溶液∶液体石蜡=1∶(4~8)的体积比将壳聚糖/明胶溶液加入到液体石蜡与乳化剂的混合溶液中,在25~35℃乳化10~25min得乳液;2) Emulsion preparation: add emulsifier to liquid paraffin at a volume ratio of emulsifier: liquid paraffin = 1: (100-300) to obtain a mixed solution of liquid paraffin and emulsifier, said emulsifier being Span 80 and emulsifier Wen 80, wherein the volume ratio of Span 80 and Tween 80 is (1~6): 1; Then by the volume ratio of chitosan/gelatin solution: liquid paraffin=1: (4~8) chitosan/ Add the gelatin solution to the mixed solution of liquid paraffin and emulsifier, and emulsify at 25-35°C for 10-25 minutes to obtain an emulsion;

3)交联固化:向上述乳液中逐滴加入质量浓度为50%的戊二醛溶液,戊二醛与壳聚糖的质量比为1∶(2~5),在40~60℃交联2~5h使微球交联固化;3) Cross-linking and curing: add a glutaraldehyde solution with a mass concentration of 50% to the above emulsion dropwise, the mass ratio of glutaraldehyde to chitosan is 1: (2-5), and cross-link at 40-60°C 2 to 5 hours to crosslink and solidify the microspheres;

4)后处理:用异丙醇和无水乙醚反复冲洗反应产物去除液体石蜡,然后将其置于40~55℃的烘箱中干燥得到基于壳聚糖/明胶复合材料的活性染料净洗剂。4) Post-treatment: wash the reaction product repeatedly with isopropanol and anhydrous ether to remove liquid paraffin, then place it in an oven at 40-55° C. to dry to obtain a reactive dye detergent based on chitosan/gelatin composite material.

本发明的水洗工艺如下:Washing process of the present invention is as follows:

将染色后的产品依次经冷水洗、酸性皂洗、碱洗、热水洗、温水洗后烘干;The dyed products are washed with cold water, acid soap, alkali, hot water and warm water in sequence, and then dried;

所说的冷水洗采用常温水洗1~3格;Said cold water washing adopts normal temperature water washing for 1 to 3 compartments;

所说的酸性皂洗是在40~60℃的皂洗液中皂洗1~2格,且皂洗液的pH值为3~5,皂液中净洗剂的用量为0.6~1.2g/l;Said acidic soaping is soaping 1 to 2 grids in the soaping liquid at 40-60°C, and the pH value of the soaping liquid is 3-5, and the consumption of cleaning agent in the soaping liquid is 0.6-1.2g/ l;

所说的碱洗是在40~50℃的pH为8~10的碱性溶液中进行碱洗;Said alkali washing is carried out in an alkaline solution with a pH of 8 to 10 at a temperature of 40 to 50°C;

所说的热水洗是在90~95℃的热水中洗1~2格;The hot water washing is to wash 1 to 2 grids in hot water at 90-95°C;

所说的温水洗是在45~60℃的温水中洗1~2格。Said warm water washing is washing 1 to 2 compartments in warm water of 45 to 60°C.

所说的酸性皂洗步骤中采用醋酸或盐酸调节溶液的pH值为3~5。In the acidic soaping step, acetic acid or hydrochloric acid is used to adjust the pH value of the solution to 3-5.

所说的碱性溶液为碳酸氢钠或碳酸钠溶液。Said alkaline solution is sodium bicarbonate or sodium carbonate solution.

所说的烘干温度为100~130℃。Said drying temperature is 100-130°C.

与现有技术相比,本发明的优点是:Compared with prior art, the advantage of the present invention is:

1)节约用水用汽:皂洗前省掉了热水洗与酸洗工艺,节约用水,皂洗工艺的温度由常规工艺的95℃降到40~60℃,节约蒸汽的用量,实现节能减排的目的。1) Saving water and steam: hot water washing and pickling processes are omitted before soaping, saving water, and the temperature of the soaping process is reduced from 95°C in the conventional process to 40-60°C, saving the amount of steam and realizing energy saving and emission reduction the goal of.

2)保护染料:传统皂洗工艺使用的净洗剂一般为碱性,在高温皂洗时,已固着于织物上的活性染料易发生断键而被破坏,本发明采用酸性条件下皂洗,并降低皂洗温度,可达到保护棉织物上活性染料的作用,同时可降低水洗工艺过程对活性染料的破坏程度。2) Protecting dyes: the cleaning agent used in the traditional soaping process is generally alkaline. When soaping at high temperature, the reactive dyes that have been fixed on the fabric are prone to break bonds and be destroyed. The present invention adopts soaping under acidic conditions. And reducing the soaping temperature can achieve the effect of protecting the reactive dyes on cotton fabrics, and at the same time reduce the damage to the reactive dyes in the washing process.

3)工艺简单,应用前景广泛,适合工业化生产:本发明所提出的水洗工艺简单易行,印染厂目前的设备能够完全满足工艺要求。3) The process is simple, the application prospect is wide, and it is suitable for industrialized production: the washing process proposed by the present invention is simple and easy, and the current equipment of the printing and dyeing factory can fully meet the process requirements.

4)净洗效果好:采用本发明提出的水洗工艺所得到的布,其摩擦牢度与皂洗牢度均优于常规水洗得到的布。4) Good cleaning effect: the cloth obtained by the washing process proposed by the present invention has better rubbing fastness and soaping fastness than cloth obtained by conventional washing.

三种纯棉织物在相同的染色条件下,分别采用常规水洗工艺与本发明水洗工艺。结果对比如下:Three kinds of pure cotton fabrics adopt the conventional water washing process and the water washing process of the present invention respectively under the same dyeing conditions. The results are compared as follows:

表1纯棉织物常规水洗与本发明水洗效果对比Table 1 Pure Cotton Fabric Routine Washing and Washing Effect Contrast of the present invention

Figure GSA00000037500100041
Figure GSA00000037500100041

干、湿摩擦牢度按GB/T3920-1997方法测定;皂洗牢度按GB/T3921.3-1997方法测定。Dry and wet rubbing fastness are measured according to GB/T3920-1997; soaping fastness is measured according to GB/T3921.3-1997.

由试验结果对比分析得出:应用本发明水洗工艺后的活性染料棉织物的摩擦牢度和皂洗牢度均优于常规水洗得到的布,而且质量稳定。From the comparative analysis of the test results, it is concluded that the rubbing fastness and soaping fastness of the reactive dyed cotton fabric after applying the washing process of the present invention are better than those obtained by conventional washing, and the quality is stable.

具体实施方式 Detailed ways

实施例1:一、净洗剂的制备:Embodiment 1: one, the preparation of detergent:

1)水相溶液的制备:首先将脱乙酰度为96%的壳聚糖溶于体积比为2%的醋酸溶液中得到质量百分比浓度为0.5%的壳聚糖溶液,然后将明胶溶于水中得到质量浓度为3%的明胶溶液;1) Preparation of aqueous phase solution: at first dissolving chitosan with a degree of deacetylation of 96% in the acetic acid solution of 2% by volume to obtain a chitosan solution with a mass percent concentration of 0.5%, then dissolving gelatin in water Obtaining a gelatin solution with a mass concentration of 3%;

按壳聚糖∶明胶为1∶1的质量比将壳聚糖溶液与明胶溶液混合得壳聚糖/明胶溶液;By chitosan: gelatin is 1: 1 mass ratio chitosan solution and gelatin solution are mixed to obtain chitosan/gelatin solution;

2)乳液制备:按乳化剂∶液体石蜡=1∶300的体积比向液体石蜡中加入乳化剂得液体石蜡与乳化剂的混合溶液,所说的乳化剂为司盘80和吐温80,其中司盘80和吐温80的体积比为1∶1;再按壳聚糖/明胶溶液∶液体石蜡=1∶4的体积比将壳聚糖/明胶溶液加入到液体石蜡与乳化剂的混合溶液中,在25℃乳化25min得乳液;2) Emulsion preparation: add emulsifier to liquid paraffin to obtain a mixed solution of liquid paraffin and emulsifier by volume ratio of emulsifier: liquid paraffin=1:300, said emulsifier is Span 80 and Tween 80, wherein The volume ratio of Span 80 and Tween 80 is 1: 1; then chitosan/gelatin solution is added to the mixed solution of liquid paraffin and emulsifier by the volume ratio of chitosan/gelatin solution: liquid paraffin=1:4 medium, emulsified at 25°C for 25 minutes to obtain an emulsion;

3)交联固化:向上述乳液中逐滴加入质量浓度为50%的戊二醛溶液,戊二醛与壳聚糖的质量比为1∶2,在40℃交联5h使微球交联固化;3) Cross-linking and curing: add a glutaraldehyde solution with a mass concentration of 50% to the above emulsion dropwise, the mass ratio of glutaraldehyde to chitosan is 1:2, cross-link at 40°C for 5 hours to cross-link the microspheres curing;

4)后处理:用异丙醇和无水乙醚反复冲洗反应产物去除液体石蜡,然后将其置于40℃的烘箱中干燥得到基于壳聚糖/明胶复合材料的活性染料净洗剂。4) Post-treatment: wash the reaction product repeatedly with isopropanol and anhydrous ether to remove liquid paraffin, and then place it in an oven at 40° C. to dry to obtain a reactive dye detergent based on chitosan/gelatin composite material.

二、水洗工艺如下:Second, the washing process is as follows:

将染色后的产品依次经冷水洗、酸性皂洗、碱洗、热水洗、温水洗后烘干;The dyed products are washed with cold water, acid soap, alkali, hot water and warm water in sequence, and then dried;

所说的冷水洗采用常温水洗2格;Said cold water washing adopts 2 grids of normal temperature water washing;

所说的酸性皂洗是在40℃的净洗剂用量0.6g/l的皂洗液中皂洗1格,并用醋酸调节溶液的pH值为5。Said acidic soaping is soaping 1 lattice in the soaping liquid of the cleaning agent consumption 0.6g/l of 40 ℃, and the pH value is 5 with acetic acid regulation solution.

所说的碱洗是在50℃的pH为8的碳酸氢钠溶液中进行碱洗;Said alkali washing is to carry out alkali washing in the sodium bicarbonate solution of 8 at the pH of 50 DEG C;

所说的热水洗是在90℃的热水中洗1格;The so-called hot water washing is to wash one compartment in hot water at 90°C;

所说的温水洗是在60℃的温水中洗1格The so-called warm water washing is to wash 1 compartment in warm water at 60°C.

所说的烘干温度为100℃。Said drying temperature is 100°C.

本实施例适用于活性染料染浅色品种时的水洗工艺。This embodiment is applicable to the washing process when reactive dyes dye light-colored varieties.

实施例2:一、净洗剂的制备:Embodiment 2: one, the preparation of detergent:

1)水相溶液的制备:首先将脱乙酰度为94%的壳聚糖溶于体积比为3%的醋酸溶液中得到质量百分比浓度为1%的壳聚糖溶液,然后将明胶溶于水中得到质量浓度为4%的明胶溶液;1) Preparation of aqueous phase solution: at first dissolving chitosan with a degree of deacetylation of 94% in acetic acid solution of 3% by volume to obtain a chitosan solution with a mass percent concentration of 1%, then dissolving gelatin in water Obtaining a gelatin solution with a mass concentration of 4%;

按壳聚糖∶明胶为2∶1的质量比将壳聚糖溶液与明胶溶液混合得壳聚糖/明胶溶液;By chitosan: gelatin is the mass ratio of 2: 1 that chitosan solution and gelatin solution are mixed to obtain chitosan/gelatin solution;

2)乳液制备:按乳化剂∶液体石蜡=1∶150的体积比向液体石蜡中加入乳化剂得液体石蜡与乳化剂的混合溶液,所说的乳化剂为司盘80和吐温80,其中司盘80和吐温80的体积比为2∶1;再按壳聚糖/明胶溶液∶液体石蜡=1∶5的体积比将壳聚糖/明胶溶液加入到液体石蜡与乳化剂的混合溶液中,在30℃乳化15min得乳液;2) Emulsion preparation: add emulsifier to liquid paraffin to obtain a mixed solution of liquid paraffin and emulsifier by volume ratio of emulsifier: liquid paraffin=1:150, said emulsifier is Span 80 and Tween 80, wherein The volume ratio of Span 80 and Tween 80 is 2: 1; then chitosan/gelatin solution is added to the mixed solution of liquid paraffin and emulsifier by the volume ratio of chitosan/gelatin solution: liquid paraffin=1:5 , emulsified at 30°C for 15 minutes to obtain an emulsion;

3)交联固化:向上述乳液中逐滴加入质量浓度为50%的戊二醛溶液,戊二醛与壳聚糖的质量比为1∶3,在45℃交联4h使微球交联固化;3) Cross-linking and curing: Add glutaraldehyde solution with a mass concentration of 50% to the above emulsion dropwise, the mass ratio of glutaraldehyde to chitosan is 1:3, cross-link at 45°C for 4 hours to cross-link the microspheres curing;

4)后处理:用异丙醇和无水乙醚反复冲洗反应产物去除液体石蜡,然后将其置于45℃的烘箱中干燥得到基于壳聚糖/明胶复合材料的活性染料净洗剂。4) Post-treatment: wash the reaction product repeatedly with isopropanol and anhydrous ether to remove liquid paraffin, and then place it in an oven at 45° C. to dry to obtain a reactive dye detergent based on chitosan/gelatin composite material.

二、水洗工艺如下:Second, the washing process is as follows:

将染色后的产品依次经冷水洗、酸性皂洗、碱洗、热水洗、温水洗后烘干;The dyed products are washed with cold water, acid soap, alkali, hot water and warm water in sequence, and then dried;

所说的冷水洗采用常温水洗1格;Said cold water washing adopts normal temperature water washing for 1 cell;

所说的酸性皂洗是在50℃的净洗剂用量0.8g/l的皂洗液中皂洗1格,并用盐酸调节溶液的pH值为4.5;Said acidic soaping is soaping 1 lattice in the soaping liquid of 0.8g/l detergent consumption of 50 ℃, and the pH value of adjusting solution with hydrochloric acid is 4.5;

所说的碱洗是在45℃的pH为9的碳酸钠溶液中进行碱洗;Said alkali washing is to carry out alkali washing in the sodium carbonate solution of 9 in the pH of 45 ℃;

所说的热水洗是在93℃的热水中洗1格;The hot water washing is to wash one cell in hot water at 93°C;

所说的温水洗是在55℃的温水中洗2格The so-called warm water washing is to wash 2 compartments in warm water at 55°C

所说的烘干温度为110℃。Said drying temperature is 110°C.

本实施例适用于活性染料染浅色品种时水洗工艺。This embodiment is applicable to the water washing process when dyeing light-colored varieties with reactive dyes.

实施例3:一、净洗剂的制备:Embodiment 3: one, the preparation of detergent:

1)水相溶液的制备:首先将脱乙酰度为92%的壳聚糖溶于体积比为4%的醋酸溶液中得到质量百分比浓度为2%的壳聚糖溶液,然后将明胶溶于水中得到质量浓度为6%的明胶溶液;1) Preparation of aqueous phase solution: at first dissolving chitosan with a degree of deacetylation of 92% in acetic acid solution of 4% by volume to obtain a chitosan solution with a mass percentage concentration of 2%, then dissolving gelatin in water Obtaining a gelatin solution with a mass concentration of 6%;

按壳聚糖∶明胶为3∶1的质量比将壳聚糖溶液与明胶溶液混合得壳聚糖/明胶溶液;By chitosan: gelatin is the mass ratio of 3: 1 that chitosan solution and gelatin solution are mixed to obtain chitosan/gelatin solution;

2)乳液制备:按乳化剂∶液体石蜡=1∶200的体积比向液体石蜡中加入乳化剂得液体石蜡与乳化剂的混合溶液,所说的乳化剂为司盘80和吐温80,其中司盘80和吐温80的体积比为4∶1;再按壳聚糖/明胶溶液∶液体石蜡=1∶6的体积比将壳聚糖/明胶溶液加入到液体石蜡与乳化剂的混合溶液中,在28℃乳化20min得乳液;2) Emulsion preparation: add emulsifier to liquid paraffin to obtain a mixed solution of liquid paraffin and emulsifier by volume ratio of emulsifier: liquid paraffin=1:200, said emulsifier is Span 80 and Tween 80, wherein The volume ratio of Span 80 and Tween 80 is 4: 1; then chitosan/gelatin solution is added to the mixed solution of liquid paraffin and emulsifier by the volume ratio of chitosan/gelatin solution: liquid paraffin=1:6 medium, emulsified at 28°C for 20 minutes to obtain an emulsion;

3)交联固化:向上述乳液中逐滴加入质量浓度为50%的戊二醛溶液,戊二醛与壳聚糖的质量比为1∶4,在55℃交联3h使微球交联固化;3) Cross-linking and curing: Add glutaraldehyde solution with a mass concentration of 50% to the above emulsion dropwise, the mass ratio of glutaraldehyde to chitosan is 1:4, cross-link at 55°C for 3h to cross-link the microspheres curing;

4)后处理:用异丙醇和无水乙醚反复冲洗反应产物去除液体石蜡,然后将其置于50℃的烘箱中干燥得到基于壳聚糖/明胶复合材料的活性染料净洗剂。4) Post-treatment: wash the reaction product repeatedly with isopropanol and anhydrous ether to remove liquid paraffin, and then place it in an oven at 50° C. to dry to obtain a reactive dye detergent based on chitosan/gelatin composite material.

二、水洗工艺如下:Second, the washing process is as follows:

将染色后的产品依次经冷水洗、酸性皂洗、碱洗、热水洗、温水洗后烘干;The dyed products are washed with cold water, acid soap, alkali, hot water and warm water in sequence, and then dried;

所说的冷水洗采用常温水洗2格;Said cold water washing adopts 2 grids of normal temperature water washing;

所说的酸性皂洗是在50℃的净洗剂用量1g/l的皂洗液中皂洗1格,并用醋酸调节溶液的pH值为3.5;Said acidic soaping is soaping 1 compartment in soaping solution with detergent dosage of 1g/l at 50°C, and adjusting the pH value of the solution to 3.5 with acetic acid;

所说的碱洗是在45℃的pH为9的碳酸钠溶液中进行碱洗;Said alkali washing is to carry out alkali washing in the sodium carbonate solution of 9 in the pH of 45 ℃;

所说的热水洗是在90℃的热水中洗2格;The hot water washing is to wash 2 grids in hot water at 90°C;

所说的温水洗是在50℃的温水中洗2格The so-called warm water washing is to wash 2 compartments in warm water at 50°C.

所说的烘干温度为120℃。Said drying temperature is 120°C.

本实施例适用于活性染料染中等深度品种时的水洗工艺。This embodiment is applicable to the washing process when reactive dyes dye medium-depth varieties.

实施例4:一、净洗剂的制备:Embodiment 4: one, the preparation of detergent:

1)水相溶液的制备:首先将脱乙酰度为89%的壳聚糖溶于体积比为6%的醋酸溶液中得到质量百分比浓度为3%的壳聚糖溶液,然后将明胶溶于水中得到质量浓度为7%的明胶溶液;1) Preparation of aqueous phase solution: at first dissolving chitosan with a degree of deacetylation of 89% in the acetic acid solution of 6% by volume to obtain a chitosan solution with a mass percent concentration of 3%, then dissolving gelatin in water Obtaining a gelatin solution with a mass concentration of 7%;

按壳聚糖∶明胶为4∶1的质量比将壳聚糖溶液与明胶溶液混合得壳聚糖/明胶溶液;By chitosan: gelatin is the mass ratio of 4: 1 that chitosan solution and gelatin solution are mixed to obtain chitosan/gelatin solution;

2)乳液制备:按乳化剂∶液体石蜡=1∶100的体积比向液体石蜡中加入乳化剂得液体石蜡与乳化剂的混合溶液,所说的乳化剂为司盘80和吐温80,其中司盘80和吐温80的体积比为6∶1;再按壳聚糖/明胶溶液∶液体石蜡=1∶8的体积比将壳聚糖/明胶溶液加入到液体石蜡与乳化剂的混合溶液中,在35℃乳化10min得乳液;2) Emulsion preparation: add emulsifier to liquid paraffin to obtain a mixed solution of liquid paraffin and emulsifier by volume ratio of emulsifier: liquid paraffin=1:100, said emulsifier is Span 80 and Tween 80, wherein The volume ratio of Span 80 and Tween 80 is 6: 1; then chitosan/gelatin solution is added to the mixed solution of liquid paraffin and emulsifier by the volume ratio of chitosan/gelatin solution: liquid paraffin=1:8 , emulsified at 35°C for 10 minutes to obtain an emulsion;

3)交联固化:向上述乳液中逐滴加入质量浓度为50%的戊二醛溶液,戊二醛与壳聚糖的质量比为1∶5,在60℃交联2h使微球交联固化;3) Cross-linking and curing: Add glutaraldehyde solution with a mass concentration of 50% to the above emulsion dropwise, the mass ratio of glutaraldehyde to chitosan is 1:5, cross-link at 60°C for 2h to cross-link the microspheres curing;

4)后处理:用异丙醇和无水乙醚反复冲洗反应产物去除液体石蜡,然后将其置于55℃的烘箱中干燥得到基于壳聚糖/明胶复合材料的活性染料净洗剂。4) Post-treatment: wash the reaction product repeatedly with isopropanol and anhydrous ether to remove liquid paraffin, and then place it in an oven at 55° C. to dry to obtain a reactive dye detergent based on chitosan/gelatin composite material.

二、水洗工艺如下:Second, the washing process is as follows:

将染色后的产品依次经冷水洗、酸性皂洗、碱洗、热水洗、温水洗后烘干;The dyed products are washed with cold water, acid soap, alkali, hot water and warm water in sequence, and then dried;

所说的冷水洗采用常温水洗3格;Said cold water washing adopts 3 grids of normal temperature water washing;

所说的酸性皂洗是在60℃的净洗剂用量1.2g/l的皂洗液中皂洗2格,并用盐酸调节溶液的pH值为3;Said acidic soaping is soaping 2 lattices in the soaping liquid of 1.2g/l detergent consumption of 60 ℃, and the pH value of adjusting solution with hydrochloric acid is 3;

所说的碱洗是在40℃的pH为10的碳酸氢钠溶液中进行碱洗;Said alkali washing is to carry out alkali washing in the sodium bicarbonate solution of 10 at the pH of 40 DEG C;

所说的热水洗是在95℃的热水中洗2格;The hot water washing is to wash 2 grids in hot water at 95°C;

所说的温水洗是在45℃的温水中洗2格The so-called warm water washing is to wash 2 compartments in warm water at 45°C

所说的烘干温度为130℃。Said drying temperature is 130°C.

本实施例适用于活性染料染深色品种时的水洗工艺。This embodiment is applicable to the washing process when reactive dyes dye dark varieties.

活性染料的水洗后处理是整个染色工艺过程的重要环节,对于染色织物的牢度及染色时间、能源、水的节约具有重要意义。活性染料的水洗过程一般包括冷水洗、热水洗、皂洗、热水洗、冷水洗等。皂洗以前要经过冷水洗和热水洗,这是稀释阶段,目的是尽可能去除织物上的盐、碱及纤维表面未固着的染料,这样可以使下一阶段的皂洗更有效,皂洗前要在醋酸浴中进行中和,可以防止染料在皂洗过程中水解,也可避免碱剂去除不净。The post-washing treatment of reactive dyes is an important part of the whole dyeing process, which is of great significance to the fastness of dyed fabrics and the saving of dyeing time, energy and water. The washing process of reactive dyes generally includes cold water washing, hot water washing, soap washing, hot water washing, cold water washing, etc. Before soaping, wash with cold water and hot water. This is the dilution stage. The purpose is to remove as much as possible the salt, alkali and unfixed dyes on the surface of the fabric, which can make the next stage of soaping more effective. Neutralization in an acetic acid bath can prevent the dye from being hydrolyzed during the soaping process, and can also avoid unclean removal by alkaline agents.

皂洗过程是促使纤维内部未固着的水解染料扩散到纤维表面,同时解吸到洗涤液中。皂洗后应进行热水洗,冷水洗,进一步冲淡、去除粘附在纤维上的染料,使干燥后的织物上的未固着的染料尽可能少。The soaping process is to promote the unfixed hydrolyzed dye inside the fiber to diffuse to the surface of the fiber and desorb into the washing liquid at the same time. After soaping, it should be washed with hot water and cold water to further dilute and remove the dye adhered to the fiber, so that the unfixed dye on the dried fabric is as little as possible.

本发明由于所选用的净洗剂对未固着的活性染料和水解的活性染料具有良好的吸附能力,所以在工艺中省去皂洗前的热水洗工艺,由于净洗剂中含有壳聚糖,在酸性条件下,净洗剂带正电荷,对活性染料具有较高的吸附能力。所以皂洗工艺中pH应控制在5.0以下,皂洗之前省去酸洗,皂洗之后要用碳酸氢钠进行碱洗,使布面的pH为中性。In the present invention, because the selected cleaning agent has good adsorption capacity to unfixed reactive dyes and hydrolyzed reactive dyes, the hot water washing process before soaping is omitted in the process, because chitosan is contained in the cleaning agent, Under acidic conditions, the detergent is positively charged and has a high adsorption capacity for reactive dyes. Therefore, in the soaping process, the pH should be controlled below 5.0. Before soaping, pickling should be omitted, and after soaping, sodium bicarbonate should be used for alkaline washing to make the pH of the cloth surface neutral.

Claims (4)

1. the washing process of an active dye detergent is characterized in that:
1) preparation of detergent:
1.1) preparation of aqueous phase solution: at first shitosan is dissolved in that to obtain mass percent concentration in the acetum be 0.5~3% chitosan solution; Be 3~7% gelatin solution with the gelatin mass concentration that obtains soluble in water then; The deacetylation of described shitosan is 89~96%, and the volume ratio of acetum is 2~6%;
By shitosan: gelatin is (1~4): 1 mass ratio with chitosan solution mix with gelatin solution shitosan/gelatin solution;
1.2) emulsion preparation: by emulsifying agent: atoleine=1: the volume ratio of (100~300) adds the mixed solution that emulsifying agent gets atoleine and emulsifying agent in atoleine; Described emulsifying agent is sorbester p17 and Tween 80, and wherein the volume ratio of sorbester p17 and Tween 80 is (1~6): 1; Again by shitosan/gelatin solution: atoleine=1: the volume ratio of (4~8) joins shitosan/gelatin solution in the mixed solution of atoleine and emulsifying agent, gets emulsion at 25~35 ℃ of emulsification 10~25min;
1.3) crosslinking curing: in above-mentioned emulsion, dropwise add mass concentration and be 50% glutaraldehyde solution, the mass ratio of glutaraldehyde and shitosan is 1: (2~5) make micro-sphere crosslinked curing at 40~60 ℃ of crosslinked 2~5h;
1.4) post processing: wash product repeatedly with isopropyl alcohol and absolute ether and remove atoleine, be placed on then and dryly in 40~55 ℃ the baking oven obtain active dye detergent based on shitosan/gelatin composite material;
2) product after will dyeing is soaped, is dried after the alkali cleaning, hot water wash, Warm Wash through cold wash, acidity successively;
Normal temperature washing 1~3 lattice are adopted in described cold wash;
It is 1~2 lattice of in 40~60 ℃ the liquid of soaping, soaping that described acidity is soaped, and the pH value of the liquid of soaping is 3~5, and the consumption of detergent is 0.6~1.2g/l in the soap lye;
Described alkali cleaning is in 40~50 ℃ pH is 8~10 alkaline solution, to carry out alkali cleaning;
Described hot water wash is in 90~95 ℃ hot water, to wash 1~2 lattice;
Described Warm Wash is in 45~60 ℃ warm water, to wash 1~2 lattice.
2. the washing process of active dye detergent according to claim 1 is characterized in that: said acidity is soaped and adopted the pH value of acetic acid or hydrochloric acid conditioning solution in the step is 3~5.
3. the washing process of active dye detergent according to claim 1, it is characterized in that: said alkaline solution is sodium acid carbonate or sodium carbonate liquor.
4. the washing process of active dye detergent according to claim 1, it is characterized in that: said bake out temperature is 100~130 ℃.
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