CN116376317B - 耐晒型绿色液体分散染料及其制备方法 - Google Patents
耐晒型绿色液体分散染料及其制备方法 Download PDFInfo
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- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 1
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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
- C09B67/0041—Blends of pigments; Mixtured crystals; Solid solutions mixtures containing one azo dye
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- 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
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- 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
- C09B67/0066—Aqueous dispersions of pigments containing only dispersing agents
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- 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
- C09B67/0079—Azoic dyestuff preparations
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- 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
- C09B67/008—Preparations of disperse dyes or solvent dyes
- C09B67/0082—Preparations of disperse dyes or solvent dyes in liquid form
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- 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
- C09B67/0084—Dispersions of dyes
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- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0084—Dispersions of dyes
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Abstract
本发明属于染料领域,具体涉及一种耐晒型绿色液体分散染料及其制备方法。本发明的耐晒型绿色液体分散染料,其配方由以下重量含量的成分组成:5%~24%的黄色染料、6%~25%的蓝色染料,9~11%复合分散剂和作为余量的水;黄色染料和蓝色染料的重量之和占耐晒型绿色液体分散染料总重的28~32%。本发明的耐晒型绿色分散染料弥补了粉状分散染料废水污染严重、粉尘污染等弊端,在具有优良耐晒牢度的同时,还丰富了分散染料中较为缺乏的绿色品种。
Description
技术领域
本发明属于染料领域,涉及一种耐晒型绿色液体分散染料及其制备方法。
技术背景
分散染料为我国产销量最大的染料类别,在所有染料中占据不可撼动的地位。分散染料品种丰富,现有商品分散染料存在较多的黄、橙、红、紫、蓝等品种,而绿色品种较为匮乏,且大多数存在色光不全、耐晒牢度欠佳的问题,尤其在一些特殊环境如:沙漠、高山、海上、户外、车内等,对纺织品耐晒性能要求比较严苛,能够满足高耐晒要求的绿色分散染料品种数量非常有限,因此通常需要利用耐晒牢度优良的黄、蓝两种原色分散染料复配得到高耐晒牢度的绿色品种的分散染料。
近几年随着国家对节能减排的重视程度不断提升,加之印染行业在生产加工中产生的废水污染和能耗问题较为突出,传统的生产加工方式已不能满足绿色环保的应用需求。对于分散染料而言,传统粉状分散染料在生产加工时,由于其本身微溶于水,在染色应用时往往需要加入大量的分散剂,使染料聚集体得以分散,继而分散悬浮于水中,便于向纤维表面靠近吸附,扩散进入纤维内部,完成上染。在染色结束后,大量分散剂留存于染色残液中,增加印染废水的COD。此外,粉状分散染料在前期加工时还存在喷雾干燥这一工序,能耗大且存在粉尘污染问题,对操作人员的身体健康带来不利影响。为响应节能降碳、绿色环保的号召,开发出更加环保、节能、高品质的染料剂型与相关染色工艺迫在眉睫。
分散染料液体化是解决以上粉状染料高能耗、高碳排放的最佳方案,如今众多企业已经开始转向研发液体分散染料的生产工艺,液体分散染料较粉状分散染料具有低分散剂用量、无粉尘污染等优点,加工过程中省去了喷雾干燥工序,避免了粉尘污染的同时,保证了操作人员的身体健康,分散染料液体化已成为分散染料绿色环保发展的必然趋势。
分散染料液体化是以水为主要溶剂降低分散剂的使用量,少量分散剂的加入可能会导致液体分散染料的稳定性下降,出现染料团聚沉降的现象,影响应用性能。因此开发助剂含量低且储存稳定性高的液体染料,是当前染料制造企业的重点研究方向。
上述4只已知染料,均为常规的粉末固体状。黄色染料A的名称为C.I.分散黄54;蓝色染料B的名称为C.I.分散蓝77;蓝色染料C的名称为C.I.分散蓝73;可通过常规的市购获得。蓝色染料D的名称为分散蓝D5,其合成方法在《耐晒可碱洗分散染料的设计、合成与应用性能研究》中有相应告知。
发明内容
本发明解决的技术问题是提供一种耐晒型绿色液体分散染料及其制备方法,该绿色液体分散染料具有高耐晒牢度、高强度、稳储性好等特点。
为了解决上述技术问题,本发明提供一种耐晒型绿色液体分散染料,其配方由以下重量含量的成分组成:5%~24%的黄色染料、6%~25%的蓝色染料,9~11%复合分散剂和作为余量的水;
黄色染料和蓝色染料的质量之和占耐晒型绿色液体分散染料总重的28~32%;
所述黄色染料为:
所述蓝色染料为以下任一:
作为本发明的耐晒型绿色液体分散染料的改进:
黄色染料和蓝色染料的质量之和占耐晒型绿色液体分散染料总重的30%;
复合分散剂含量为10%(即,复合分散剂占耐晒型绿色液体分散染料总重的10%)。
作为本发明的耐晒型绿色液体分散染料的进一步改进:
所述复合分散剂为由分散剂MF、木质素类分散剂(85A)与分散剂萘酚聚氧乙烯醚按照4:3:1的质量比组成的复合分散剂。
木质素类分散剂(85A),即,木质素磺酸钠85A。
作为本发明的耐晒型绿色液体分散染料的进一步改进,为以下任一配方:
黄色染料A20%、蓝色染料B10%、复合分散剂10%、水60%;
黄色染料A22.5%、蓝色染料B7.5%、复合分散剂10%、水60%;
黄色染料A23.3%、蓝色染料B 6.7%、复合分散剂10%、水60%;
黄色染料A24%、蓝色染料B 6%、复合分散剂10%、水60%。
本发明还同时提供了上述耐晒型绿色液体分散染料的制备方法,包括以下步骤:
将配方所述的黄色染料、蓝色染料、复合分散剂和水加入至砂磨容器中,再加入砂磨用的锆珠;研磨时间为4~5h,研磨结束后,除去锆珠,得到耐晒型绿色液体分散染料。
本发明还同时提供了上述耐晒型绿色液体分散染料的制备方法:
锆珠的粒径为0.4~0.6mm,锆珠为配方重量的2±0.2倍。
具体而言:本发明选用一种高耐晒黄色分散染料及一种高耐晒蓝色分散染料形成组合1(染料A及染料B)、组合2(染料A及染料C)、组分3(染料A及染料D)三对组合进行复配研究,并进一步优化配方。
说明:本发明在制备过程中每研磨一段时间,从砂磨罐中用玻璃棒蘸取一滴,用50mL水进行稀释,用《染料扩散性能测试》(GB/T 27597-2011)检测研磨染料的扩散性能,研磨至4-5h时,用滤纸渗圈法检验研磨效果观察到,滤纸渗圈扩散均匀,中心无颗粒物残留,研磨完毕。用尼龙布过滤出砂磨罐中的锆珠,染液倒出至染料专用收集瓶中,得到绿色液体分散染料。
本发明采用的实验方法如下:
(1)本发明的耐晒型绿色液体分散染料适用于PET疏水性聚酯纤维的染色,其染色工艺为:从研磨好的绿色液体分散染料中取1-2g于容量瓶中,并加水定容至500mL,得染料原液;按1-2%owf的色度要求移取分散染料色浆,按浴比1:30-50加入水后转移至染色杯中,加入欲染色的PET织物放入高温高压染色仪中,按2℃/min的升温速度升温至90℃,再以1℃/min缓慢升温至130℃,保温1小时后降至室温,取出染色布样,洗涤。染色布样经还原清洗后按《纺织品色牢度测试耐人造光色牢度:氙弧》(GB/T 8427-2008)测试其耐晒牢度。
(2)观察布样色光并采用GB/T6688-2008中规定的方法测其染料强度,用紫外可见分光光度计UV-2550测其染色残液在波长为380-750nm的色度abs值,用GB11914-89化学需氧量一重铬酸盐法测定其染色残液COD。
(3)得到的绿色液体分散染料在常温下进行常温放置,观察其出现沉淀的时间及测试其粒径变化。粒径测试方法为:取0.5g研磨好的初始绿色液体分散染料及放置一段时间的液体分散染料,用水稀释2万倍,经粒度仪测试其粒径。
本发明的绿色液体分散染料适用于涤纶织物的染色和印花,特别适用于涤纶织物染色的自动化生产。本发明的耐晒型绿色分散染料弥补了粉状分散染料废水污染严重、粉尘污染等弊端,同时作为复配的绿色分散染料,采用高耐晒黄色分散染料、及若干只蓝色分散染料进行复配,得到一系列耐晒牢度高的绿色分散染料,具有优良耐晒牢度的同时,还丰富了分散染料中较为缺乏的绿色品种。
本发明通过筛选配伍性好的高耐晒黄、蓝单色染料,通过分散体系复配与液体染料制备工艺研究,开发获得一种高强度、稳储、染色性能优异的高耐晒绿色液体分散染料。
具体实施方法
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此:
实施例1-1、耐晒型绿色液体分散染料的制备方法,按以下步骤进行:
准确称取15g黄色染料A和15g蓝色染料B,以及10g的复合分散剂(由5g MF、3.75g85A及1.25g萘酚聚氧乙烯醚组成),全部加入到150mL砂磨罐中,再向砂磨罐中加入60mL的水,开启研磨机进行研磨,边研磨边从上口处缓慢加入200g锆珠。研磨期间每隔1h从上口处用玻璃棒沾取少量研磨染料,点到滤纸上观察渗圈情况,研磨至4h时,观察到滤纸渗圈均匀,渗圈中心无颗粒物残留,研磨结束。取20cm×20cm的细尼龙布,折叠成漏斗形状固定于收集瓶之上,将研磨后的所得物进行过滤,收集瓶中所得为高耐晒型绿色液体分散染料;锆珠停留在尼龙布上,后对尼龙布和锆珠进行常规清洗。
实验1
(1)从实施例1-1所得的绿色液体分散染料中取2g于容量瓶中,并加水定容至500mL,得染料原液;按2%owf的色度要求移取分散染料色浆,按浴比1:50加入水后转移至染色杯中,加入欲染色的1g PET织物放入高温高压染色仪中,按2℃/min的升温速度升温至90℃,再以1℃/min缓慢升温至130℃,保温1小时后降至室温,取出染色布样,洗涤。
染色布样按照国家标准《分散染料染色色光和强度的测定方法》(GB/T 2394-1980)要求进行还原清洗,还原清洗后的布样进行按照《纺织品色牢度测试耐人造光色牢度:氙弧》(GB/T8427-2008)测试耐晒牢度,测试结果显示其耐晒牢度为6-7级。
(2)观察染色布样色光并采用GB/T6688-2008中规定的方法测其染料强度为104.2,用紫外可见分光光度计UV-2550测其染色残液在波长为380-750nm的色度abs值为62.127,用GB11914-89化学需氧量一重铬酸盐法测定其染色残液COD值为1462。
(3)得到的绿色液体分散染料在常温(20~25℃)下进行放置,观察其在80~100天出现明显沉淀,放置165天时粒径与初始粒径比增加了约103nm,即,初始粒径为205nm,165天时粒径为308nm。
(4)按照GB/T2374-2017,取染色后涤纶布样进行色光的检测,其L*、a*、b*的数据分别为37.56、-18.74、15.08,因此判定成为绿色染料。
实验2、单色染料:单色的黄色染料A、蓝色染料B、蓝色染料C、蓝色染料D作为单色染料分别进行如下操作:
取单色染料30g替代实施例1-1中的“15g黄色染料A和15g蓝色染料B”,其余按照实施例1-1的制备工艺,制备所得的所得液体分散染料按照上述实验1所述方法进行测试,测试数据如表1所示。
表1
实施例1-2~实施例1-10,
仅仅改变实施例1-1高耐晒型绿色液体分散染料的配方中的黄色染料A重量和蓝色染料B重量,具体如下表2所述,其余等同于实施例1。分别获得相应的实施例1-2~实施例1-10所述的高耐晒型绿色液体分散染料。根据其L*、a*、b*的数据,均判定成为绿色染料。
按照实验1所述方法对上述绿色液体分散染料进行性能测试,所得结果见表1。
表2
实施例2-1~实施例2-10:
将实施例1-1~实施例1-10中的蓝色染料B改成蓝色染料C,其余等同;从而相应分别获得实施例2-1~实施例2-10所述的高耐晒型绿色液体分散染料。根据其L*、a*、b*的数据,均判定成为绿色染料。
按照实验1所述方法对上述绿色液体分散染料进行性能测试,所得结果见表3。
表3
实施例3-1~实施例3-10:
将实施例1-1~实施例1-10中的蓝色染料B改成蓝色染料D,其余等同;从而相应分别获得实施例3-1~实施例3-10所述的高耐晒型绿色液体分散染料。根据其L*、a*、b*的数据,均判定成为绿色染料。
按照实验1所述方法对上述绿色液体分散染料进行性能测试,所得结果见表4。
表4
对比表1中4只染料单独使用和表2~4染料复配使用情况可看出,组合1(染料A及染料B)、组合2(染料A及染料C)、组合3(染料A及染料D)得到的复配染料较单色染料的日晒牢度及沉淀时间有所提高。根据表2~表4可知,3类复配组合得到的绿色液体分散染料具有染色强度高、染色脚水色度浅、COD低、节能环保、不易沉淀、耐晒牢度优良等特点。表2(实施例1-1~实施例1-10)得到的一系列绿色分散染料染色强度均高于表3(实施例2-1~实施例2-10)和表4(实施例3-1~实施例3-10),脚水色度abs值及脚水COD均低于表2和表2,且表2耐晒牢度均达到了6-7级及7级,各项指标均优于表3和表4,是3个复配组合中的最优组合。且表2中实施例1-7~实施例1-10各项指标最优,为优选复配比例。
对比例1、仅仅采用粉状黄色染料A与粉状蓝色染料B按照实施例1-7~实施例1-10的复配比例配置成粉状复合染料,将实验1中的“绿色液体分散染料取2g”改成“粉状复合染料取2g”,其余等同于实验1的测试方法,对涤纶纤维进行染色,所得染色强度、脚水色度abs值及脚水COD值如表5所示。
表5
根据表5与表2对比,可得知:绿色粉状复合染料的脚水色度abs值与脚水COD相较于本发明的绿色液体复合染料有明显的增高,加剧了废水处理的负担,不利于节能减排。
对比例2、将黄色染料A改用另一种高耐晒黄色染料X(C.I.分散黄56)代替,其余参照实施例1-7~实施例1-10,所得结果为如下表6所示。
表6
根据表6与表2对比,可得知:改用黄色染料X与蓝色染料B按照优选比例进行复配,得到的绿色分散染料的脚水色度abs值及脚水COD均高于本发明实施例1-7~实施例1-10所得到绿色液体分散染料,不利于绿色环保,同时储存过程中出现沉淀的时间早于实施例1-7~实施例1-10所得到绿色液体分散染料,染色强度和耐日晒牢度也不及本发明。
最后,还需要注意的是,以上列举的仅是本发明的若干个具体实施例。显然,本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (6)
1.耐晒型绿色液体分散染料,其特征在于耐晒型绿色液体分散染料的配方由以下重量含量的成分组成:5%~24%的黄色染料、6%~25%的蓝色染料,9~11%复合分散剂和作为余量的水;
黄色染料和蓝色染料的重量之和占耐晒型绿色液体分散染料总重的28~32%;
所述黄色染料为:;
所述蓝色染料为以下任一:、/>。
2.根据权利要求1所述的耐晒型绿色液体分散染料,其特征在于:
黄色染料和蓝色染料的重量之和占耐晒型绿色液体分散染料总重的30%;
复合分散剂含量为10%。
3.根据权利要求1或2所述的耐晒型绿色液体分散染料,其特征在于:
所述复合分散剂为由分散剂MF、木质素类分散剂85A与分散剂萘酚聚氧乙烯醚按照4:3:1的重量比组成的复合分散剂。
4.根据权利要求3所述的耐晒型绿色液体分散染料,其特征在于为以下任一配方:
黄色染料A20%、蓝色染料B 10% 、复合分散剂10%、水60%;
黄色染料A22.5%、蓝色染料B7.5 %、复合分散剂10%、水60%;
黄色染料A23.3%、蓝色染料B 6.7 %、复合分散剂10%、水60%;
黄色染料A24%、蓝色染料B 6%、复合分散剂10%、水60%。
5.如权利要求1~4任一所述的耐晒型绿色液体分散染料的制备方法,其特征在于包括以下步骤:
将配方所述的黄色染料、蓝色染料、复合分散剂和水加入至砂磨容器中,再加入砂磨用的锆珠;研磨时间为4~5h,研磨结束后,除去锆珠,得到耐晒型绿色液体分散染料。
6.根据权利要求5所述的耐晒型绿色液体分散染料的制备方法,其特征在于:
锆珠的粒径为0.4~0.6 mm,锆珠为配方重量的2±0.2倍。
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