CN109486329B - 一种荧光涂料及其制备方法与应用 - Google Patents
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Abstract
本发明公开了一种荧光涂料及其制备方法与应用,属于荧光涂料技术领域,本发明采用一种低毒、稳定性能好的疏水改性铜微粒作为分散剂,相比于传统的分散剂,疏水改性铜颗粒不溶于水,环保低毒,能够稳定地存在于油/水界面,有效地阻止微滴之间的聚集,从而起到稳定发光颜料的目的,另外采用pickering乳液聚合方法制备出该分散剂并应用于荧光涂料,可大大减少荧光涂料制备过程中表面活性剂、稳定剂等助剂的使用量,更加环保,荧光涂料耐紫外线性能提高;同时,该荧光涂料应用在织物上时可降低传统粘合剂的用量,同时织物具有柔软、透气的优点。
Description
技术领域:
本发明涉及一种新型荧光涂料,特别是涉及一种低毒、抗紫外的荧光涂料、制备方法及在纺织品上的应用。
背景技术:
荧光涂料是由成膜物质、发光颜料及助剂组成的一种功能性涂料。目前,用于荧光涂料的助剂通常包括流平剂、增稠剂、表面活性剂、分散剂、催干剂、稳定剂以及填料等。由于发光颜料通常不溶于水,且耐光性差,为了延长其使用寿命,提高荧光涂料在织物上的使用性能,常常需要加入大量的光稳定剂、分散剂、乳化剂等助剂,来帮助发光颜料在水中的均匀分散及稳定,如聚氨酯、烷基苯基磺酸盐、烷基磷酸酯。这些助剂的大量使用对环境造成一定的负面影响。
另一方面,荧光涂料在使用到纺织品上,尤其是服装时,为了提高其水洗牢度会使用较多的粘合剂,这将造成织物手感发硬,透气性和舒适性大大降低。
发明内容:
本发明的第一方面目的是提供一种环保低毒、且能有效降低助剂使用量的荧光涂料。
本发明采取的技术方案如下:
一种荧光涂料,其特征在于,包括按质量百分比的下述组成:
进一步的设置在于:
所述铜微粒分散剂与玫瑰精B的质量比为3:1.
本发明第二方面目的是提供一种荧光涂料的制备方法,其特征在于,包括以下步骤:
(1)制备改性铜微粒分散剂:
将无水乙醇和水配制成混合液,称取六甲基二硅胺烷在搅拌下加入上述混合液中,加入L-抗坏血酸,搅拌至完全溶解;将上述混合溶液转移至装有磁力搅拌、冷凝回流的三口烧瓶中,开始加热搅拌,取无水硫酸铜加入其中,加热回流,冷却至室温,离心分离,用无水乙醇洗涤,真空干燥,得到疏水改性铜微粒分散剂;
(2)制备荧光涂料:
将玫瑰精B分散到含有2,2’-偶氮二异丁腈、丙烯酸丁酯和苯乙烯的混合溶液中,然后将该混合溶液加热,加入上述制备的改性铜微粒分散剂和适量的蒸馏水,在高速搅拌下反应得到悬浮分散液;转移到氮气保护的玻璃反应釜中,反应得到荧光涂料微胶囊胶乳;
在荧光涂料微胶囊胶乳中,加入十二烷基苯磺酸钠、乙二醇及去离子水,充分搅拌,然后在室温下放置,再转移到砂磨机中研磨,即可得荧光涂料。
进一步地:
一种荧光涂料的制备方法,其特征在于:
(1)、制备改性铜微粒分散剂:
将无水乙醇和水按体积比1:1的比例配制50mL混合液,称取4.0347g的六甲基二硅胺烷在搅拌下加入上述混合液中,加入5.283g的L-抗坏血酸,搅拌至完全溶解;将上述混合溶液转移至装有磁力搅拌、冷凝回流的三口烧瓶中,开始加热搅拌,用滴液漏斗缓慢加入0.5mol/L五水硫酸铜溶液50mL,然后待搅拌均匀并且温度升至85℃时加热回流2.5h,冷却至室温,离心分离,用无水乙醇洗涤3次,真空干燥24h,得到改性铜微粒分散剂;
(2)、制备荧光涂料:
荧光涂料配方,按重量百分比的下述组成:
制备方法如下:
将玫瑰精B分散到含有2,2’-偶氮二异丁腈、丙烯酸丁酯和苯乙烯的混合溶液中,在0~4℃水浴中超声分散20次,每次5s。然后将该混合溶液加热到40℃,同时加入上述制备的改性铜微粒分散剂和适量的蒸馏水,在高速搅拌下反应30min得到悬浮分散液,转移到氮气保护的玻璃反应釜中,升温至90℃反应30min,得到荧光涂料微胶囊胶乳;
在荧光涂料微胶囊胶乳中,加入十二烷基苯磺酸钠、乙二醇及去离子水,在40℃、转速500转/min的条件下充分搅拌45~60min,然后在室温下放置4小时,再转移到砂磨机中研磨2分钟,砂磨机转速3000转/分钟,即可得荧光涂料。
本发明的第三方面目的是提供一种荧光涂料在纯棉织物上的应用,其特征在于,包括以下步骤:将质量分数10%荧光涂料、质量分数5%粘合剂和质量分数5%增稠剂及适量的水调成印花色浆,对全棉织物进行手工刮印,织物在80℃烘干3-5min,焙烘温度100-150℃时间2-3min。
进一步地:焙烘温度110℃,时间2min。
本发明的有益效果如下:
本发明制备一种低毒、稳定性能好的疏水改性铜微粒作为分散剂,相比于传统的分散剂,疏水改性铜颗粒不溶于水,环保低毒,能够稳定地存在于油/水界面,有效地阻止微滴之间的聚集,从而起到稳定发光颜料的目的;采用pickering乳液聚合方法制备出该分散剂并应用于荧光涂料,可大大减少荧光涂料制备过程中表面活性剂、稳定剂等助剂的使用量,更加环保,荧光涂料耐紫外线性能提高;同时,该荧光涂料应用在织物上时可降低传统粘合剂的用量,同时织物具有柔软、透气的优点。
以下结合具体实施方式对本发明做进一步说明。
具体实施方式:
实施例1:
1、制备改性铜微粒分散剂:
将无水乙醇和水按体积比1:1的比例配制50mL混合液,称取4.0347g的六甲基二硅胺烷(HMDS)在搅拌下加入上述混合液中,加入5.283g的L-抗坏血酸,搅拌至完全溶解。将上述混合溶液转移至装有磁力搅拌、冷凝回流的三口烧瓶中,开始加热搅拌,用滴液漏斗缓慢加入0.5mol/L五水硫酸铜溶液50mL,然后待搅拌均匀并且温度升至85℃时加热回流2.5h,冷却至室温,离心分离,用无水乙醇洗涤3次,真空干燥24h,得到改性铜微粒分散剂。
2、制备荧光涂料:
荧光涂料配方(重量百分比):
制备方法如下:
将玫瑰精B分散到含有2,2’-偶氮二异丁腈、丙烯酸丁酯和苯乙烯的混合溶液中,在0~4℃水浴中超声分散20次,每次5s。然后将该混合溶液加热到40℃,同时加入上述制备的改性铜微粒分散剂和适量的蒸馏水,在高速搅拌下反应30min得到悬浮分散液,转移到氮气保护的玻璃反应釜中,升温至90℃反应30min,得到荧光涂料微胶囊胶乳;
在荧光涂料微胶囊胶乳中,加入十二烷基苯磺酸钠、乙二醇及去离子水,在40℃、转速500转/min的条件下充分搅拌45~60min,然后在室温下放置4小时,再转移到砂磨机中研磨2分钟,砂磨机转速3000转/分钟,即可得荧光涂料。
3、荧光涂料在纯棉织物上的应用:
将质量分数10%荧光涂料、质量分数5%粘合剂和质量分数5%增稠剂及适量的水调成印花色浆,对全棉织物进行手工刮印,织物在80℃烘干3-5min,焙烘温度100-150℃时间2-3min。印花后棉织物具有优异的荧光性能及耐水洗性,耐皂洗色牢度达到4级;而且具有柔软的手感,棉织物的抗紫外线性能得到提高。
对比例1:采用市售荧光红涂料在纯棉织物上印花
将质量分数:10%的市售荧光红涂料和质量分数20%粘合剂、质量分数5%增稠剂和水调成印花色浆,对全棉织物进行手工刮印,织物在80℃烘干5min,焙烘温度110℃时间2min。
对比例2:将质量分数15%的市售荧光红涂料和质量分数20%粘合剂、质量分数5%增稠剂和水调成印花色浆,对全棉织物进行手工刮印,织物在80℃烘干5min,焙烘温度110℃时间2min。
上述实施例中,粘合剂选择市售涂料印花粘合剂YH-50B,增稠剂选择市售涂料印花增稠剂HR-1411。
将本发明实施例和对比例印花后的织物分别进行检测,测试印花后织物的K/S值、荧光性能、耐水洗色牢度、耐摩擦色牢度及防紫外线性能,具体检测方法如下,检测结果如表2所示:
K/S值的测定利用DataColor 600电脑测色配色仪,采用D65光源和10o视场条件测定,织物折叠4层,取四个不同的点测定后取平均值。
织物的荧光性能测定参照GB 20653-2006《职业用高可视性警示服》方法评价,色彩应处于表1所述的一个色彩区域当中,最小亮度系数应超过表1最小的相应值。
表1、基底材料要求:
其中,x,y和β值通过Datacolor 600电脑测色配色仪采用D65光源和2o视场角测定。
耐水洗色牢度测试:按GB/T3920—2008《纺织品色牢度试验耐皂洗色牢度》第1号说明测试。
耐摩擦色牢度测试:按GB/T3920—2008《纺织品色牢度试验耐摩擦色牢度》测试。
防紫外线性能参照AS/NZS 4399:1996《防紫外线面料的评估和分类》测试织物的UVA透过率。UVA透过率越小,则防紫外线性能越好。
表2、本发明的荧光红涂料与常规荧光红涂料的性能对比
如表2所示,本发明制备的荧光涂料应用于纯棉织物,对比市售的荧光红涂料,在K/S值、荧光性能(亮度系数)、耐水洗色牢度、耐摩擦色牢度、手感及防紫外线性能(UVA透过率)均有显著提高,分析其原因:含有铜微粒的分散剂在荧光涂料中起到良好的分散效果,荧光涂料分布更加均匀,所以织物的荧光性格更优,改性铜分散剂在织物表面也有较好的成膜性能,所以织物耐水洗、耐摩擦色牢度提高,防紫外线性能提高。
玫瑰精B与分散剂的配比对荧光涂料性能的影响:
基于实施例1,区别在于:调整荧光涂料中玫瑰精B与改性铜微粒分散剂的质量比,并分别检测涂料印花后织物荧光涂料性能,如表3所示:
表3
如表3所示:调整玫瑰精B与改性铜分散剂的质量比制备出荧光涂料,并测试涂料稳定性及粒径大小,发现当玫瑰精质量为10%,改性铜微粒分散剂质量为30%时制备的荧光涂料稳定性最好,粒径较小。当改性铜分散剂用量较低而玫瑰精用量过高时会造成涂料稳定剂较差,放置时间较长后会出现分层和沉淀,影响涂料的使用。
涂料印花工艺对于涂料性能的影响:
基于实施例1,区别在于:调整棉织物的涂料印花工艺条件,并分别检测荧光涂料性能,如表4所示:
表4
如表4所示:焙烘温度及焙烘时间,对印花后棉织物的各项性能有显著影响,发现随着焙烘温度的提高焙烘时间的延长,织物的K/S值及荧光性能(亮度系数)、防紫外线性能(UVA透射比)略有增加,但是织物的手感下降明显,这可能是因为长时间高温处理会使得粘合剂发硬造成织物手感变差。
Claims (6)
1.一种荧光涂料,其特征在于,包括按质量百分比的下述组成:
改性铜微粒分散剂 20~40
玫瑰精B 5~15
2,2’-偶氮二异丁腈 1~3
丙烯酸丁酯 3~8
苯乙烯 3~8
十二烷基苯磺酸钠 5~10
乙二醇 5~10
余量为去离子水;
所述改性铜微粒分散剂,采用以下方法制备:
将无水乙醇和水配制成混合液,称取六甲基二硅胺烷在搅拌下加入上述混合液中,加入L-抗坏血酸,搅拌至完全溶解;将上述混合溶液转移至装有磁力搅拌、冷凝回流的三口烧瓶中,开始加热搅拌,取无水硫酸铜加入其中,加热回流,冷却至室温,离心分离,用无水乙醇洗涤,真空干燥,得到疏水改性铜微粒分散剂。
2.根据权利要求1所述的一种荧光涂料,其特征在于:所述改性铜微粒分散剂与玫瑰精B的质量比为3:1。
3.一种荧光涂料的制备方法,其特征在于,包括以下步骤:
(1)制备改性铜微粒分散剂:
将无水乙醇和水配制成混合液,称取六甲基二硅胺烷在搅拌下加入上述混合液中,加入L-抗坏血酸,搅拌至完全溶解;将上述混合溶液转移至装有磁力搅拌、冷凝回流的三口烧瓶中,开始加热搅拌,取无水硫酸铜加入其中,加热回流,冷却至室温,离心分离,用无水乙醇洗涤,真空干燥,得到疏水改性铜微粒分散剂;
(2)制备荧光涂料:
将玫瑰精B分散到含有2,2’-偶氮二异丁腈、丙烯酸丁酯和苯乙烯的混合溶液中,然后将该混合溶液加热,加入上述制备的改性铜微粒分散剂和适量的蒸馏水,在高速搅拌下反应得到悬浮分散液;转移到氮气保护的玻璃反应釜中,反应得到荧光涂料微胶囊胶乳;
在荧光涂料微胶囊胶乳中,加入十二烷基苯磺酸钠、乙二醇及去离子水,充分搅拌,然后在室温下放置,再转移到砂磨机中研磨,即可得荧光涂料。
4.根据权利要求3所述的一种荧光涂料的制备方法,其特征在于:
(1)、制备改性铜微粒分散剂:
将无水乙醇和水按体积比1:1的比例配制50mL混合液,称取4.0347g的六甲基二硅胺烷在搅拌下加入上述混合液中,加入5.283g的L-抗坏血酸,搅拌至完全溶解;将上述混合溶液转移至装有磁力搅拌、冷凝回流的三口烧瓶中,开始加热搅拌,用滴液漏斗缓慢加入0.5mol/L五水硫酸铜溶液50mL,然后待搅拌均匀并且温度升至85℃时加热回流2.5 h,冷却至室温,离心分离,用无水乙醇洗涤3次,真空干燥24 h,得到改性铜微粒分散剂;
(2)、制备荧光涂料:
荧光涂料配方,按重量百分比的下述组成:
改性铜微粒分散剂 30
玫瑰精B 10
2,2’-偶氮二异丁腈 2
丙烯酸丁酯 5
苯乙烯 5
十二烷基苯磺酸钠 5
乙二醇 5
余量为去离子水;
制备方法如下:
将玫瑰精B分散到含有2,2’-偶氮二异丁腈、丙烯酸丁酯和苯乙烯的混合溶液中,在0~4℃水浴中超声分散20次,每次5s,然后将该混合溶液加热到40℃,同时加入上述制备的改性铜微粒分散剂和适量的蒸馏水,在高速搅拌下反应30min得到悬浮分散液,转移到氮气保护的玻璃反应釜中,升温至90℃反应30min,得到荧光涂料微胶囊胶乳;
在荧光涂料微胶囊胶乳中,加入十二烷基苯磺酸钠、乙二醇及去离子水,在40℃、转速500转/min的条件下充分搅拌45~60min,然后在室温下放置4小时,再转移到砂磨机中研磨2分钟,砂磨机转速3000转/分钟,即可得荧光涂料。
5.一种权利要求1所述荧光涂料在纯棉织物上的应用,其特征在于,包括以下步骤:将质量分数10%荧光涂料、质量分数5%粘合剂和质量分数5%增稠剂及适量的水调成印花色浆,对全棉织物进行手工刮印,织物在80℃烘干3-5min,焙烘温度100-150℃时间2-3min。
6.根据权利要求5所述的一种荧光涂料在纯棉织物上的应用,其特征在于:焙烘温度110℃,时间2min。
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