CN113668231A - 一种改性纳米氧化锌及其制备方法和应用 - Google Patents

一种改性纳米氧化锌及其制备方法和应用 Download PDF

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CN113668231A
CN113668231A CN202110975482.2A CN202110975482A CN113668231A CN 113668231 A CN113668231 A CN 113668231A CN 202110975482 A CN202110975482 A CN 202110975482A CN 113668231 A CN113668231 A CN 113668231A
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zinc oxide
nano zinc
modified nano
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廖师琴
杨陈
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Jiangxi Institute of Fashion Technology
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Abstract

本发明公开了一种改性纳米氧化锌，并公开了其制备方法和在配置成织物整理剂整理织物的应用。本发明以纳米氧化锌为核心，其本身，具有良好的紫外线屏蔽性和优越的抗菌、抑菌性能，添加入织物中，能赋予织物以防晒、抗菌、除臭等功能，同时能提供抗皱性和耐水洗性能。进行改性后，提高了防紫外线的效果，增强材料的弹性及持久耐用性，同时增大材料的可使用范围，增加抗菌性能。本发明制备方法简单，易于进行大规模生产使用。将本发明制得的改性纳米氧化锌应用于作为织物整理剂整理织物，整理后的织物的防紫外线性能、抗拉性和韧性均可以大幅提升，延长了织物的使用寿命。

Description

一种改性纳米氧化锌及其制备方法和应用
技术领域
本发明属于纺织技术领域，具体涉及一种改性纳米锌及其制备方法和应用。
背景技术
随着技术发展和社会的不断进步，人们在生活水平大大提高的同时，对生活质量的要求也越来越高。全球环境遭到破坏的今天，返璞归真，回归大自然已经成为人们衡量生活质量的重要标准，人们越来越追求织物的多功能性。露天环境下，紫外线对人体皮肤损害很大，高强度或者长时间的户外生活中，皮肤会因为紫外线产生各种问题，甚至造成癌症。
目前市场中常见的制作防紫外线面料的技术手段主要有两种：一种为在纺丝时混入防紫外线材料以达到防紫外线的效果；另一种为利用后整理的方法对织物进行防紫外线整理。后整理方法中最常见的为利用涂层技术在织物表面涂覆一层材料，涂覆材料一般为黑胶、银胶或其他具有防紫外线效果的材料。但是目前的织物处理后防紫外线和韧性较差，无法达到使用的要求。
发明内容
为此，本发明的所要解决的技术问题是现有防紫外线织物防护效果不佳，韧性不好的缺陷，进而提供了一种改性纳米锌及其制备方法和配置成织物整理剂整理织物的应用。
为解决上述技术问题，本发明采用的技术方案如下：
本发明提供一种改性纳米氧化锌，包括如下重量份数的原料：
Figure BDA0003227474600000021
优选地，由如下重量份数的原料组成：
纳米氧化锌40份；
溶剂10份；
碳酸氢钠9份；
抗菌剂6份；
纳米晶纤维素8份；
抗紫外线剂3份；
复合改性剂6份。
进一步地，所述溶剂为乙醇；
所述抗菌剂为壳聚糖；
所述抗紫外线剂由氯乙烯-醋酸乙烯酯共聚乳液、2,4-二氯苯甲酸、微孔木质素和纳米二氧化钛组成；
所述所述复合改性剂由蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土组成。
优选地，
所述抗紫外线剂中氯乙烯-醋酸乙烯酯共聚乳液、2,4-二氯苯甲酸、微孔木质素和纳米二氧化钛的质量比为3:2:2:3；
所述复合改性剂中蓖麻油酸酯硫酸钠、十二水硫酸铝钠和氧化石墨烯-凹凸棒土的质量比为0.5-1.5:0.5-1.5:0.25-0.75。
本发明还提供上述改性纳米氧化锌的制备方法，包括如下步骤：
S1：将纳米氧化锌、溶剂、碳酸氢钠混合，得到纳米氧化锌分散液；
S2：在分散液中加入抗菌剂、纳米晶纤维素，充分混合后水浴加热，得到第一混合液；
S3：在第一混合液中加入复合改性剂，然后进行超声处理，得到第二混合液；
S4：在第二混合液中加入抗紫外线剂混合，得到改性纳米氧化锌液；
S5：最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，即得到所述改性纳米氧化锌。
进一步地，步骤S1中所述混合是在搅拌罐中进行加热分散，分散温度为45-55℃，搅拌速率为600-800转/分，时间为12min-22min。
步骤S2中所述水浴温度为60-70℃，时间为10min-18min；
步骤S3中超声处理时，频率为60-80KHz，时间20-40min；
步骤S4中所述混合的温度为常温。
优选地，步骤S5中得到的所述改性纳米氧化锌粒径为20-30nm。
本发明还公开了上述改性纳米氧化锌的应用，应用于配置成织物整理剂整理织物。
本发明技术方案具备以下优点：
(1)本发明以纳米氧化锌为核心，其本身，具有良好的紫外线屏蔽性和优越的抗菌、抑菌性能，添加入织物中，能赋予织物以防晒、抗菌、除臭等功能，同时能提供抗皱性和耐水洗性能。本发明在里面再添加抗紫外线剂，起到了复合防紫外线的效果，达到1+1>2的效果。同时也弥补了单一纳米氧化锌防紫外线时对防紫外线波长选择性吸收反射这一效果不足的弊病。有助于增加对紫外线各个波长的吸收和反射；碳酸氢钠是制作纳米氧化锌的原料，这里添加的碳酸氢钠有助于保持纳米氧化锌的稳定；加入纳米结晶纤维素有助于增强材料的弹性及持久耐用性，且大幅度提高了其强度，从而增大材料的可使用范围。
(2)本申请限定抗菌剂为壳聚糖，溶解后的壳聚糖呈凝胶状态，具有较强的吸附能力，在增加纳米氧化锌抗菌效果的同时，可在一定程度上缓解氧化锌的分解，延长使用时间，有助于提高材料的使用寿命；限定了复合改性剂的成分，其中的氧化石墨烯成分在添加入纳米氧化锌中后，由于氧化石墨烯整齐结构，造成其比表面积大、强度高，从而引起整体材料的强力的提升。
(3)本申请还限定了抗紫外线剂中的组分，其中氯乙烯-醋酸乙烯酯共聚乳液是一种改性的聚氯乙烯乳液，具有软化温度较低、流动性好、柔韧性较好、溶解性能好、制品的尺寸稳定性好,还具有一定的内增性作用等优点，在此抗紫外线剂里只做溶剂使用；而2,4-二氯苯甲酸是做为制造改抗紫外线剂中间体存在；微孔木质素和二氧化钛是作用于抗紫外线，两者相辅相成结合使用，抗紫外线效果才会更好；微孔木质素主要在此中的作用主要是吸收紫外线，因为微孔木质素有较好的吸附降解功能，辅助二氧化钛，在二氧化钛反射和吸收紫外线达到极限后，起到了候补吸收分解剩余的紫外线功效，使整体试剂抗紫外线安全性更为提高；当将该限定组分的抗紫外线剂应用于纳米氧化锌时，能使其表面性质发生变化，其原料相互配合，改善了纳米氧化锌表面性能，增加纳米颗粒与基体之间的相容性。
(2)本发明制备方法简单，易于进行大规模生产使用。
(3)将本发明制得的改性纳米氧化锌应用于作为织物整理剂整理织物，整理后的织物的防紫外线性能、抗拉性和韧性均可以大幅提升，延长了织物的使用寿命。
具体实施方式
提供下述实施例是为了更好地进一步理解本发明，并不局限于所述最佳实施方式，不对本发明的内容和保护范围构成限制，任何人在本发明的启示下或是将本发明与其他现有技术的特征进行组合而得出的任何与本发明相同或相近似的产品，均落在本发明的保护范围之内。
实施例中未注明具体实验步骤或条件者，按照本领域内的文献所描述的常规实验步骤的操作或条件即可进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规试剂产品。
各实施例中使用的纳米晶纤维素购自河南多希化工贸易有限公司。
各实施例中使用的氯乙烯-醋酸乙烯酯共聚乳液购自上海奥克化学有限公司。
各实施例中使用的微孔木质素购自上海阿拉丁生化科技股份有限公司。
各实施例中使用的氧化石墨烯-凹凸棒土购自德国巴斯夫,型号为Attagel50。
试验例中使用的织物为浙江美欣达印染集团股份有限公司生产的300D聚酯纤维织物。
实施例1
本实施例提供一种改性纳米氧化锌，其原料包括纳米氧化锌20g、乙醇4g、碳酸氢钠3g、壳聚糖2g、纳米晶纤维素4g、抗紫外线剂1g和复合改性剂2g。
其中，抗紫外线剂由30wt％氯乙烯-醋酸乙烯酯共聚乳液、20wt％2,4-二氯苯甲酸、20wt％微孔木质素、20％纳米二氧化钛组成。
复合改性剂采用蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土，其质量比为1:1:0.5。
具体制备方法如下：
(1)首先将纳米氧化锌、乙醇、碳酸氢钠放入搅拌罐中进行加热分散，分散温度为45℃，搅拌速率为600转/分，时间为12min，得到纳米氧化锌分散液；
(2)在分散液中加入壳聚糖、纳米晶纤维素，充分混合后加入水浴锅中水浴加热，水浴加热温度为60℃，时间为10min，得到混合液A；
(3)在混合液A中加入复合改性剂，混合后将混合液加入超声波发生器进行超声处理，超声频率为60KHz，超声时间20min，得到混合液B；
(4)在混合液B中加入抗紫外线剂，在常温下充分混合后，得到改性纳米氧化锌液；
(5)最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，得到粒径为20-30nm的改性纳米氧化锌。
实施例2
本实施例提供一种改性纳米氧化锌，其原料包括纳米氧化锌40g、乙醇10g、碳酸氢钠9g、壳聚糖6g、纳米晶纤维素8g、抗紫外线剂3g和复合改性剂6g。
其中，抗紫外线剂由30wt％氯乙烯-醋酸乙烯酯共聚乳液、20wt％2,4-二氯苯甲酸、20wt％微孔木质素、20％纳米二氧化钛组成。
复合改性剂采用蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土，其质量比为1:1:0.5。
具体制备方法如下：
(1)首先将纳米氧化锌、乙醇、碳酸氢钠放入搅拌罐中进行加热分散，分散温度为55℃，搅拌速率为800转/分，时间为22min，得到纳米氧化锌分散液；
(2)在分散液中加入壳聚糖、纳米晶纤维素，充分混合后加入水浴锅中水浴加热，水浴加热温度为70℃，时间为18min，得到混合液A；
(3)在混合液A中加入复合改性剂，混合后将混合液加入超声波发生器进行超声处理，超声频率为80KHz，超声时间40min，得到混合液B；
(4)在混合液B中加入抗紫外线剂，在常温下充分混合后，得到改性纳米氧化锌液；
(5)最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，得到粒径为20-30nm的改性纳米氧化锌。
实施例3
本实施例提供一种改性纳米氧化锌，其原料包括纳米氧化锌25g、乙醇5g、碳酸氢钠4g、壳聚糖3g、纳米晶纤维素5g、抗紫外线剂2g和复合改性剂3g。
其中，抗紫外线剂由30wt％氯乙烯-醋酸乙烯酯共聚乳液、20wt％2,4-二氯苯甲酸、20wt％微孔木质素、20％纳米二氧化钛组成。
复合改性剂采用蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土，其质量比为1:1:0.5。
具体制备方法如下：
(1)首先将纳米氧化锌、乙醇、碳酸氢钠放入搅拌罐中进行加热分散，分散温度为46℃，搅拌速率为650转/分，时间为13min，得到纳米氧化锌分散液；
(2)在分散液中加入壳聚糖、纳米晶纤维素，充分混合后加入水浴锅中水浴加热，水浴加热温度为62℃，时间为12min，得到混合液A；
(3)在混合液A中加入复合改性剂，混合后将混合液加入超声波发生器进行超声处理，超声频率为65KHz，超声时间25min，得到混合液B；
(4)在混合液B中加入抗紫外线剂，在常温下充分混合后，得到改性纳米氧化锌液；
(5)最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，得到粒径为20-30nm的改性纳米氧化锌。
实施例4
本实施例提供一种改性纳米氧化锌，其原料包括纳米氧化锌35g、乙醇8g、碳酸氢钠8g、壳聚糖5g、纳米晶纤维素7g、抗紫外线剂2g和复合改性剂5g。
其中，抗紫外线剂由30wt％氯乙烯-醋酸乙烯酯共聚乳液、20wt％2,4-二氯苯甲酸、20wt％微孔木质素、20％纳米二氧化钛组成。
复合改性剂采用蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土，其质量比为1:1:0.5。
具体制备方法如下：
(1)首先将纳米氧化锌、乙醇、碳酸氢钠放入搅拌罐中进行加热分散，分散温度为52℃，搅拌速率为750转/分，时间为20min，得到纳米氧化锌分散液；
(2)在分散液中加入壳聚糖、纳米晶纤维素，充分混合后加入水浴锅中水浴加热，水浴加热温度为68℃，时间为16min，得到混合液A；
(3)在混合液A中加入复合改性剂，混合后将混合液加入超声波发生器进行超声处理，超声频率为75KHz，超声时间35min，得到混合液B；
(4)在混合液B中加入抗紫外线剂，在常温下充分混合后，得到改性纳米氧化锌液；
(5)最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，得到粒径为20-30nm的改性纳米氧化锌。
实施例5
本实施例提供一种改性纳米氧化锌，其原料包括纳米氧化锌30g、乙醇7g、碳酸氢钠6g、壳聚糖4g、纳米晶纤维素6g、抗紫外线剂2g和复合改性剂4g。
其中，抗紫外线剂由30wt％氯乙烯-醋酸乙烯酯共聚乳液、20wt％2,4-二氯苯甲酸、20wt％微孔木质素、20％纳米二氧化钛组成。
复合改性剂采用蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土，其质量比为1:1:0.5。
具体制备方法如下：
(1)首先将纳米氧化锌、乙醇、碳酸氢钠放入搅拌罐中进行加热分散，分散温度为50℃，搅拌速率为700转/分，时间为17min，得到纳米氧化锌分散液；
(2)在分散液中加入壳聚糖、纳米晶纤维素，充分混合后加入水浴锅中水浴加热，水浴加热温度为65℃，时间为14min，得到混合液A；
(3)在混合液A中加入复合改性剂，混合后将混合液加入超声波发生器进行超声处理，超声频率为70KHz，超声时间30min，得到混合液B；
(4)在混合液B中加入抗紫外线剂，在常温下充分混合后，得到改性纳米氧化锌液；
(5)最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，得到粒径为20-30nm的改性纳米氧化锌。
对比例1
本对比例和实施例1的区别在于，不对纳米氧化锌进行改性。
对比例2
本对比例和实施例1的区别在于，不添加抗紫外线剂。
试验例
对本发明各实施例和对比例进行性能测试，将得到的纳米氧化锌制成含量为5wt％的分散液用作织物整理剂原料，所述织物整理剂含有2.5wt％的纳米氧化锌分散液和50wt％的PVA。使用织物整理剂对织物进行喷涂，采用两步喷涂法，喷涂2层，成膜厚度为0.05mm，洗涤12次做性能测试，其性能测试结果如表1所示，其中断裂强力测定按：GB/T3923.1-2013《纺织品织物拉伸性能第1部分：断裂强力和断裂伸长率的测定(条样法)》；耐磨性能测定按：GB/T 21196.2-2007《纺织品马丁代尔法织物耐磨性的测定第2部分：试样破损的测定》；抗菌面料抗菌性的性能测定参照：AATCC 100－2012《抗菌纺织品的评价方法》；防紫外线性能测定按：GB/T 18830-2009《纺织品防紫外线性能的评定》；
表1各实施例和对比例进行织物整理的性能效果
Figure BDA0003227474600000111
从上表可以看出，本申请优选特定比例的实施例2中，其各方面性能最好，在没有对纳米氧化锌进行改性的对比例1中，和实施例1相比，其各方面性能均有大幅下降；而对比例2中，没有添加本申请限定的抗紫外线剂，和实施例1相比，除了紫外线遮挡率不佳外，其断裂伸长率、抑菌率、断裂强力和出现破损时摩擦次数均有不同程度的下降，这是由于在未添加抗紫外线剂后，整体织物的韧性未有增强，由于缺少韧性的原因，便会造成摩擦时，织物与外界的直接冲撞力增大，故而造成织物破损的提早出现，造成抗摩擦性能降低；同时纳米二氧化钛有辅助抗菌作用并可以强韧度，在未添加抗紫外线剂后，整体织物的抗菌性和强韧度未有增强，会直接造成强力的降低、断裂伸长率的降低及抑菌率的降低；同时由于少喷涂抗紫外线剂层，也造成了强力的下降、抗摩擦性的降低、断裂伸长率的降低。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (9)

1.一种改性纳米氧化锌，其特征在于，包括如下重量份数的原料：
Figure FDA0003227474590000011
2.根据权利要求1所述的改性纳米氧化锌，其特征在于，由如下重量份数的原料组成：
纳米氧化锌40份；
溶剂10份；
碳酸氢钠9份；
抗菌剂6份；
纳米晶纤维素8份；
抗紫外线剂3份；
复合改性剂6份。
3.根据权利要求1或2所述的改性纳米氧化锌，其特征在于，所述溶剂为乙醇；
所述抗菌剂为壳聚糖；
所述抗紫外线剂由氯乙烯-醋酸乙烯酯共聚乳液、2,4-二氯苯甲酸、微孔木质素和纳米二氧化钛组成；
所述所述复合改性剂由蓖麻油酸酯硫酸钠、十二水硫酸铝钠、氧化石墨烯-凹凸棒土组成。
4.根据权利要求3所述的改性纳米氧化锌，其特征在于，
所述抗紫外线剂中氯乙烯-醋酸乙烯酯共聚乳液、2,4-二氯苯甲酸、微孔木质素和纳米二氧化钛的质量比为3:2:2:3；
所述复合改性剂中蓖麻油酸酯硫酸钠、十二水硫酸铝钠和氧化石墨烯-凹凸棒土的质量比为0.5-1.5:0.5-1.5:0.25-0.75。
5.权利要求1-4任一项所述的改性纳米氧化锌的制备方法，其特征在于，包括如下步骤：
S1：将纳米氧化锌、溶剂、碳酸氢钠混合，得到纳米氧化锌分散液；
S2：在分散液中加入抗菌剂、纳米晶纤维素，充分混合后水浴加热，得到第一混合液；
S3：在第一混合液中加入复合改性剂，然后进行超声处理，得到第二混合液；
S4：在第二混合液中加入抗紫外线剂混合，得到改性纳米氧化锌液；
S5：最后将改性纳米氧化锌液经过滤，干燥，粉碎，过筛，即得到所述改性纳米氧化锌。
6.根据权利要求5所述的制备方法，其特征在于，步骤S1中所述混合是在搅拌罐中进行加热分散，分散温度为45-55℃，搅拌速率为600-800转/分，时间为12min-22min。
7.根据权利要求5或6所述的制备方法，其特征在于，步骤S2中所述水浴温度为60-70℃，时间为10min-18min；
步骤S3中超声处理时，频率为60-80KHz，时间20-40min；
步骤S4中所述混合的温度为常温。
8.根据权利要求5-7任一项所述的制备方法,其特征在于，步骤S5中得到的所述改性纳米氧化锌粒径为20-30nm。
9.权利要求1-4任一项所述改性纳米氧化锌的应用，其特征在于，应用于配置成织物整理剂整理织物。
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Application publication date: 20211119