CN106996036B - 一种耐水洗型天然抗菌除臭剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种耐水洗型天然抗菌除臭剂及其制备方法，该抗菌除臭剂包括以下成分：黄柏提取物，溪黄草提取物，牛至提取物，羧甲基壳聚糖，ZnO‑SiO2复合纳米颗粒，海藻胶，十八烷基二甲基甜菜碱，水性聚硅氧烷以及增稠剂。该抗菌除臭剂、对多种细菌有抑制作用，具有较强的抗菌除臭功能。该处理剂可以与纤维有较强的连接力，经过多次水洗以及长时间穿着摩擦后仍能保持良好的抗菌性能。
Description
技术领域
本发明涉及纺织助剂领域，特别是涉及一种耐水洗型天然抗菌除臭剂及其制备方法。
背景技术
多孔性纺织品容易吸收人体分泌的汗水、皮质、新陈代谢产物等，从而可以为微生物提供营养，有助于微生物的滋生和繁殖。尤其在潮湿、营养以及合适的温度条件下，微生物繁殖迅速，并会在织物中生成菌斑使得织物发生霉变、脆化，从在穿着或应用中对人体带来不良影响。此外，细菌还会通过分解人体分泌物产生臭味，并导致皮肤疾病的传染。通过对织物进行抗菌除臭整理赋予织物良好的抗菌功能，抑制有害微生物的传播生长，纺织细菌在织物上不断繁殖产生的臭气，可以有效的提高纺织品的综合品质。
纺织品中抗菌除臭剂有多种分类方法，根据杀菌或抑菌作用的不同，可以分为杀菌剂和抑菌剂两种。根据溶出性不同，可以分为溶出性抗菌剂和非溶出性抗菌剂。按照抗菌除臭剂与纤维的结合方式的不同，抗菌除臭剂还可以分为直接吸附型抗菌剂、交联结合型抗菌剂以及反应结合型抗菌剂。按照结构的不同，抗菌剂又可以分为有机类、无机类和天然生物抗菌剂。天然抗菌剂为来自动植物以及微生物等所含的有抗菌性能的成分，取材天然，刺激性小。
中国专利CN201510480817.8公开了一种新型天然抗菌整理剂及其制备方法，所述的天然抗菌整理剂包括壳聚糖3-6份、桧柏油4-9份、甘草水提物3-7份、木通水提物2-5份、榆白皮乙醇提取物3-5份、桂丁乙醇提取物3-6份、月桂酰二乙醇胺2-4份、二癸基二甲基氯化铵3-7份、甘油5-10份、水200-300份。该抗菌整理剂的制备方法包括热浸提、过滤、真空薄膜干燥、混合，制备的天然抗菌整理剂对大肠杆菌和金黄色葡萄球菌具有良好的抑制作用。
发明内容
本发明的目的是提供一种耐水洗型天然抗菌除臭剂，该抗菌除臭剂、对多种细菌有抑制作用，具有较强的抗菌除臭功能。该处理剂可以与纤维有较强的连接力，经过多次水洗以及长时间穿着摩擦后仍能保持良好的抗菌性能。
本发明的另一目的是提供该耐水洗型天然抗菌除臭剂的制备方法。
为实现上述目的，本发明采用以下技术方案：
一种耐水洗型天然抗菌除臭剂的制备方法，包括以下步骤：
1、将黄柏提取物，溪黄草提取物，牛至提取物加入水中混合均匀后，加入羧甲基壳聚糖，搅拌混合，之后将ZnO-SiO2复合纳米颗粒浸渍与其中，浸渍24-36h后，60-70℃烘干，之后在100-120℃条件下烘焙1-2h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒加入海藻胶溶液中，使用高剪切搅拌器，以10000-15000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱，使用超声波仪进行分散处理，制得纳米浆液；
3、将纳米浆液，水性聚硅氧烷，增稠剂混合，制得所述耐水洗型天然抗菌除臭剂。
优选的，所述黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物。
优选的，所述黄柏提取物，每1L至少由8Kg黄柏制备而成；所述溪黄草提取物，每1L至少由15Kg溪黄草制备而成；所述牛至提取物，每1L至少由10Kg牛至制备而成。
优选的，所述ZnO-SiO2复合纳米颗粒的制备方法为：将醋酸锌溶解于水中，加入纳米SiO2粉末，加热至60-80℃，剧烈搅拌条件下滴加无水乙醇，滴加完成后，加入柠檬酸三铵，搅拌均匀后，静置24-48h，制备成凝胶，将凝胶干燥后，研磨，在480℃条件下焙烧4h，制得ZnO-SiO2复合纳米颗粒。
优选的，所述ZnO-SiO2复合纳米颗粒中ZnO和SiO2的摩尔比为3：2。
优选的，所述步骤(1)中各原料的使用量为，以重量份数计：黄柏提取物15-20份，溪黄草提取物18-25份，牛至提取物30-50份，羧甲基壳聚糖20-30份，ZnO-SiO2复合纳米颗粒100份。
优选的，所述步骤(2)中各原料的使用量为，以重量份数计：负载纳米颗粒100份，海藻胶20-40份，十八烷基二甲基甜菜碱10-17份。
优选的，所述步骤(2)中制备的纳米浆液固含量为60-70％。
优选的，所述步骤(3)中各原料的使用量为，以重量份数计：
纳米浆液100份，水性聚硅氧烷60-70份，增稠剂5-9份。
优选的，所述增稠剂为甲基羟乙基纤维素，乙基羟乙基纤维素或羟乙基纤维素中的一种或多种混合物。
一种耐水洗型天然抗菌除臭剂，由以上方法制备而成。
本发明具有以下有益效果，
纳米ZnO具有良好的杀菌效果，对皮肤无刺激，热稳定性好。纳米SiO2为多孔结构，具有较强的吸附，负载能力。通过制备ZnO-SiO2复合纳米颗粒，将纳米ZnO与纳米SiO2结合在一起，并将天然抗菌成分负载与复合纳米颗粒中，有助于ZnO与天然抗菌成分相互接触，在抗菌过程中可以相互配合，从而达到更优良的抗菌效果。
通过将天然抗菌成分负载与复合纳米颗粒中，再在其表面包裹海藻胶，减缓了天然抗菌成分的流失速度，延长了织物的抗菌效果。利用十八烷基二甲基甜菜碱对复合纳米颗粒表面进行改性，有助于提高复合纳米颗粒的分散稳定性，同时十八烷基二甲基甜菜碱本身即具有一定的抗菌效果，有助于提高该抗菌除臭剂的抗菌性能。
具体实施方式
为了更好的理解本发明，下面通过实施例对本发明进一步说明，实施例只用于解释本发明，不会对本发明构成任何的限定。
实施例1
将醋酸锌溶解于水中，加入纳米SiO2粉末，加热至75℃，剧烈搅拌条件下滴加无水乙醇，滴加完成后，加入柠檬酸三铵，搅拌均匀后，静置48h，制备成凝胶，将凝胶干燥后，研磨，在480℃条件下焙烧4h，制得ZnO-SiO2复合纳米颗粒。
制备的ZnO-SiO2复合纳米颗粒中ZnO和SiO2的摩尔比为3：2。
实施例2
一种耐水洗型天然抗菌除臭剂的制备方法，包括以下步骤：
1、将黄柏提取物15份，溪黄草提取物18份，牛至提取物30份加入水中混合均匀后，加入羧甲基壳聚糖20份，搅拌混合，之后将实施例1制备的ZnO-SiO2复合纳米颗粒100份浸渍与其中，浸渍24h后，60℃烘干，之后在100℃条件下烘焙1h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒100份加入溶解有20份海藻胶的溶液中，使用高剪切搅拌器，以10000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱10份，使用超声波仪进行分散处理，制得纳米浆液，纳米浆液固含量为60％；
3、将纳米浆液100份，水性聚硅氧烷60份，甲基羟乙基纤维素5份混合，制得所述耐水洗型天然抗菌除臭剂。
其中黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，每1L由10Kg黄柏制备而成；溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，每1L由20Kg溪黄草制备而成；牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物，每1L由14Kg牛至制备而成。
织物经制备的耐水洗型天然抗菌除臭剂整理后，具有良好的抗菌除臭性能，并经过多次水洗后仍能保持较高的抗菌除臭性能。
实施例3
一种耐水洗型天然抗菌除臭剂的制备方法，包括以下步骤：
1、将黄柏提取物20份，溪黄草提取物25份，牛至提取物50份加入水中混合均匀后，加入羧甲基壳聚糖30份，搅拌混合，之后将实施例1制备的ZnO-SiO2复合纳米颗粒100份浸渍与其中，浸渍36h后，70℃烘干，之后在120℃条件下烘焙2h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒100份加入溶解有40份海藻胶的溶液中，使用高剪切搅拌器，以15000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱17份，使用超声波仪进行分散处理，制得纳米浆液，纳米浆液固含量为70％；
3、将纳米浆液100份，水性聚硅氧烷70份，羟乙基纤维素9份混合，制得所述耐水洗型天然抗菌除臭剂。
其中黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，每1L由10Kg黄柏制备而成；溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，每1L由20Kg溪黄草制备而成；牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物，每1L由14Kg牛至制备而成。
织物经制备的耐水洗型天然抗菌除臭剂整理后，具有良好的抗菌除臭性能，并经过多次水洗后仍能保持较高的抗菌除臭性能。
实施例4
一种耐水洗型天然抗菌除臭剂的制备方法，包括以下步骤：
1、将黄柏提取物15份，溪黄草提取物25份，牛至提取物30份加入水中混合均匀后，加入羧甲基壳聚糖30份，搅拌混合，之后将实施例1制备的ZnO-SiO2复合纳米颗粒100份浸渍与其中，浸渍24h后，70℃烘干，之后在100℃条件下烘焙2h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒100份加入溶解有20份海藻胶的溶液中，使用高剪切搅拌器，以15000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱10份，使用超声波仪进行分散处理，制得纳米浆液，纳米浆液固含量为70％；
3、将纳米浆液100份，水性聚硅氧烷60份，甲基羟乙基纤维素，乙基羟乙基纤维素或羟乙基纤维素9份混合，制得所述耐水洗型天然抗菌除臭剂。
其中黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，每1L由10Kg黄柏制备而成；溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，每1L由20Kg溪黄草制备而成；牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物，每1L由14Kg牛至制备而成。
织物经制备的耐水洗型天然抗菌除臭剂整理后，具有良好的抗菌除臭性能，并经过多次水洗后仍能保持较高的抗菌除臭性能。
实施例5
一种耐水洗型天然抗菌除臭剂的制备方法，包括以下步骤：
1、将黄柏提取物20份，溪黄草提取物18份，牛至提取物50份加入水中混合均匀后，加入羧甲基壳聚糖20份，搅拌混合，之后将实施例1制备的ZnO-SiO2复合纳米颗粒100份浸渍与其中，浸渍36h后，60℃烘干，之后在120℃条件下烘焙1h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒100份加入溶解有40份海藻胶的溶液中，使用高剪切搅拌器，以10000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱17份，使用超声波仪进行分散处理，制得纳米浆液，纳米浆液固含量为60％；
3、将纳米浆液100份，水性聚硅氧烷70份，乙基羟乙基纤维素5份混合，制得所述耐水洗型天然抗菌除臭剂。
其中黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，每1L由10Kg黄柏制备而成；溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，每1L由20Kg溪黄草制备而成；牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物，每1L由14Kg牛至制备而成。
织物经制备的耐水洗型天然抗菌除臭剂整理后，具有良好的抗菌除臭性能，并经过多次水洗后仍能保持较高的抗菌除臭性能。
实施例6
一种耐水洗型天然抗菌除臭剂的制备方法，包括以下步骤：
1、将黄柏提取物17份，溪黄草提取物20份，牛至提取物38份加入水中混合均匀后，加入羧甲基壳聚糖24份，搅拌混合，之后将实施例1制备的ZnO-SiO2复合纳米颗粒100份浸渍与其中，浸渍36h后，65℃烘干，之后在110℃条件下烘焙2h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒100份加入溶解有30份海藻胶的溶液中，使用高剪切搅拌器，以15000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱15份，使用超声波仪进行分散处理，制得纳米浆液，纳米浆液固含量为60％；
3、将纳米浆液100份，水性聚硅氧烷65份，乙基羟乙基纤维素和羟乙基纤维素的混合物7份混合，制得所述耐水洗型天然抗菌除臭剂。
其中黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，每1L由10Kg黄柏制备而成；溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，每1L由20Kg溪黄草制备而成；牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物，每1L由14Kg牛至制备而成。
织物经制备的耐水洗型天然抗菌除臭剂整理后，具有良好的抗菌除臭性能，并经过多次水洗后仍能保持较高的抗菌除臭性能。
Claims (10)
1.一种耐水洗型天然抗菌除臭剂的制备方法，其特征在于：包括以下步骤：
1、将黄柏提取物，溪黄草提取物，牛至提取物加入水中混合均匀后，加入羧甲基壳聚糖，搅拌混合，之后将ZnO-SiO2复合纳米颗粒浸渍与其中，浸渍24-36h后，60-70℃烘干，之后在100-120℃条件下烘焙1-2h，制得负载纳米颗粒；
2、将上一步骤制备的负载纳米颗粒加入海藻胶溶液中，使用高剪切搅拌器，以10000-15000rpm的速度搅拌分散，之后向其中加入十八烷基二甲基甜菜碱，使用超声波仪进行分散处理，制得纳米浆液；
3、将纳米浆液，水性聚硅氧烷，增稠剂混合，制得所述耐水洗型天然抗菌除臭剂。
2.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述黄柏提取物为黄柏在水中通过浸泡加热回流制备的提取物，每1L至少由8Kg黄柏制备而成；溪黄草提取物为溪黄草在乙醇中通过浸泡加热回流制备的提取物，每1L至少由15Kg溪黄草制备而成；牛至提取物为牛至在乙醇中通过浸泡加热回流制备的提取物，每1L至少由10Kg牛至制备而成。
3.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述ZnO-SiO2复合纳米颗粒的制备方法为：将醋酸锌溶解于水中，加入纳米SiO2粉末，加热至60-80℃，剧烈搅拌条件下滴加无水乙醇，滴加完成后，加入柠檬酸三铵，搅拌均匀后，静置24-48h，制备成凝胶，将凝胶干燥后，研磨，在480℃条件下焙烧4h，制得ZnO-SiO2复合纳米颗粒。
4.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述ZnO-SiO2复合纳米颗粒中ZnO和SiO2的摩尔比为3：2。
5.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述步骤(1)中各原料的使用量为，以重量份数计：黄柏提取物15-20份，溪黄草提取物18-25份，牛至提取物30-50份，羧甲基壳聚糖20-30份，ZnO-SiO2复合纳米颗粒100份。
6.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述步骤(2)中各原料的使用量为，以重量份数计：负载纳米颗粒100份，海藻胶20-40份，十八烷基二甲基甜菜碱10-17份。
7.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述步骤(2)中制备的纳米浆液固含量为60-70％。
8.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述步骤(3)中各原料的使用量为，以重量份数计：
纳米浆液100份，水性聚硅氧烷60-70份，增稠剂5-9份。
9.根据权利要求1所述的耐水洗型天然抗菌除臭剂的制备方法，其特征在于：所述增稠剂为甲基羟乙基纤维素，乙基羟乙基纤维素或羟乙基纤维素中的一种或多种混合物。
10.一种耐水洗型天然抗菌除臭剂，其特征在于：由权利要求1-9任一项所述的方法制备而成。
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