CN113439767B - 一种除菌除螨剂、其制备方法及浓缩洗衣液 - Google Patents

一种除菌除螨剂、其制备方法及浓缩洗衣液 Download PDF

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CN113439767B
CN113439767B CN202110702018.6A CN202110702018A CN113439767B CN 113439767 B CN113439767 B CN 113439767B CN 202110702018 A CN202110702018 A CN 202110702018A CN 113439767 B CN113439767 B CN 113439767B
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mite
degerming
laundry detergent
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removing agent
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CN113439767A (zh
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牟维林
孙本平
唐文金
赵乐荣
于建伟
毕利顺
杜可欣
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Yantai New Era Health Industry Daily Chemical Co ltd
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Abstract

本发明公开了一种除菌除螨剂，其包括植物复配提取物以及醋酸钙；所述的植物复配提取物为柚皮、淡竹叶和柿叶的提取物。制备植物复配提取物的原料中，柚皮、淡竹叶、柿叶的质量比为(0.5‑3)：(2‑3)：1。本发明还公开了上述除菌除螨剂的制备方法，并公开了配方中包含上述除菌除螨剂的超浓缩洗衣液。本发明通过醇提水沉法，获得柚皮、淡竹叶和柿叶的提取物，各提取物与醋酸钙组成除菌除螨剂，产生协同效应，获得了显著的抑菌和除螨效果。通过筛选多款表活搭配，克服了表活浓度过高形成立方相液晶的问题，可获得活性物含量超过50％的超浓缩洗衣液。本发明超浓缩洗衣液兼顾了抑菌除螨效果与安全性，去污力强劲。

Description

一种除菌除螨剂、其制备方法及浓缩洗衣液
技术领域
本发明属于日化领域，具体涉及一种除菌除螨剂、其制备方法及浓缩洗衣液。
背景技术
各种物品表面、体表皮肤以及与外界相通的腔道中都存在有大量微生物，对人类致病比较重要的常见代表性细菌主要为金黄色葡萄球菌、大肠杆菌、沙门氏菌以及自色念珠菌等。螨虫在一般家庭中大量存在，大多寄生于床垫被褥、衣物等。螨虫对人的危害主要是引起过敏症和皮脂炎，还会增加哮喘等过敏性疾患的发生率。
除菌除螨洗衣液属于近年来热点，受到越来越多消费者的关注，各大知名品牌也相继推出了相关产品。越来越多的研究加上商家的引导，使消费者认识到，衣物、床品等纺织品，其携带的细菌螨虫与鼻炎、呼吸道感染、皮肤过敏瘙痒、粉刺痤疮等问题都有关联。尤其是近些年的疫情影响，消费者对于除菌除螨产品有较大需求。然而，现有日化用品中的灭菌、除螨成分存在刺激性强、有安全风险、灭菌除螨效果不显著等缺陷。调研市场上目前的除菌除螨洗衣液产品，常用的除菌除螨剂为对氯间二甲苯酚，对氯间二甲基苯酚一般具有中等到低毒性，会引起严重的眼部刺激，通过呼吸渠道摄入具有低毒，此外还会引起轻微的皮肤刺激。对氯间二甲苯酚的副作用也非常大，一旦进入人体之后，可以导致食管和肠胃的黏膜细胞坏死，这就会使患者出现食道灼伤，并且还会使患者出现中毒性肠炎。除此之外，这种药物还会导致身体的肠均衡失调，这就会对消化***造成非常严重的影响。并且这种药物还有可能造成患者出现急性呼吸衰竭，急性肾功能衰竭等疾病，会严重的危害生命安全。因此，亟需一种安全性高、抑菌除螨效果好的日化用品专用抑菌除螨剂。
浓缩型洗衣液是目前洗衣液的主流趋势，既响应了国家节能减排的号召，也容易漂洗，省水省力。但受技术限制，表活浓度过高会导致形成立方相液晶或层状液晶，导致析出或结块，目前多数浓缩洗衣液活性物含量基本在25-32％之间，研发高浓度洗衣液是无数日化工作者的奋斗目标。
发明内容
本发明针对上述现有技术存在的不足，提供一种除菌除螨剂、其制备方法及浓缩洗衣液制备方法，抑菌除螨效果好，安全性高，活性物含量可达50％以上。
具体技术方案如下：
本发明的目的之一是提供一种除菌除螨剂，其包括植物复配提取物以及醋酸钙；经过几十种植物提取物的抑菌性能筛选，最终选定的植物复配提取物为柚皮、淡竹叶和柿叶的提取物。
其中，柚皮提取物含有丰富的柚皮苷，除菌效果显著，而且可耐碱性环境，有较强的抗氧化性，对大肠杆菌、金黄色葡萄球菌、沙门氏菌均有抑制活性。价格低廉、易得。
其中，淡竹叶提取物有良好的抗菌性，对金黄葡萄球菌、溶血性链球菌、绿脓杆菌和大肠杆菌均有一定的抑制作用。淡竹叶提取物的动物实验表明，它具有抑制过敏和搔痒的功能。
其中，柿叶提取物除菌效果明显，对大肠杆菌、金黄色葡萄球菌、荧光假单胞菌、伤寒沙门氏菌、枯草芽孢杆菌、蜡样芽孢杆菌、变形杆菌等多种细菌均有不同程度的抑制效果。价格低廉、易得。
在本发明中，柚皮提取物、淡竹叶提取物、柿叶提取物、醋酸钙产生了显著的协同效应，抑菌、除螨效果好，安全性高。
进一步，制备植物复配提取物的原料中，柚皮、淡竹叶、柿叶的质量比为(0.5-3)：(2-3)：1。
上述配比中，柚皮、淡竹叶、柿叶的质量均为以干制后的质量计。
再进一步，植物复配提取物与醋酸钙的质量比为10：(1-2)。
进一步，所述的植物复配提取物为柚皮、淡竹叶和柿叶的醇提水沉提取物。
本发明的目的之二是提供一种上述除菌除螨剂的制备方法，其中，所述的植物复配提取物为通过醇提水沉工艺获得。
进一步，所述的植物复配提取物的制备方法包括如下步骤：将柚皮、淡竹叶、柿叶原料粉碎，置于75-95％的乙醇溶液中70-80℃回流提取1.5-3h，慢速定性滤纸过滤，敞口浓缩至浸膏状态，加入浸膏质量4-6倍的去离子水，8-12h后再次过滤，滤液干燥后，得植物复配提取物。
其中，柚皮、淡竹叶、柿叶原料与75-95％的乙醇溶液的质量比为1：(20-40)。乙醇的浓度为体积分数。
其中，所述的干燥优选为冷冻干燥。
进一步，将制备获得的植物复配提取物与醋酸钙按比例混合，获得除菌除螨剂。
本发明的目的之三是提供一种超浓缩洗衣液，其配方包括上述除菌除螨剂。
进一步，所述的超浓缩洗衣液以重量份数计包括除菌除螨剂0.5wt％-5wt％。
再进一步，所述的超浓缩洗衣液以重量份数计，其配方以质量百分数计包括：除菌除螨剂0.5wt％-5wt％，Lutensol XL70 30wt％-50wt％，α-烯基磺酸钠2wt％-10wt％、辛基磺酸钠2wt％-10wt％，皂粒1wt％-3wt％，脂肪醇聚氧乙烯醚(AEO-9)4wt％-10wt％，柠檬酸钠1wt％-4wt％，无水氯化钙0.01wt％-0.1wt％，甘油2wt％-5wt％，丙二醇2wt％-5wt％，乙醇0.5wt％-1wt％，蛋白酶0.1wt％-0.5wt％，以及脂肪酶0.1wt％-0.5wt％。其中，上述配方中还可包括防腐剂0.1wt％-1wt％，香精0.1wt％-1wt％。上述配方的余量为水。
其中，Lutensol XL70，其分子式为RO-(C2H4O)nH，R为C10，属于脂肪醇聚氧乙烯醚中的一类，相对于AEO-9的C12-18而言，碳链缩短，溶解度增大，其原料本身状态就是液态，在水溶液中也是粘度较低的液态，可配置浓度为0-60的洗衣液产品，非常适合制作超浓缩洗衣液，可比普通浓缩洗衣液浓度高一倍以上。通过α-烯基磺酸钠、辛基磺酸钠两款阴离子表面活性剂与Lutensol XL70、AEO-9两款非离子表面活性剂搭配，利用非离子表面活性剂来降低胶束电荷密度，且非离子表面活性剂庞大的极性头可有效增加空间位阻，阻碍立方相液晶的形成。并通过添加甘油、丙二醇、乙醇，可有效降低体系粘度，且避免低温析出。得到稳定的超浓缩洗衣液。
进一步，所述的超浓缩洗衣液的制备方法包括如下步骤：其制备方法包括如下步骤：水中添加皂粒，升温至80-90℃，加入Lutensol XL70、α-烯基磺酸钠、辛基磺酸钠、脂肪醇聚氧乙烯醚、柠檬酸钠、无水氯化钙、甘油、丙二醇、乙醇，溶解均匀后开始降温，降为至38℃后加入除菌除螨剂、蛋白酶、脂肪酶、防腐剂、香精，补水至100wt％即得。
本发明的有益效果如下：
本发明通过醇提水沉法，获得柚皮、淡竹叶和柿叶的提取物，各提取物与醋酸钙组成除菌除螨剂，产生协同效应，获得了显著的抑菌和除螨效果。比常用的对氯间二甲苯酚、三氯生等常用除菌除螨剂安全、绿色。通过筛选多款表活搭配，克服了表活浓度过高形成立方相液晶的问题，通过α-烯基磺酸钠、辛基磺酸钠两款阴离子表面活性剂与LutensolXL70、AEO-9两款非离子表面活性剂搭配，辅以甘油、丙二醇、乙醇，可获得活性物含量超过50％的超浓缩洗衣液。将本发明的除菌除螨剂应用于超浓缩洗衣液中，兼顾了抑菌除螨效果与安全性，去污力强劲，5mL即可满足8kg洗衣机的满负荷清洗要求。
具体实施方式
以下结合实例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1
1、制备除菌除螨剂：所述的除菌除螨剂由质量比为10：1的植物复配提取物和醋酸钙组成；
其制备方法如下：
(1)制备植物复配提取物：作为原料的柚皮、淡竹叶、柿叶的质量比为2：2：1；将上述原料粉碎，置于85％的乙醇溶液中，原料与乙醇溶液的质量比为1:25；75℃回流提取2h，慢速定性滤纸过滤，敞口浓缩至浸膏状态，加入浸膏质量5倍的去离子水，10h后再次过滤，滤液冷冻干燥后，得植物复配提取物。
(2)将步骤(1)获得的植物复配提取物与醋酸钙按质量比10：1混合，得除菌除螨剂。
2.使用步骤1获得的除菌除螨剂，制备超浓缩洗衣液：按照重量份数计，所述的超浓缩洗衣液的配方如下：除菌除螨剂2wt％，Lutensol XL70(巴斯夫)30wt％，α-烯基磺酸钠10wt％、辛基磺酸钠10wt％，皂粒1wt％，脂肪醇聚氧乙烯醚(AEO-9)4wt％，柠檬酸钠2wt％，无水氯化钙0.05wt％，甘油3wt％，丙二醇3wt％，乙醇0.5wt％，蛋白酶0.3wt％，以及脂肪酶0.3wt％，防腐剂0.05wt％，以及香精0.5wt％，加水补至100wt％。
其制备方法如下：
水中加皂粒，升温至85℃，加入Lutensol XL70、α-烯基磺酸钠、辛基磺酸钠、脂肪醇聚氧乙烯醚、柠檬酸钠、无水氯化钙、甘油、丙二醇、乙醇，溶解均匀后开始降温，降为至38℃后加入除菌除螨剂、蛋白酶、脂肪酶、防腐剂、香精，补水至100wt％即得。
对比例1
与实施例1的区别在于，所述的除螨除菌剂仅包括植物复配提取物，不包括醋酸钙；
其余技术特征与实施例1相同。
对比例2
与实施例1的区别在于，所述的植物复配提取物的原料为质量比为1：1的柚皮和淡竹叶，不包括柿叶；
其余技术特征与实施例1相同。
对比例3
与实施例1的区别在于，所述的植物复配提取物的原料为质量比为2：1的柚皮和柿叶，不包括淡竹叶；
其余技术特征与实施例1相同。
对比例4
与实施例1的区别在于，所述的植物复配提取物的原料为质量比为2：1的淡竹叶和柿叶，不包括柚皮；
其余技术特征与实施例1相同。
实施例2
1、制备除菌除螨剂：所述的除菌除螨剂由质量比为10：2的植物复配提取物和醋酸钙组成；
其制备方法如下：
(1)制备植物复配提取物：与实施例1的区别在于，柚皮、淡竹叶与柿叶的质量比为1：2：1，制备方法同实施例1；
(2)将步骤(1)获得的植物复配提取物与醋酸钙混合。
2.使用步骤1获得的除菌除螨剂，制备超浓缩洗衣液：按照重量份数计，所述的超浓缩洗衣液的配方如下：除菌除螨剂4wt％，Lutensol XL70(巴斯夫)45wt％，α-烯基磺酸钠4wt％、辛基磺酸钠4wt％，皂粒1wt％，脂肪醇聚氧乙烯醚(AEO-9)5wt％，柠檬酸钠2wt％，无水氯化钙0.05wt％，甘油3wt％，丙二醇3wt％，乙醇0.5wt％，蛋白酶0.3wt％，以及脂肪酶0.3wt％，防腐剂0.05wt％，以及香精0.5wt％，加水补至100wt％；
超浓缩洗衣液的制备方法同实施例1。
实验1除菌实验
试验菌株：大肠杆菌8099、金黄色葡萄球菌ATCC6538由中国工业微生物菌种保藏管理中心提供，第4-8代新鲜斜面培养物。
试验样品：实施例1与对比例1-4获得的洗衣液。
检测方法：按照《一次性使用卫生用品卫生标准GB 15979 2002》附录C进行检测，试验温度19-21℃，试验重复3次。结果见表1。
表1实施例1与对比例1-4的抑菌效果对比
Figure BDA0003130455170000071
根据以上数据可知，实施例1对大肠杆菌、金黄色葡萄球菌具有较强的抑菌作用，而其他对比例的抑菌作用则显著弱于实施例1。
实验2除螨实验
螨虫种类：本实验采用粉尘螨雌雄成螨。
试验样品：实施例1与对比例1-4获得的洗衣液。
试验方法：剪取18块圆形50mm直径的100％纯棉制品，经高温蒸煮后晾干待用，将18块纯棉制品至于培养皿中，标记1-18号，分别均匀撒上0.05g螨虫饲料，并投放150只存活螨虫。
将培养皿放入恒温恒湿箱中，温度为25±2℃，相对湿度为75±5％，培养7天，然后取实施例1获得的洗衣液15g，将1-3号纯棉制品用常规滚筒洗衣机进行标准洗衣操作，洗后取出，自然风干，计数螨虫数量。
同理，对对比例1-4获得的洗衣液按照上述方法进行操作，对比例1清洗4-6号，对比例2清洗7-9号，对比例3清洗10-12号，对比例4清洗13-15号，16-18号作为对照组，直接用清水冲洗。
设三块试验组存活螨虫数的平均值为T，三块对照组存活螨虫数的平均值为B，螨虫抑制率为(B-T)/B*100％。结果见表2。
表2实施例1与对比例1-4除螨效果对比
Figure BDA0003130455170000081
根据以上结果可知，实施例1对螨虫具有较强的抑制作用，而其他对比例的抑制作用则弱于实施例1。
实验3多次完整皮肤刺激实验
实验动物的情况见表3。
表3实验3中实验动物情况
Figure BDA0003130455170000091
试验前将动物背部脊柱两侧被毛剪掉，去毛范围各3cm*3cm，涂覆面积为2.5cm*2.5cm。
取0.5mL实施例1样品涂覆在一侧皮肤上，另一侧作为对照，涂覆4h后用水冲洗，除去残留物。每天涂一次，连续涂14天，在每次涂覆后24h观察现象。按规范要求进行评分分级。结果见表4。
表4多次完整皮肤刺激实验
Figure BDA0003130455170000092
Figure BDA0003130455170000101
通过表4可知，实施例1对家兔多次完整皮肤刺激性检测结果为轻刺激性，未见其他毒性。
实验4产品去污力测试
选取市场销量较好的6款浓缩型洗衣液产品，作为对照样1-6，与实施例1进行去污力对比。
测试方法：依据GB/T 13174-2003《衣料用洗涤剂去污力及抗污渍再沉积能力的测定》进行去污力检测。
评价标准：QB/T 1224-2007，去污力A级规定为三种污布的去污力≥标准粉去污力，去污力B级规定为二种污布的去污力≥标准粉去污力，去污力C级规定为一种污布的去污力≥标准粉去污力。且每一级都通过碳黑污布。
测试仪器：WSD-Ⅲ白度仪，RHLQ立式去污机。结果见表5。
表5实施例1与其他浓缩型洗衣液的去污力对比
Figure BDA0003130455170000102
Figure BDA0003130455170000111
通过表5可见，实施例1具有良好的去污力。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (3)

1.一种超浓缩洗衣液，其特征在于，按照重量份数计，包括除菌除螨剂2wt％，LutensolXL70(巴斯夫)30wt％，α-烯基磺酸钠10wt％、辛基磺酸钠10wt％，皂粒1wt％，脂肪醇聚氧乙烯醚(AEO-9)4wt％，柠檬酸钠2wt％，无水氯化钙0.05wt％，甘油3wt％，丙二醇3wt％，乙醇0.5wt％，蛋白酶0.3wt％，以及脂肪酶0.3wt％，加水补至100wt％；
所述除菌除螨剂由植物复配提取物和醋酸钙组成，其制备方法如下：
(1)制备植物复配提取物：作为原料的柚皮、淡竹叶、柿叶的质量比为2：2：1；将上述原料粉碎，置于85％的乙醇溶液中，原料与乙醇溶液的质量比为1：25；75℃回流提取2h，慢速定性滤纸过滤，敞口浓缩至浸膏状态，加入浸膏质量5倍的去离子水，10h后再次过滤，滤液冷冻干燥后，得植物复配提取物；
(2)将步骤(1)获得的植物复配提取物与醋酸钙按质量比10：1混合，得除菌除螨剂。
2.根据权利要求1所述的超浓缩洗衣液，其特征在于，还包括防腐剂0.1wt％-1wt％，香精0.1wt％-1wt％。
3.根据权利要求1所述的超浓缩洗衣液，其特征在于，其制备方法包括如下步骤：水中添加皂粒，升温至85℃，加入LutensolXL70、α-烯基磺酸钠、辛基磺酸钠、脂肪醇聚氧乙烯醚、柠檬酸钠、无水氯化钙、甘油、丙二醇、乙醇，溶解均匀后开始降温，降至38℃后加入除菌除螨剂、蛋白酶、脂肪酶、防腐剂、香精，补水至100wt％即得。
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