CN113749982A - 一种抗菌洗手液的制备方法 - Google Patents
一种抗菌洗手液的制备方法 Download PDFInfo
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- CN113749982A CN113749982A CN202111035208.3A CN202111035208A CN113749982A CN 113749982 A CN113749982 A CN 113749982A CN 202111035208 A CN202111035208 A CN 202111035208A CN 113749982 A CN113749982 A CN 113749982A
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- Prior art keywords
- hand sanitizer
- sodium
- acid
- deionized water
- tio2
- Prior art date
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Abstract
本发明提供了一种抗菌洗手液的制备方法,所述洗手液通过阴离子表面活性、两性表面活性剂、非离子表面活性剂复配为表面活性剂获得高效的发泡、去污性能,并以次氯酸为杀菌原料,杀菌去污能力强对于大肠杆菌、金黄色葡萄球菌2分钟内的杀菌对数值为4.48左右,洗手液整体具有护肤润肤、抗菌抑菌,抗敏舒缓、杀菌去污能力强的性能。
Description
技术领域
本发明属于洗涤剂领域,具体涉及一种抗菌洗手液的制备方法。
背景技术
洗手液作为一种新型手部清洁产品,在宾馆、餐饮部门、机场等公共场所,已经取代了以往普遍使用的肥皂。相比肥皂,洗手液具有独特的优点,洗手液能避免与手部接触,防止使用后或在环境中沾染污垢、细菌、病毒等成为二次污染源,易于保存,自然消耗比较少。肥皂在涂抹和使用过程中对机械揉搓依赖性强,在公共场所使用时长期处于湿润状态,有利于细菌病毒滋生。
洗手液配方灵活多变,可塑性强,易于改进,性能温和、不刺激皮肤、抗硬水、泡沫丰富、成分多元化、易于加工的特点,市场上的洗手液产品种类繁多,按照不同的用途大致可分为:(1)普通洗手液:未添加特殊成分,一般只有去除手部污垢油脂的作用;(2)护肤型洗手液:在洗手液中添加纯甘油、芦荟等护肤成分,在清洁手部的同时,起到滋润皮肤的功能;(3)重油污型洗手液:主要适用于从事机修、炼油、汽车修理等行业工作人员,这些工作人员手部经常沾有重油污,普通的肥皂和洗手液很难洗净;(4)消毒杀菌型洗手液:应对现在的很多公共卫生问题,将有效杀菌成分加入洗手液中,可以阻断疾病传播;(5)免水型
洗手液:一般以酒精为主要成分,不需要用水冲洗,使用简便,一般用于缺水条件下的手部清洁和消毒;(6)其他功能型洗手液:针对不同的消费人群开发出的特殊功能洗手液,如除铅洗手液、复合功能洗手液等。洗手液的种类功能如此丰富,也再次证明洗手液易于加工,产品可塑性强,有广宽的市场前景,可以在预防疾病中起到更加重要的作用。
次氯酸是含氯稀溶液中最有效的消毒剂,通常通过电化学方法制备,为酸性电解水,是一种PH为5.0~6.5、有效氯浓度为10-30mg/L的水,这种次氯酸水具有较强的氧化能力和快速杀灭微生物的作用,因此广泛的用于洗手液中。
如山东舒达生物科技有限公司CN111481452 A公开了种安全防护洗手液及其制备方法,由以下成分组成:弱酸性次氯酸钠溶液、0-苯基苯酚、盐酸聚六亚甲基胍、氯代二甲苯酚、季铵盐、醋酸氯已定、甘油和表面活性剂,所述弱酸性次氯酸钠溶液中含有效氯50~100mg/L,PH值范围为5~7。。其制备包括以下具体步骤:步骤一:用水分别稀释盐酸和次氯酸钠溶液,并充分混合;步骤二:将步骤一溶液在反应器中充分反应;步骤三:向步骤二中制备好的弱酸性次氯酸钠溶液中加入剩余成分并通过搅拌装置搅拌混合均匀后装瓶封装即可。本发明与现有技术相比的优点在于:不含有酒精成分,无色无味,使用较为安全方便,同时杀菌后没有次生物污染生成,杀菌抑菌效果较好。
此外,如与本发明类似的CN201110066196A公开了一种不需防腐剂的天然消毒洗涤组合物,该组合物同时具有消毒和洗涤功能,所述组合物含有电解氯氧化剂、APG,用于洗涤餐具、炊具、蔬菜、瓜果、织物、或汗脚、汗袜的异味,电解氯氧化剂含有次氯酸根离子和次氯酸,通过无隔膜电解槽中电解氯化钠的稀溶液获得。
发明内容
基于上述内容,本发明提供了一种抗菌洗手液的制备方法,所述洗手液中以次氯酸为杀菌物质,对大肠杆菌、金黄色葡萄球菌、白色念珠菌显示出极强的杀菌效果,且所述洗手液清洁环保、安全、去污功效良好,是安全有效的生活日用品。
本发明还采用特殊阳极电解氯化钠制备高效次氯酸溶液,所述阳极通过设计微弧氧化中间层显著提高基材与活性层的结合力,金属氧化物强化电解寿命长,通过制备(Ir-Nb-Rh)Ox活性层实现Ti-W- Ir-Nb-Rh复配,获得高催化活性、高耐腐蚀性,高导电性电极,并降低析氧、析氯电位,提高电化学转换效率,阳极电流效率85.3-94.2%。
一种抗菌洗手液的制备方法, 所述洗手液通过如下方法制备:
(1)将α-烯烃基磺酸钠AOS阴离子表面活性剂、椰油酰胺丙级甜菜碱CAB-35两性表面活性剂、椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂溶于去离子水中,混合搅拌均匀,搅拌速度400-500r/min;
(2)将步骤(1)所得混合物加热至50-70℃,加入甘油保湿剂、聚丙烯酸PPA增稠剂使其溶解,并混合均匀,然后,冷却至室温;
(3)继续加入氯化钠无机盐、乙二胺四乙酸二钠EDTA-2Na、云母粉珠光添加剂、柠檬香精,并混合搅拌均匀;
(4)采用次氯酸去离子水溶液将步骤(3)所得混合液的pH值调至5.75-6.75,获得洗手液。
进一步的,α-烯烃基磺酸钠AOS阴离子表面活性剂:7-9wt.%;椰油酰胺丙级甜菜碱CAB-35两性表面活性剂:6-7 wt.%;椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂:5-6wt.%。
进一步的,甘油保湿剂:1-3 wt.%;氯化钠无机盐:0.01-0.12 wt.%;聚丙烯酸PPA增稠剂:1-4 wt.%。
进一步的,乙二胺四乙酸二钠EDTA-2Na络合剂:0.05-0.12 wt.%;云母粉珠光添加剂0.5-1wt;柠檬香精:0.1-1.0%;有效氯成分50-70ppm的次氯酸去离子水溶液:余量。
进一步的,所述次氯酸钠水溶液通过如下方法制备:
(1)设置反应槽:所述反应槽中至少包括一个Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极,一个钛合金或不锈钢为阴极:
(2)电解氯化钠:向反应槽底部通入饱和食盐水和盐酸混合液;
(3)稀释收集次氯酸消毒液:由电解槽顶部收集流出液,然后使用并使用去离子水稀释,获得次氯酸消毒水。
进一步的,所述Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极的制备方法如下:
(a)预处理钛板或钛网基材;
(b)于基材表面制备TiO2-WO3复合中间层:将经过预处理的基材作为阳极,置于电解液中进行微弧氧化处理,所述电解液中由三水钨酸钠、氢氧化钠、氟化钠、六偏磷酸钠和去离子水组成;
电解参数:双向脉冲电压,正压350-400V,负压30-50V,占空比30-40%,频率700-800Hz,正负向脉冲比为1:1,时间4-8min,中间层的厚度为5-10μm;
(c)制备(Ir-Nb-Rh)Ox活性层:将一定量的NbCl4溶解于异丙醇中、将一定量的氯铑酸铵、氯铱酸溶解于1:1的异丙醇和盐酸的混合液中,将氯铱酸、氯铑酸铵、四氯化铌按(10~25)∶(15~20)∶(5~10)的摩尔比例混合获得前驱液,将所述前驱液刷涂覆于TiO2-WO3复合中间层表面,于60-70℃下干燥3-5min后,转化马弗炉,马弗炉的程序升温为5℃/min升至450-500℃,保持20-30min,自然冷却,重复刷涂过程直至于所需负载量,然后450-500℃退火1-1.5h,获得Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极。
进一步的,所述预处理包括有除油、喷砂和冲洗,所述除油:将所述基材放置于3-5wt.%Na2CO3溶液,保持5-10min,然后60-80oC超声1-3min;喷砂粗化:0.1-0.5mm石英砂,硬度≈400HV,空气压力0.1-0.15MPa;所述冲洗为去离子水冲洗。
进一步的,三水钨酸钠为13-17g/L,氢氧化钠为1.5-2.5g/L,氟化钠为2-3g/L,六偏磷酸钠为4-5g/L,去离子水为余量。
进一步的,所述TiO2-WO3复合中间层的厚度为5-10μm,(Ir-Nb-Rh)Ox活性层的厚度为12-15μm。
进一步的,所述步骤(c)中负载量为2.2-2.5mg/cm2。
进一步的,所述次氯酸钠水溶液通过如下方法制备:
(1)设置反应槽:所述反应槽中至少包括一个Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极,一个钛合金或不锈钢为阴极:
(2)电解氯化钠:向反应槽底部通入饱和食盐水和盐酸混合液;
(3)稀释收集次氯酸消毒液:由电解槽顶部收集流出液,然后使用并使用去离子水稀释,获得次氯酸消毒水。
所述Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极的制备方法如下:
(a)预处理钛板或钛网基材;
(b)于基材表面制备TiO2-WO3复合中间层:将经过预处理的基材作为阳极,置于电解液中进行微弧氧化处理,所述电解液中由三水钨酸钠、氢氧化钠、氟化钠、六偏磷酸钠和去离子水组成;
电解参数:双向脉冲电压,正压350-400V,负压30-50V,占空比30-40%,频率700-800Hz,正负向脉冲比为1:1,时间4-8min,中间层的厚度为5-10μm;
(c)制备(Ir-Nb-Rh)Ox活性层:将一定量的NbCl4溶解于异丙醇中、将一定量的氯铑酸铵、氯铱酸溶解于1:1的异丙醇和盐酸的混合液中,将氯铱酸、氯铑酸铵、四氯化铌按(10~25)∶(15~20)∶(5~10)的摩尔比例混合获得前驱液,将所述前驱液刷涂覆于TiO2-WO3复合中间层表面,于60-70℃下干燥3-5min后,转化马弗炉,马弗炉的程序升温为5℃/min升至450-500℃,保持20-30min,自然冷却,重复刷涂过程直至于所需负载量,然后450-500℃退火1-1.5h,获得Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极。
进一步的,所述预处理包括有除油、喷砂和冲洗,所述除油:将所述基材放置于3-5wt.%Na2CO3溶液,保持5-10min,然后60-80oC超声1-3min;喷砂粗化:0.1-0.5mm石英砂,硬度≈400HV,空气压力0.1-0.15MPa;所述冲洗为去离子水冲洗。
进一步的,所述三水钨酸钠为13-17g/L,氢氧化钠为1.5-2.5g/L,氟化钠为2-3g/L,六偏磷酸钠为4-5g/L,去离子水为余量。
进一步的,所述TiO2-WO3复合中间层的厚度为5-10μm,(Ir-Nb-Rh)Ox活性层的厚度为12-15μm。
进一步的,所述步骤(c)中负载量为2.2-2.5mg/cm2。
洗手液是指以去除手上污渍、细菌为目的而设计的清洁产品,由必需的活性成分、杀菌成分、辅助成分构成,本发明作为活性成分的是表面活性剂,所述杀菌成分为次氯酸、辅助成分为保湿剂、无机盐、增稠剂、络合剂珠光剂和香精,用于满足消费者关于洗手液的各种效能需求。
表面活性剂:基本功能是清洁功能,在洗手液中主要是清洁手上的油污,表面活性剂可以产生丰富的泡沫,表面活性剂在较低浓度下 溶于水不仅可以大幅度的降低溶液体系的表面张力,随着表面活性剂达到临界胶束浓度,溶液中能形成大量的胶束,这些胶束可以起到润湿、增溶、乳化、分散的作用,将油污清洗干净,本发明以阴离子表面活性、两性表面活性剂、非离子表面活性剂复配为表面活性剂改善洗手液的发泡性能和润湿性能。
保湿剂:对于市场需求而言,不仅仅是简单的清洗去污,清洗后的人体感觉同样非常重要,避免出现手部的干燥和粗糙,因此需要保湿剂改善身体感觉,保湿剂的定义为能够保持皮肤角质层中的水分或是能够延缓和阻止角质层中的水分挥发,尤其在低湿度下更能显现这种特性的一类物质,本发明采用低挥发性、高沸点且具有强吸湿性甘油作为保湿剂。
增稠剂:在使用洗手液时,如果黏度太小,洗手液非常容易从手中溜走,造成浪费,去污能力也会受到影响,黏度调节得过大,则不易挤压和冲洗。洗手液具有适宜的粘度既能增强消费者的感官效果,本发明采用氯化钠和聚丙烯酸PPA作为增稠剂。
络合剂:平常的水质中含有Ca2+、Mg2+等硬金属离子,有些表面活性剂耐硬水性比较差,会和这些水中的金属离子形成沉淀影响洗涤剂的性能。络合剂加入到洗涤剂中,可以和这些金属离子络合以溶解络合物的形式被消除,从而使硬水软化,本发明采用EDTA-2Na作为络合剂,所述络合剂在水中可以形成一个可溶性的环状结构,将金属离子束缚在环儿里面,从而防止金属离子形成沉淀,使溶液具有一个良好的外观。
香精和珠光粉,用于改善洗手液的感触效果,可依需选用客户所需味道和外观。
杀菌剂:由于次氯酸不带电荷且分子量相对较低,因此它比其他基于杀菌剂或抑菌剂更能穿透细胞壁,它与有机物(即微生物细胞的关键成分)发生氧化反应的速度也更快,因此,消毒作用更加高效,仅在低浓度条件下,可通过攻击生理学相关分子(氨类、硫醚、硫醇、核苷酸等)的方式,穿透细胞膜,使蛋白氧化,达到杀灭细菌繁殖体、病毒、真菌、结核杆菌和细菌芽孢的目的。
关于本发明的电解过程和使用的阳极:
首先:对钛基材进行表面预处理,表面处理包括有除油和喷砂,其中除油步骤为非必要处理过程,主要是由于后续会进行微弧氧化,微弧氧化过程电压较大,会发生明显的阳极电化学脱脂过程,因此脱脂为非必选,但脱脂一定程度上会影响微弧氧化层与基材的结合力,因此本发明预先对基材进行脱脂处理,脱脂后对基材进行喷砂处理,喷砂的主要目的并非在于除去氧化,主要的目的在于提高基材的表面粗糙度,顺便除去表面的杂质,喷砂能够显著的提高基材与微弧氧化中间层的结合面积,进而提高基材与活性层的结合力。
其次,关于中间层,中间层的作用是增加钛基体和活性涂层之间的结合力,可以耐气体冲刷,防止涂层过早剥落,同时中间层的存在又阻挡了氧气向基体的扩散和渗透,减慢了基体与活性层之间不导电的氧化钛膜形成的速度,延缓了基体的钝化失活,提高氧化物阳极的使用寿
命。现有技术中的中间层主要是 SnO2、Sn-Sb 氧化物、Ir-Co 氧化物、Sn-Sb-Mn氧化物、Sn-Ru-Mn 氧化物、Ru-Sn-Sb 氧化物、Ru-Sb-Mn 氧化物、Nb-Sn 氧化物等中间层,当然也有部分的以钛基阳极氧化膜为中间层,鲜有以钛基微弧氧化膜为中间层,以阳极氧化或者微弧氧化膜为中间层可以有效的提高基材与中间层层的结合力,主要是由于氧化膜是原位产生,不存在明显的界面,钛基材表面的中间层与基材之间没有明显的界面,过渡良好,而涂覆、电镀或者其他沉积方法存在明显的界面,所述界面在后续的热处理活性层时,必然会发生一定程度热剥离或者蓄积热应力,此外相比于阳极氧化膜,微弧氧化膜在耐腐蚀性(耐盐雾性)、硬度、寿命方面远远高于微弧氧化膜,但微弧氧化膜的形貌中的孔隙率较低,导致活性涂层与基材的结合力下降,单纯的氧化钛微弧氧化膜表面粗糙,存在有大小不一的放电残留孔洞,孔洞的范围变化较大,孔隙率范围大约2-8wt.%,其中孔隙率的主要贡献在于表面多孔层,物化贡献主要在于过渡层,结合力贡献主要在于底部的致密层,致密层的孔吸率低于1%,所述微弧氧化滑膜的比表面积为10.32m2/g。相比而言,在微弧氧化膜的中增加W元素,显示出更高的孔隙率,比表面积提升至13.9 m2/g,孔隙率和表面积的提升显著的提高了中间层与活性层的接触面积,提高了两者的结合力,在复合协同活化过程中也提供了更多的活性位点,获得的中间层中TiO2的质量分数大约50-55wt.%,W的质量分数大约25-30wt.%,Ti的成分较多是由于Ti4+参与至少两个主反应,而W参与至少一个主反应,反应式如下:
Ti4++2OH-+2H2O→TiO2+2H2O+
Ti4++2WO4 2-+TiO2+2WO3。
即本发明的TiO2-WO3具有耐蚀性、良好的导电性、与钛基体结合紧密的有益效果。
活性层:将电极中混合的两种或多种成分寻求一种协同效应,使组元间达成紧密的电子联系
来改善电极活性,是活性层研究的主要目的,本发明采用的主要活性元素为Ir、Nb、Rh,即涂层的主体为Ir、Nb和Rh元素,其中Ir和Rh为主要氧化物,提供高的催化活性和耐蚀性,Nb用于改善涂层表面氧化物颗粒形态,细化涂层晶粒,增加电极微观面积,粗糙度更大,表面活性比表面积提高,进而改善涂层的催化活性。
本发明的(Ir-Nb-Rh)Ox固溶体不能完全固溶,部分会以IrOX 和RuO2析出,因此会增加阳极的微观比表面积和活性位点,提高析氯效率,电极表面有大量的微孔与缝隙,且缝隙出析出明显的晶簇,增加微观比表面积,电流密度小,有利于延长电极的使用寿命,整体而言,涂层表面平整、结晶较为致密,裂缝深度浅、宽度窄,裂缝细。
关于电解次氯酸的过程,本发明采用无隔膜的电解槽,反应槽中至少包括一个Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极,一个钛合金或不锈钢为阴极,阳极为析氯反应,即氯离子失去电子后形成氯气分子,同时,氯气与水反应后生成次氯酸和氯离子,以及少部分的氯酸根离子。同时,阳极的水分子电解后会析出氧气,析氧反应为副反应,应尽量避免析氧反应的发生,在析氯反应和析氧反应的竞争中,以析氯反应占优势,但是氯化钠电解液浓度过低时,电离的氯离子不能满足电解槽的电解速度,从而开始电解水,析出氧气,氧气的析出会明显降低阳极活性氧化物的氧缺陷,导致催化层失活,关于电流密度:本发明的电流密度为100-150 mA/cm2,有效氯会随着电流密度的增加而增加,pH值缓慢向中性偏移,析氯电位为会明显下降,如实施例3中提高电流密度后,析氯电位为0.98V,低于实施例2的析氯电位,此外,随着电流密度的增加,电流效率会降低,主要是由于析氧竞争反应会导致电流效率降低。
本发明流出液的pH为2.5-4,在该该范围内,所述次氯酸几乎无法保存,大概在20-30天内,获得的流出液的有效氯几乎为零,因此必须对新获得的流出液进行稀释,将pH稀释为6.5-7,如实施例2中获得的流出液使用去离子水稀释至pH=6.75,在避光,密封条件下测试不同时间有效氯的含量,初始有效氯含量为62mg/L,在第120天后,有效氯的保存率为97%,保存效果极好,对密封避光保存的有效氯测试其对大肠杆菌和金黄色葡萄球菌的杀菌效果,其ORP值为1040mV,有效氯为60 mg/L左右,3min内,几乎100%的消杀效果。
有益技术效果:
(1)通过阴离子表面活性、两性表面活性剂、非离子表面活性剂复配为表面活性剂获得高效的发泡、去污性能。
(2)所述洗手液具有护肤润肤、抗菌抑菌,抗敏舒缓、杀菌去污能力强,对于大肠杆菌、金黄色葡萄球菌在1min内的杀菌效率为99.99%,2分钟内的杀菌对数值为4.48(99.99668%)。
(3)通过在钛基材表面原位氧化制备TiO2-WO3中间层,有效的提高了基材钛与活性层的结合力,所述中间层的比表面积较高,为活性层的涂覆提供了微观接触比表面积,进而提高中间层与活性层之间的稳定。
(4)通过在中间层表面涂覆Ir、Nb和Rh元素为主的固溶体活性组分,显著提高了电解的催化活性,细化涂层晶粒,获得的涂层表面平整、结晶较为致密,裂缝深度浅、宽度窄,裂缝细,提高涂层的催化活性、稳定性和使用寿命。
(5)电解氯化钠制备次氯酸的析氯电位低、电流效率高,有效氯浓度高,杀菌效果优秀。
具体实施方式:
本发明所有的洗手液制备过程如下:
(1)将α-烯烃基磺酸钠AOS阴离子表面活性剂、椰油酰胺丙级甜菜碱CAB-35两性表面活性剂、椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂溶于去离子水中,混合搅拌均匀,搅拌速度400-500r/min;
(2)将步骤(1)所得混合物加热至50-70℃,加入甘油保湿剂、聚丙烯酸PPA增稠剂使其溶解,并混合均匀,然后,冷却至室温;
(3)继续加入氯化钠无机盐、乙二胺四乙酸二钠EDTA-2Na、云母粉珠光添加剂、柠檬香精,并混合搅拌均匀;
(4)采用次氯酸去离子水溶液将步骤(3)所得混合液的pH值调至5.75-6.75,获得洗手液。
本发明实施例1-3所有的次氯酸制备过程如下:
一种消毒液的制备方法,所述消毒液为次氯酸,所述制备方法包括如下步骤:
(1)设置反应槽:所述反应槽中至少包括一个Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极,一个钛合金或不锈钢为阴极, 阴极和阳极的极距为3.5mm。
(2)电解氯化钠:向反应槽底部通入饱和食盐水和盐酸混合液,混合液的pH值为0.9,混合进液速度为1.5L/h,电流密度125mA/cm2。
(3)稀释收集次氯酸消毒液:由电解槽顶部收集流出液,然后使用并使用去离子水稀释。
所述Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极的制备方法如下。
(a)预处理钛板或钛网基材:预处理包括有除油、喷砂和冲洗,所述除油:将所述基材放置于4wt.%Na2CO3溶液,保持7.5min,然后70oC超声2min;喷砂粗化:0.1-0.5mm石英砂,硬度≈400HV,空气压力0.125MPa;所述冲洗为去离子水冲洗。
(b)于基材表面制备TiO2-WO3复合中间层:将经过预处理的基材作为阳极,置于电解液中进行微弧氧化处理,所述电解液中由三水钨酸钠、氢氧化钠、氟化钠、六偏磷酸钠和去离子水组成, 所述三水钨酸钠为15g/L,氢氧化钠为2g/L,氟化钠为2.5g/L,六偏磷酸钠为4.5g/L,去离子水为余量。
电解参数:双向脉冲电压,正压375V,负压40V,占空比35%,频率750Hz,正负向脉冲比为1:1,时间6min。
(c)制备(Ir-Nb-Rh)Ox活性层:将一定量的NbCl4溶解于异丙醇中、将一定量的氯铑酸铵、氯铱酸溶解于1:1的异丙醇和盐酸的混合液中,将氯铱酸、氯铑酸铵、四氯化铌按(17.5)∶(17.5)∶(7.5)的摩尔比例混合获得前驱液,将所述前驱液刷涂覆于TiO2-WO3复合中间层表面,于70℃下干燥5min后,转化马弗炉,马弗炉的程序升温为5℃/min升至475℃,保持25min,自然冷却,重复刷涂过程直至于所需2.35mg/cm2负载量,然后475℃退火1.25h,获得Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极。
实施例1
α-烯烃基磺酸钠AOS阴离子表面活性剂:7wt.%;
椰油酰胺丙级甜菜碱CAB-35两性表面活性剂: 6 wt.%;
椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂:5 wt.%;
甘油保湿剂:1wt.%;
氯化钠无机盐:0.01-0.12 wt.%;
聚丙烯酸PPA增稠剂:1-4 wt.%;
乙二胺四乙酸二钠EDTA-2Na络合剂:0.05-0.12 wt.%;
云母粉珠光添加剂0.5-1wt;
柠檬香精:0.1-1.0%;
有效氯为60ppm的次氯酸去离子水溶液:余量。
pH为5.75。
实施例2
α-烯烃基磺酸钠AOS阴离子表面活性剂:7-9wt.%;
椰油酰胺丙级甜菜碱CAB-35两性表面活性剂: 6-7 wt.%;
椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂:5-6 wt.%;
甘油保湿剂:1-3 wt.%;
氯化钠无机盐:0.01-0.12 wt.%;
聚丙烯酸PPA增稠剂:1-4 wt.%;
乙二胺四乙酸二钠EDTA-2Na络合剂:0.05-0.12 wt.%;
云母粉珠光添加剂0.5-1wt;
柠檬香精:0.1-1.0%;
有效氯为60ppm的次氯酸去离子水溶液:余量。
pH为6.2。
实施例3
α-烯烃基磺酸钠AOS阴离子表面活性剂:7-9wt.%;
椰油酰胺丙级甜菜碱CAB-35两性表面活性剂: 6-7 wt.%;
椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂:5-6 wt.%;
甘油保湿剂:1-3 wt.%;
氯化钠无机盐:0.01-0.12 wt.%;
聚丙烯酸PPA增稠剂:1-4 wt.%;
乙二胺四乙酸二钠EDTA-2Na络合剂:0.05-0.12 wt.%;
云母粉珠光添加剂0.5-1wt;
柠檬香精:0.1-1.0%;
有效氯为60ppm的次氯酸去离子水溶液:余量。
pH为6.75。
对实施例2获得的洗手液进行起泡性测试,按 GB/T 13173.6 《洗涤剂发泡力的测定》,气泡率为372%,稳定性为0-3min 时泡沫减少了 5-7%后,之后维持稳定,1小时后,泡沫稳定性减少43%,对其粘度进行测试为3752 mPa·S。对于大肠杆菌、金黄色葡萄球菌在1min内的杀菌效率为99.8%,5分钟内的杀菌对数值为4.48(99.99668%)。
虽然结合特定的实施例对本发明进行了说明,但本领域的技术人员可以 理解,对本发明可以作出许多修改和变型。因此,要认识到,权利要求书的 意图在于覆盖在本发明真正构思和范围内的所有这些修改和变型。
Claims (10)
1.一种抗菌洗手液的制备方法,其特征在于所述洗手液通过如下方法制备:
(1)将α-烯烃基磺酸钠AOS阴离子表面活性剂、椰油酰胺丙级甜菜碱CAB-35两性表面活性剂、椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂溶于去离子水中,混合搅拌均匀,搅拌速度400-500r/min;
(2)将步骤(1)所得混合物加热至50-70℃,加入甘油保湿剂、聚丙烯酸PPA增稠剂使其溶解,并混合均匀,然后,冷却至室温;
(3)继续加入氯化钠无机盐、乙二胺四乙酸二钠EDTA-2Na、云母粉珠光添加剂、柠檬香精,并混合搅拌均匀;
(4)采用次氯酸去离子水溶液将步骤(3)所得混合液的pH值调至5.75-6.75,获得洗手液。
2.如权利要求1所述的一种抗菌洗手液的制备方法,其特征在于α-烯烃基磺酸钠AOS阴离子表面活性剂:7-9wt.%;椰油酰胺丙级甜菜碱CAB-35两性表面活性剂:6-7 wt.%;椰子油脂酸单乙醇酰胺CMEA非离子表面活性剂:5-6 wt.%。
3.如权利要求1所述的一种抗菌洗手液的制备方法,其特征在于甘油保湿剂:1-3wt.%;氯化钠无机盐:0.01-0.12 wt.%;聚丙烯酸PPA增稠剂:1-4 wt.%。
4.如权利要求1所述的一种抗菌洗手液的制备方法,其特征在于乙二胺四乙酸二钠EDTA-2Na络合剂:0.05-0.12 wt.%;云母粉珠光添加剂0.5-1wt;柠檬香精:0.1-1.0%;有效氯成分50-70ppm的次氯酸去离子水溶液:余量。
5.如权利要求1所述的一种抗菌洗手液的制备方法,其特征在于所述次氯酸水溶液通过如下方法制备:
(1)设置反应槽:所述反应槽中至少包括一个Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极,一个钛合金或不锈钢为阴极:
(2)电解氯化钠:向反应槽底部通入饱和食盐水和盐酸混合液;
(3)稀释收集次氯酸:由电解槽顶部收集流出液,然后使用并使用去离子水稀释,获得次氯酸。
6.如权利要求5所述的一种抗菌洗手液的制备方法,其特征在于所述Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极的制备方法如下:
(a)预处理钛板或钛网基材;
(b)于基材表面制备TiO2-WO3复合中间层:将经过预处理的基材作为阳极,置于电解液中进行微弧氧化处理,所述电解液中由三水钨酸钠、氢氧化钠、氟化钠、六偏磷酸钠和去离子水组成;
电解参数:双向脉冲电压,正压350-400V,负压30-50V,占空比30-40%,频率700-800Hz,正负向脉冲比为1:1,时间4-8min,中间层的厚度为5-10μm;
(c)制备(Ir-Nb-Rh)Ox活性层:将一定量的NbCl4溶解于异丙醇中、将一定量的氯铑酸铵、氯铱酸溶解于1:1的异丙醇和盐酸的混合液中,将氯铱酸、氯铑酸铵、四氯化铌按 (10~25)∶(15~20)∶(5~10)的摩尔比例混合获得前驱液,将所述前驱液刷涂覆于TiO2-WO3复合中间层表面,于60-70℃下干燥3-5min后,转化马弗炉,马弗炉的程序升温为5℃/min升至450-500℃,保持20-30min,自然冷却,重复刷涂过程直至于所需负载量,然后450-500℃退火1-1.5h,获得Ti/TiO2-WO3/(Ir-Nb-Rh)Ox阳极。
7.如权利要求5所述的一种抗菌洗手液的制备方法,其特征在于所述预处理包括有除油、喷砂和冲洗,所述除油:将所述基材放置于3-5wt.%Na2CO3溶液,保持5-10min,然后60-80oC超声1-3min;喷砂粗化:0.1-0.5mm石英砂,硬度≈400HV,空气压力0.1-0.15MPa;所述冲洗为去离子水冲洗。
8.如权利要求5所述的一种抗菌洗手液,所述三水钨酸钠为13-17g/L,氢氧化钠为1.5-2.5g/L,氟化钠为2-3g/L,六偏磷酸钠为4-5g/L,去离子水为余量。
9.如权利要求5所述的一种抗菌洗手液的制备方法,其特征在于所述TiO2-WO3复合中间层的厚度为5-10μm,(Ir-Nb-Rh)Ox活性层的厚度为12-15μm。
10.如权利要求5所述的一种抗菌洗手液的制备方法,其特征在于所述步骤(c)中负载量为2.2-2.5mg/cm2。
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