CN117089413A - 一种抗菌洗衣凝珠及其制备方法 - Google Patents
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Abstract
本发明公开了一种抗菌洗衣凝珠及其制备方法,制备方法包括如下步骤:40~60℃下将抗菌剂、脂肪醇聚氧乙烯醚、羟乙磺酸酯钠、椰子油脂肪酸二乙醇酰胺加入到去离子水中搅拌均匀,冷却至室温,加入玫瑰精油、茶树油、棕榈油、丙二醇、山梨醇、甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠;制备得到的洗衣凝珠温和无刺激,具有优异的去污能力和芬芳衣物的能力,还能提供持久、稳定、高效的杀菌效果,且对人体安全无害。
Description
技术领域
本发明涉及日化洗涤剂领域,具体涉及一种抗菌洗衣凝珠及其制备方法。
背景技术
洗衣凝珠是一类近几年来兴起的机洗专用型织物清洁产品,因其具有超高浓缩的绿色配方技术、精准便捷的使用方式、时尚炫彩的包装外形等优势,现今已经受到了越来越多消费者的认可和青睐。自2014年宝洁公司于国内首推碧浪洗衣凝珠上市以来,国内几大洗涤剂生产商如纳爱斯、浪奇、立白、威莱等也纷纷紧随其后推出了旗下品牌的相应系列凝珠产品。近几年的市场运营数据表明,国内洗衣凝珠品类的销售总额逐年提高,保持了积极良好的市场增长态势。在历经几年的发展之后,洗衣凝珠现今已成为我国洗涤市场中继洗衣皂、洗衣粉、洗衣液之后的全新一代织物清洁产品,它的进一步推广和使用不仅对推动我国洗涤剂产业的浓缩化进程具有重要意义,而且也代表了如今我国洗用品行业向着“低碳节能”和“绿色环保”的发展方向前进。
现在市场上凝珠的主要形式包括单腔和多腔(一般2~3腔),多腔各个独立的部分通过水溶性膜隔开,根据配方需要,膜腔内可分别放洗衣液、柔顺剂、漂白剂、酶、除菌剂、固色剂及香精等。
洗衣凝珠的基础配方一般主要由溶剂、少量的水、表面活性剂、助剂、酶制剂等组成。凝珠中表面活性剂一般为阴离子表面活性剂和非离子表面活性剂的复配物,选择表面活性剂时除了考虑去污性还应注意溶解性、凝胶化、泡沫等问题以及与膜的兼容性;洗涤剂中使用的助剂主要是软水剂和抗再沉积剂,这些助剂可分散污渍,防止清洗下来的污渍再沉积到清洗表面;洗涤剂配方要兼顾产品稳定性和洗涤效果,还要使用更多的催化洗涤技术,例如酶;洗衣凝珠是低水、超浓缩配方,以防表面活性剂析出,最有效的方法是加入大量溶剂,常用的有乙醇、乙二醇、丙二醇、甘油等。
随着国内市场消费的升级,高性能、高质量的洗衣类产品的市场需求也越来越大,跟普通洗衣粉和洗衣液相比,洗衣凝珠产品具有以下优势:(1)具有良好的清洁去污能力,表面活性剂的含量是普通洗衣液的3~5倍,洗衣凝珠含有多种表面活性剂和生物酶,它可以轻松去除多种顽固污渍,如汗渍、油渍、血渍、奶渍、尿渍等;(2)使用方便,不需要消费者量取,一次一粒,不脏手,轻松方便,省时省心;(3)易溶于水,大多数洗衣凝珠外膜一般1min即可溶破,释放出多倍浓缩洗衣液,5min左右外膜可完全溶解于水中,随漂洗用水排出,不会残留在织物上;(4)低泡,因为洗衣凝珠较高的表面活性剂含量,多数厂家都会使用低泡配方,以免泡沫过多溢出洗衣机,低泡配方更易于漂洗,省水省时。
中国专利文献CN202010023740.2公开了一种含醇醚溶剂的洗衣凝珠及其制备方法,洗衣凝珠包括内容物和水溶膜,所述内容物包覆在水溶膜内,所述内容物包括溶剂3~80%,表面活性剂3~90%;所述溶剂中包含醇醚类溶剂,所述醇醚溶剂:其他溶剂=1:0~15;所述水溶膜的材质为聚乙烯醇PVA、改性聚乙烯醇或改性淀粉。所述配方组分按一定工艺混配好后包膜,即得含醇醚溶剂得洗衣凝珠。含醇醚溶剂得洗衣凝珠可以显著地提高洗衣凝珠的去污能力。
但是现有的洗衣凝珠具备的单纯的低泡和高去污能力的优势已经不能满足大众的需求,亟需开发一种高效、广谱、稳定性好的抗菌洗衣凝珠。
发明内容
为了解决现有技术存在的不足,本发明的目的在于提供一种抗菌洗衣凝珠及其制备方法,制备得到的洗衣凝珠温和无刺激,具有优异的去污能力和芬芳衣物的能力,还能提供持久、稳定、高效的杀菌效果,且对人体安全无害。
为了实现上述目的,本发明采用如下技术方案:
一种抗菌洗衣凝珠,由以下组分制成:抗菌剂4~8份、脂肪醇聚氧乙烯醚25~35份、羟乙磺酸酯钠15~20份、椰子油脂肪酸二乙醇酰胺10~18份、去离子水8~14份、玫瑰精油1~3份、茶树油1~3份、棕榈油1~3份,丙二醇5~12份、山梨醇8~12份、甘露醇16~24份。
优选的,由以下组分制成:抗菌剂6份、脂肪醇聚氧乙烯醚30份、羟乙磺酸酯钠18份、椰子油脂肪酸二乙醇酰胺14份、去离子水12份、玫瑰精油2份、茶树油2份、棕榈油2份,丙二醇9份、山梨醇10份、甘露醇20份。
优选的,所述抗菌剂的制备方法,包括如下步骤:
(1)将纳米ZnO加入到KH560水溶液中,搅拌均匀,得到预处理纳米ZnO;
(2)将预处理纳米ZnO加入到DMF中,超声处理,加入三乙胺,在搅拌下滴加入N,N-二甲基乙二胺,搅拌反应,将产物离心、洗涤、干燥,得到接枝纳米ZnO;
(3)将接枝纳米ZnO、溴丁烷加入到四氢呋喃中,搅拌反应,将产物旋转蒸发,洗涤、干燥,得到抗菌剂。
优选的,步骤(1)中,所述KH560水溶液的浓度为5~10wt%,纳米ZnO与KH560水溶液的质量比为10:40~50。
优选的,步骤(1)中,搅拌条件为60~70℃下搅拌反应2~4h。
优选的,步骤(2)中,步骤(2)中,超声处理时间10~20min;预处理纳米ZnO、三乙胺、N,N-二甲基乙二胺的重量比为10:0.4~1:11~16。
优选的,步骤(2)中,步骤(2)中,搅拌反应条件为40~60℃下反应6~10h。
优选的,步骤(3)中,接枝纳米ZnO、溴丁烷的重量比为10:14~22。
优选的,步骤(3)中,搅拌反应条件为45~65℃下反应16~22h。
本发明还要求保护一种所述抗菌洗衣凝珠的制备方法,包括如下步骤:40~60℃下将抗菌剂、脂肪醇聚氧乙烯醚、羟乙磺酸酯钠、椰子油脂肪酸二乙醇酰胺加入到去离子水中搅拌均匀,冷却至室温,加入玫瑰精油、茶树油、棕榈油、丙二醇、山梨醇、甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠。
与现有技术相比,本发明具有如下有益效果:
1)本发明提供了一种抗菌洗衣凝珠,以脂肪醇聚氧乙烯醚、羟乙磺酸酯钠、椰子油脂肪酸二乙醇酰胺为表面活性剂,提供优良的去污能力;以玫瑰精油、茶树油作为芬香剂,能够提供持久的香气,使洗衣过后衣物能持续释放香味,并提供一定的抑菌性能;以棕榈油为柔顺剂,能够保护衣物纤维不受损伤;并提供了抗菌剂,能够提供持久、稳定、高效的杀菌效果,且对人体安全无害。
2)本发明提供了一种抗菌剂,首先用KH560对纳米ZnO进行处理,得到环氧基改性的预处理纳米ZnO,有效改善了纳米颗粒的分散性和反应活性;随后在催化剂三乙胺的作用下,通过N,N-二甲基乙二胺上氨基与预处理纳米ZnO上环氧基的反应引入叔胺基团得到接枝纳米ZnO,最后采用溴丁烷对上述叔胺化合物进行季胺化改性,制备得到季铵盐抗菌剂;纳米ZnO在可见光下能够产生活性氧和羟基自由基杀灭微生物,而季铵盐则能够使细胞膜通透性发生改变,渗出菌体细胞内容物阻碍细菌代谢达到抑菌、杀菌的作用,制备得到的抗菌剂能够协同发挥纳米ZnO和季铵盐的作用,起到高效的杀菌效果;此外,纳米ZnO上接枝长链基团后,改变了纳米ZnO的表面极性,由于疏水长链间的静电斥力,能够实现纳米ZnO在料液中的良好分散,使制备得到的洗衣凝珠具有较佳的稳定性。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本发明的某些实施例示意图,因此不应被看作是对范围的限定,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他相关的附图。
图1为本发明提供的抗菌剂的制备流程图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚,以下结合实施例,对本发明作进一步的详细说明。当然,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
如无特殊说明外,本发明中的化学试剂和材料均通过市场途径购买或通过市场途径购买的原料合成。
纳米ZnO购自江苏纳盾科技有限公司,粒径为82~110nm。
下面通过具体实施例,来对本发明作进一步的说明。
实施例1
一种抗菌洗衣凝珠的制备方法,包括如下步骤:
(1)将10g纳米ZnO加入到50g 10wt%KH560水溶液中,70℃下搅拌反应4h,得到预处理纳米ZnO;
(2)将10预处理纳米ZnO加入到50mL DMF中,超声处理20min,加入1g三乙胺,在搅拌下滴加入16g N,N-二甲基乙二胺,60℃下搅拌反应10h,将产物离心,用DMF、去离子水分别洗涤3次,干燥得到接枝纳米ZnO;
(3)将10g接枝纳米ZnO、22g溴丁烷加入到60mL四氢呋喃中,65℃下搅拌反应22h,旋转蒸发去除未反应物,洗涤、干燥,得到抗菌剂;
(4)50℃下将6g抗菌剂、30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠。
实施例2
一种抗菌洗衣凝珠的制备方法,包括如下步骤:
(1)将10g纳米ZnO加入到40g 5wt%KH560水溶液中,60℃下搅拌反应2h,得到预处理纳米ZnO;
(2)将10预处理纳米ZnO加入到50mL DMF中,超声处理10min,加入0.4g三乙胺,在搅拌下滴加入11g N,N-二甲基乙二胺,40℃下搅拌反应6h,将产物离心,用DMF、去离子水分别洗涤3次,干燥得到接枝纳米ZnO;
(3)将10g接枝纳米ZnO、14g溴丁烷加入到60mL四氢呋喃中,45℃下搅拌反应16h,旋转蒸发去除未反应物,洗涤、干燥,得到抗菌剂;
(4)50℃下将6g抗菌剂、30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠。
实施例3
一种抗菌洗衣凝珠的制备方法,包括如下步骤:
(1)将10g纳米ZnO加入到45g 8wt%KH560水溶液中,65℃下搅拌反应3h,得到预处理纳米ZnO;
(2)将10预处理纳米ZnO加入到50mL DMF中,超声处理15min,加入0.6g三乙胺,在搅拌下滴加入14g N,N-二甲基乙二胺,50℃下搅拌反应8h,将产物离心,用DMF、去离子水分别洗涤3次,干燥得到接枝纳米ZnO;
(3)将10g接枝纳米ZnO、16g溴丁烷加入到60mL四氢呋喃中,50℃下搅拌反应18h,旋转蒸发去除未反应物,洗涤、干燥,得到抗菌剂;
(4)50℃下将6g抗菌剂、30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠。
实施例4
一种抗菌洗衣凝珠的制备方法,包括如下步骤:
(1)将10g纳米ZnO加入到50g 10wt%KH560水溶液中,65℃下搅拌反应3h,得到预处理纳米ZnO;
(2)将10预处理纳米ZnO加入到50mL DMF中,超声处理15min,加入0.8g三乙胺,在搅拌下滴加入15g N,N-二甲基乙二胺,50℃下搅拌反应8h,将产物离心,用DMF、去离子水分别洗涤3次,干燥得到接枝纳米ZnO;
(3)将10g接枝纳米ZnO、18g溴丁烷加入到60mL四氢呋喃中,60℃下搅拌反应20h,旋转蒸发去除未反应物,洗涤、干燥,得到抗菌剂;
(4)50℃下将6g抗菌剂、30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠。
对比例1
一种洗衣凝珠的制备方法,包括如下步骤:
(1)将10g纳米ZnO加入到50g 10wt%KH560水溶液中,70℃下搅拌反应4h,得到预处理纳米ZnO;
(2)50℃下将6g预处理纳米ZnO、30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到洗衣凝珠。
对比例2
一种洗衣凝珠的制备方法,包括如下步骤:
(1)将16g N,N-二甲基乙二胺、22g溴丁烷加入到60mL四氢呋喃中,65℃下搅拌反应22h,旋转蒸发去除未反应物,洗涤、干燥,得到季铵盐;
(2)50℃下将6g季铵盐、30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到洗衣凝珠。
对比例3
一种洗衣凝珠的制备方法,包括如下步骤:
50℃下将30g脂肪醇聚氧乙烯醚、18g羟乙磺酸酯钠、14g椰子油脂肪酸二乙醇酰胺加入到12g去离子水中搅拌均匀,冷却至室温,加入2g玫瑰精油、2g茶树油、2g棕榈油、9g丙二醇、10g山梨醇、20g甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到洗衣凝珠。
参照GB/T 13174-2021《衣料用洗涤剂去污力及循环洗涤性能的测定》,将试验所需各种污布裁成6cm×6cm大小的试片,四片为一组。试验时用250mg/kg硬水,试样试验浓度为0.1%,标准洗衣液试验浓度为0.2%,以恒温30℃且固定转速120r/min持续20min后停止,漂洗二次后晾干,测定洗涤前后的白度值,计算出各个样品的去污力,具体数据见表1。
表1各洗衣凝珠的去污能力
炭黑污布 | 皮脂污布 | 食用油污布 | |
实施例1 | 1.3 | 1.4 | 1.6 |
实施例2 | 1.1 | 1.1 | 1.2 |
实施例3 | 1.2 | 1.2 | 1.3 |
实施例4 | 1.3 | 1.4 | 1.5 |
标准洗衣液 | 1.0 | 1.0 | 1.0 |
实施例1~4制备得到的洗衣凝胶的去污效果均>1,符合QB/T 1224-2012《衣料用液体洗涤剂》的要求。
取各实施例制备所得洗衣凝珠1颗溶解于1L去离子水中得到洗衣液,参考QB/T2738-2012《日化产品抗菌抑菌效果的评价方法》测定洗衣液的抗菌性能,具体数据见表2。
表2洗衣凝胶的抗菌效果(%)
大肠杆菌 | 金黄色葡萄球菌 | 白色念珠菌 | |
实施例1 | 99.3 | 99.9 | 93.2 |
实施例2 | 98.7 | 99.9 | 91.5 |
实施例3 | 98.9 | 99.9 | 92.3 |
实施例4 | 99.2 | 99.9 | 92.8 |
对比例1 | 43.5 | 36.8 | 33.9 |
对比例2 | 51.2 | 56.3 | 41.6 |
对比例3 | 15.8 | 16.7 | 12.4 |
取实施例1、对比例1制备所得洗衣凝珠1颗溶解于1L去离子水中得到洗衣液,将洗衣液在-5℃、25℃、45℃下存放20d、50d,观察洗衣液的外观、色泽,判断其稳定性,具体数据见表3。
表3洗衣凝胶的稳定性
对比例1制备所得洗衣凝胶得到的洗衣液,在室温、较高温度下存放20d时,便会观察到混浊物,推测为纳米ZnO的沉淀,而实施例1制备所得洗衣凝胶得到的洗衣液,则能在较高温度(45℃)下存放较长时间,说明接枝了疏水长链后能够有效增加纳米ZnO的分散性,使得洗衣凝胶具有较佳的储存稳定性。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种抗菌洗衣凝珠,其特征在于,由以下组分制成:抗菌剂4~8份、脂肪醇聚氧乙烯醚25~35份、羟乙磺酸酯钠15~20份、椰子油脂肪酸二乙醇酰胺10~18份、去离子水8~14份、玫瑰精油1~3份、茶树油1~3份、棕榈油1~3份,丙二醇5~12份、山梨醇8~12份、甘露醇16~24份。
2.根据权利要求1所述的抗菌洗衣凝珠,其特征在于,由以下组分制成:抗菌剂6份、脂肪醇聚氧乙烯醚30份、羟乙磺酸酯钠18份、椰子油脂肪酸二乙醇酰胺14份、去离子水12份、玫瑰精油2份、茶树油2份、棕榈油2份,丙二醇9份、山梨醇10份、甘露醇20份。
3.根据权利要求1所述的抗菌洗衣凝珠,其特征在于,所述抗菌剂的制备方法,包括如下步骤:
(1)将纳米ZnO加入到KH560水溶液中,搅拌均匀,得到预处理纳米ZnO;
(2)将预处理纳米ZnO加入到DMF中,超声处理,加入三乙胺,在搅拌下滴加入N,N-二甲基乙二胺,搅拌反应,将产物离心、洗涤、干燥,得到接枝纳米ZnO;
(3)将接枝纳米ZnO、溴丁烷加入到四氢呋喃中,搅拌反应,将产物旋转蒸发,洗涤、干燥,得到抗菌剂。
4.根据权利要求3所述的抗菌洗衣凝珠,其特征在于,步骤(1)中,所述KH560水溶液的浓度为5~10wt%,纳米ZnO与KH560水溶液的质量比为10:40~50。
5.根据权利要求3所述的抗菌洗衣凝珠,其特征在于,步骤(1)中,搅拌条件为60~70℃下搅拌反应2~4h。
6.根据权利要求3所述的抗菌洗衣凝珠,其特征在于,步骤(2)中,步骤(2)中,超声处理时间10~20min;预处理纳米ZnO、三乙胺、N,N-二甲基乙二胺的重量比为10:0.4~1:11~16。
7.根据权利要求3所述的抗菌洗衣凝珠,其特征在于,步骤(2)中,步骤(2)中,搅拌反应条件为40~60℃下反应6~10h。
8.根据权利要求3所述的抗菌洗衣凝珠,其特征在于,步骤(3)中,接枝纳米ZnO、溴丁烷的重量比为10:14~22。
9.根据权利要求3所述的抗菌洗衣凝珠,其特征在于,步骤(3)中,搅拌反应条件为45~65℃下反应16~22h。
10.一种如权利要求1~9任一项所述抗菌洗衣凝珠的制备方法,其特征在于,包括如下步骤:40~60℃下将抗菌剂、脂肪醇聚氧乙烯醚、羟乙磺酸酯钠、椰子油脂肪酸二乙醇酰胺加入到去离子水中搅拌均匀,冷却至室温,加入玫瑰精油、茶树油、棕榈油、丙二醇、山梨醇、甘露醇,搅拌均匀后将料液送入自动包装机,进行PVA水溶膜包装,得到抗菌洗衣凝珠。
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