CN108978355A - 一种艾草/氧化石墨烯抗菌壁纸 - Google Patents
一种艾草/氧化石墨烯抗菌壁纸 Download PDFInfo
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Abstract
本发明公开了一种艾草/氧化石墨烯抗菌壁纸,该壁纸由如下步骤制备得到:将原料纤维经过打浆筛选处理,通过成型网成型得到湿纸幅,在前干燥后喷涂氧化石墨烯/含氟丙烯酸酯改性纤维素,经过后干燥和压光处理制备得到壁纸原纸,将壁纸原纸浸润在艾草提取物、丁香提取物物和蒲公英提取物的混合提取物中,干燥得到艾草/氧化石墨烯抗菌壁纸。本发明的艾草/氧化石墨烯抗菌壁纸在纸基制备过程中添加抗菌氧化石墨烯/改性纤维素助剂,其防水防油性能可进一步减少壁纸上的油和水分,避免细菌滋生,浸润液中的多种植物抗菌提取物复配使用进一步提高了湿巾的抗菌效果,抗菌的效果在95%以上,具有综合的抗菌防油效果,可广泛使用于建筑装修材料领域。
Description
技术领域
本发明属于建筑装饰材料技术领域,更具体地,涉及一种艾草/氧化石墨烯抗菌壁纸。
背景技术
壁纸,也称为墙纸,它是一种应用广泛的室内装饰材料。因为壁纸具有风格多变、色彩多样、图案丰富、安全环保、施工方便、价格适宜、易于更换等多种其它室内装饰材料所无法比拟的特点,故在欧美、东南亚、日韩等发达国家和地区得到相当程度的普及。随着我国人民生活水平的提升,壁纸因其色彩与风格的多样性,而广受消费者的青睐。但现今市场上的丝绸壁纸普遍存在易发霉现象,特别是在江南地区,另外,在厨房、餐厅等地方对防油和防水性能也有一定需求,显然,目前的壁纸产品无法满足这些需求。目前对壁纸抗菌性能的提升上的研究多是在纸基或者其他的壁纸基材上以压层的方式增加一层抗菌层,但是这种方法智能保证壁纸表面的抗菌性能,抗菌效果有限,而且一旦表面遭到破会,就不能很好的保证壁纸的抗菌效果。
因此,制备一种能具备有效抗菌效果的抗菌壁纸具有非常重要的实际应用价值。
发明内容
本发明要解决的技术问题是克服现有技术抗菌效果不持久,不稳定,提供一种艾草/氧化石墨烯抗菌壁纸,通过对壁纸原料纸基进行抗菌改造,抗菌效果更好。
本发明上述目的通过以下技术方案实现:
一种艾草/氧化石墨烯抗菌壁纸,由如下步骤制备得到:
S1.将原料纤维经过打浆筛选处理,通过成型网成型得到湿纸幅,在前干燥后喷涂氧化石墨烯/含氟丙烯酸酯改性纤维素,经过后干燥和压光处理制备得到壁纸原纸;
S2.将上述S1中的壁纸原纸浸润在混合提取物中,浸入2~4h,干燥得到艾草/氧化石墨烯抗菌壁纸,所述混合提取物为艾草提取物、丁香提取物物和蒲公英提取物的混合物。
木浆纤维和棉纤维都是天然纤维素原料,具有良好的透气性和生物降解性,由木浆纤维和棉纤维制备的基材具有良好的生物可降解,氧化石墨烯改性纤维素抗菌剂在制备过程中加入可以提高抗菌剂的留着率和稳定负载性,从而提高壁纸的抗菌性。
艾草对许多病毒和细菌都有抑制和杀伤作用,主要的化学成分是水芹烯、β- 细辛醚等,对金黄色葡萄球菌等有很强的杀伤力。丁香和蒲公英提取物也具有很好的植物抗菌效果,三者复配使用可以起到很好的协同抗菌作用。且植物提取还具有宜人的天然香气,可以使得壁纸使用空间更加清新。
优选地,S2中所述艾草提取物、丁香提取物物和蒲公英提取物的质量比为 1~1.5:0.8~1.2:0.5~0.8。
优选地,S2中所述艾草提取物、丁香提取物物和蒲公英提取物的质量比为 1.2:1:0.5。
优选地,S1中氧化石墨烯/含氟丙烯酸酯改性纤维素的喷涂量为纤维质量的 1.2~2.5%。
优选地,S1中所述氧化石墨烯/含氟丙烯酸酯改性纤维素的制备方法为:
S11.制备含氟丙烯酸酯改性纤维素:将乳化剂、水和含氟丙烯酸酯单体混合预乳化,在惰性气体条件下加入纤维素溶液和引发剂,聚合合成改性纤维素,其中聚合温度为50~60℃,聚合时间为4~7h,乳化剂为十二烷基硫酸钠,乳化剂用量为含氟丙烯酸酯单体质量的3~5%,引发剂为过硫酸钾,引发剂用量为含氟丙烯酸酯单体质量的2~6%,纤维素与含氟丙烯酸酯单体的质量比为1:2~1:6;
S12.制备氧化石墨烯/含氟丙烯酸酯改性纤维素:配制强碱、尿素和硫脲的混合溶液,冷却至-10~-20℃,搅拌加入S1中的改性纤维素和均匀分散的氧化石墨烯溶液,保持温度不变,搅拌反应4~6h,调节pH至中性,即得到氧化石墨烯 /含氟丙烯酸酯改性纤维素,其中改性纤维素与氧化石墨烯的质量比为1:0.2~0.5,改性纤维素与强碱、尿素、硫脲的质量比为1:1.5~2:1~1.5:1.5~2。
由于纤维素具丰富的表面羟基,可以与诸多改性基团进行改性,纤维素进行改性后可综合提升其防油抗菌性能。含氟丙烯酸酯共聚乳液具有良好的稳定性,其聚合物中含有全氟侧链基团,氟的电负性大,氟原子具有孤对电子,C-F键的键能要远大于C-H键,因此其表面自由能较低,这样使得含氟聚合物具有较好的稳定性、耐化学药品性、耐候性、电绝缘性、耐玷污性、疏水疏油性和其它一些性能等许多优异的性能。
纤维素自身为三维网络结构,其结构体系疏松多孔,可为其他辅助材料提供载体和附着点,可与石墨烯发生插层复合反应,得到氧化石墨烯/改性纤维素助剂。石墨烯具有优异的抗菌性能,单体改性的疏水疏油纤维素骨架内负载氧化石墨烯可以提高整个纤维助剂的抗菌性,得到综合抗菌抗污性能优异的助剂材料。
优选地,S12中所述改性纤维素与氧化石墨烯的质量比为1:0.3。石墨烯含量过低会导致材料的抗菌性能不够,过多则在反应体系中流失。
优选地,S1中所述乳化剂用量为含氟丙烯酸酯单体质量的4.5%。
乳化剂太少不能形成稳定的乳液体系,使得乳液容易破乳。随着乳化剂用量的增多,乳液分散得更细,更均匀,体系中增溶单体的胶束数目增多,乳胶粒数目增多,相应的粒子表面积也随之增大,有益于传质的进行,从而更容易发生接枝反应,即单体发生聚合反应转化为聚合物的场所就更多,因此接枝率增加。当乳化剂用量过大时,增加了反应体系的粘度,影响了自由基的扩散,从而阻碍了乳液合成的进度,并增加了成本,同时会影响施胶效果,聚合物乳液在使用中易发泡,易使涂膜的耐水性变差。
优选地,S1中所述引发剂用量为含氟丙烯酸酯单体质量的4%。纤维素含氟单体改性是自由基聚合反应,引发剂是自由基聚合的关键部分,直接影响产品的产量和质量,并影响聚合反应的速率。引发剂的作用主要是引发纤维素形成自由基,然后单体接枝到自由基上,引发剂量的增加会使得自由基含量增多,反应机率增加,从而使转化率、接枝率和接枝效率增大。当引发剂超过一定用量,可引发产生自由基的数量达到饱和,从而会使转化率、接枝率和接枝效率降低。
优选地,S1中所述纤维素与含氟丙烯酸酯单体的质量比1:5。因为纤维素上的活性位点是有限的,而含氟单体之间有可能发生自聚反应,自聚反应与接枝反应竞争活性链,单体浓度过高则会出现自聚反应占主导地位。
与现有技术相比,本发明的有益效果是:
本发明提供了一种艾草/氧化石墨烯抗菌壁纸,在纸基制备过程中添加氧化石墨烯/改性纤维素抗菌防油助剂,抗菌效果更稳定持久,且其防水防油性能可进一步减少壁纸上的油和水分,避免细菌滋生,浸润液中的多种植物抗菌提取物复配使用进一步提高了湿巾的抗菌效果,达到双重抗菌的效果,对大肠杆菌、金黄色葡萄球菌和霉菌的抑制率均在95%以上,具有综合的抗菌防油效果,可广泛使用于建筑装修材料领域。
具体实施方式
实施例1~7
一种艾草/氧化石墨烯抗菌壁纸,由如下步骤制备得到:
S1.将原料纤维经过打浆筛选处理,通过成型网成型得到湿纸幅,在前干燥后喷涂氧化石墨烯/含氟丙烯酸酯改性纤维素,经过后干燥和压光处理制备得到壁纸原纸;
S2.将上述S1中的壁纸原纸浸润在混合提取物中,浸入2~4h,干燥得到艾草/氧化石墨烯抗菌壁纸,所述混合提取物为艾草提取物、丁香提取物物和蒲公英提取物的混合物。
其中氧化石墨烯/含氟丙烯酸酯改性纤维素的喷涂量及混合提取物的组分具体见表1。
序号 | 喷涂量/% | 艾草提取物:丁香提取物物:蒲公英提取物 |
实施例1 | 2 | 1.2:1:0.5 |
实施例2 | 1.2 | 1.2:1:0.5 |
实施例3 | 2.5 | 1.2:1:0.5 |
实施例4 | 2 | 1:1:0.5 |
实施例5 | 2 | 1.5:1:0.5 |
实施例6 | 2 | 1.2:0.8:0.5 |
实施例7 | 2 | 1.2:0.8:0.8 |
实施例8~16
一种艾草/氧化石墨烯抗菌壁纸,其制备方法与实施例1基本相同,其中氧化石墨烯/含氟丙烯酸酯改性纤维素的制备方法如下:
S11.制备含氟丙烯酸酯改性纤维素:将乳化剂、水和甲基丙烯酸六氟丁酯混合预乳化,在惰性气体条件下加入纳米纤维素溶液和引发剂,聚合合成改性纤维素,聚合时间为6h,乳化剂为十二烷基硫酸钠,引发剂为过硫酸钾;
S12.制备氧化石墨烯/含氟丙烯酸酯改性纤维素:配制强碱、尿素和硫脲的混合溶液,冷却至-10℃,搅拌加入S11中的改性纤维素和均匀分散的氧化石墨烯溶液,保持温度不变,搅拌反应6h,调节pH至中性,即得到氧化石墨烯/含氟丙烯酸酯改性纤维素,改性纤维素与强碱、尿素、硫脲的质量比为1:1.6:1.3:1.6。
具体制备参数见表2。其中乳化剂用量为A%(以甲基丙烯酸六氟丁酯质量计);引发剂用量为B%(以甲基丙烯酸六氟丁酯质量计);纤维素与含氟丙烯酸酯单体的质量比为C,改性纤维素与氧化石墨烯的质量比为E。
表2
序号 | A | B | C | E |
实施例8 | 4.5 | 4 | 1:5 | 1:0.3 |
实施例9 | 3 | 4 | 1:5 | 1:0.3 |
实施例10 | 5 | 4 | 1:5 | 1:0.3 |
实施例11 | 4.5 | 2 | 1:5 | 1:0.3 |
实施例12 | 4.5 | 6 | 1:5 | 1:0.3 |
实施例13 | 4.5 | 4 | 1:2 | 1:0.3 |
实施例14 | 4.5 | 4 | 1:6 | 1:0.3 |
实施例15 | 4.5 | 4 | 1:5 | 1:0.2 |
实施例16 | 4.5 | 4 | 1:5 | 1:0.5 |
对比例1
一种艾草/氧化石墨烯抗菌壁纸,由如下步骤制备得到:
S1.将原料纤维经过打浆筛选处理,通过成型网成型得到湿纸幅,在前干燥后喷涂氧化石墨烯,经过后干燥和压光处理制备得到壁纸原纸,喷涂量为2%;
S2.将上述S1中的壁纸原纸浸润在混合提取物中,浸入2~4h,干燥得到艾草/氧化石墨烯抗菌壁纸,所述混合提取物为艾草提取物、丁香提取物物和蒲公英提取物的混合物,艾草提取物、丁香提取物物和蒲公英提取物的质量比为 1.2:1:0.5。
对比例2
一种抗菌壁纸,由如下步骤制备得到:
S1.将原料纤维经过打浆筛选处理,通过成型网成型得到湿纸幅,经过后干燥和压光处理制备得到壁纸原纸,;
S2.将上述S1中的壁纸原纸浸润在混合提取物中,浸入2~4h,干燥得到艾草/氧化石墨烯抗菌壁纸,所述混合提取物为艾草提取物、丁香提取物物和蒲公英提取物的混合物,艾草提取物、丁香提取物物和蒲公英提取物的质量比为 1.2:1:0.5。
结果检测
(1)防油防水性检测
采用接触角测量仪测量实施例和对比例制备的壁纸的防油防水性能。检测结果见表3。
表3
序号 | 防水接触角/度 | 防油接触角/度 |
实施例1 | 165.2 | 154.1 |
实施例2 | 151.6 | 133.7 |
实施例3 | 152.6 | 143.5 |
实施例8 | 164.4 | 153.8 |
实施例9 | 147.7 | 137.8 |
实施例10 | 156.1 | 146.2 |
实施例11 | 150.6 | 140.5 |
实施例12 | 152.7 | 142.5 |
实施例13 | 145.6 | 135.9 |
实施例14 | 155.2 | 147.3 |
实施例15 | 155.7 | 148.2 |
实施例16 | 153.7 | 144.3 |
对比例1 | 亲水 | 116.6 |
对比例2 | 32.8 | 56.8 |
(2)抗菌性检测
测定实施例和对比例制备的壁纸对金黄色葡萄球菌、大肠杆菌和霉菌的抑制率。取适当浓度的大肠杆菌、金黄色葡萄球菌和霉菌的悬液里,混合均匀,加入培养基置于灭菌平皿里,加入实施例和对比例制备的纸基薄片,培养24h,计算大肠杆菌、金黄色葡萄球菌和霉菌抑制率。检测结果如下表4。
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。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。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。
Claims (9)
1.一种艾草/氧化石墨烯抗菌壁纸,其特征在于,由如下步骤制备得到:
S1. 将原料纤维经过打浆筛选处理,通过成型网成型得到湿纸幅,在前干燥后喷涂氧化石墨烯/含氟丙烯酸酯改性纤维素,经过后干燥和压光处理制备得到壁纸原纸;
S2. 将上述S1中的壁纸原纸浸润在艾草混合提取物中,浸入2~4h,干燥得到艾草/氧化石墨烯抗菌壁纸,所述混合提取物为艾草提取物、丁香提取物物和蒲公英提取物的混合物。
2.如权利要求1所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S2中所述艾草提取物、丁香提取物物和蒲公英提取物的质量比为1~1.5:0.8~1.2:0.5~0.8。
3.如权利要求1所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S2中所述艾草提取物、丁香提取物物和蒲公英提取物的质量比为1.2:1:0.5。
4.如权利要求1所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S1中氧化石墨烯/含氟丙烯酸酯改性纤维素的喷涂量为纤维质量的1.2~2.5%。
5.如权利要求1所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S1中所述氧化石墨烯/含氟丙烯酸酯改性纤维素的制备方法为:
S11. 制备含氟丙烯酸酯改性纤维素:将乳化剂、水和含氟丙烯酸酯单体混合预乳化,在惰性气体条件下加入纤维素溶液和引发剂,聚合合成改性纤维素,其中聚合温度为50~60℃,聚合时间为4~7h,乳化剂为十二烷基硫酸钠,乳化剂用量为含氟丙烯酸酯单体质量的3~5%,引发剂为过硫酸钾,引发剂用量为含氟丙烯酸酯单体质量的2~6%,纤维素与含氟丙烯酸酯单体的质量比为1:2~1:6;
S12. 制备氧化石墨烯/含氟丙烯酸酯改性纤维素:配制强碱、尿素和硫脲的混合溶液,冷却至-10~-20℃,搅拌加入S1中的改性纤维素和均匀分散的氧化石墨烯溶液,保持温度不变,搅拌反应4~6h,调节pH至中性,即得到氧化石墨烯/含氟丙烯酸酯改性纤维素,其中改性纤维素与氧化石墨烯的质量比为1:0.2~0.5,改性纤维素与强碱、尿素、硫脲的质量比为1:1.5~2:1~1.5:1.5~2。
6.如权利要求5所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S12中所述改性纤维素与氧化石墨烯的质量比为1:0.3。
7.如权利要求5所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S1中所述乳化剂用量为含氟丙烯酸酯单体质量的4.5%。
8.如权利要求5所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S1中所述引发剂用量为含氟丙烯酸酯单体质量的4%。
9.如权利要求5所述艾草/氧化石墨烯抗菌壁纸,其特征在于,S1中所述纤维素与含氟丙烯酸酯单体的质量比1:5。
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