CN107805427B - 一种氧化镁/石墨烯抗菌涂料的制备方法 - Google Patents
一种氧化镁/石墨烯抗菌涂料的制备方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 52
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 52
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 52
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 8
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- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 8
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 10
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- 159000000003 magnesium salts Chemical class 0.000 claims description 4
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 4
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
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- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 2
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 claims description 2
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
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- ICUTUKXCWQYESQ-UHFFFAOYSA-N triclocarban Chemical compound C1=CC(Cl)=CC=C1NC(=O)NC1=CC=C(Cl)C(Cl)=C1 ICUTUKXCWQYESQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种氧化镁/石墨烯抗菌涂料的制备方法，属于功能涂料生产技术领域。在微波水热条件下，通过助剂改性，在氧化石墨表面原位生长氢氧化镁纳米片获得复合物前驱体，再通过高温热还原得到氧化镁/石墨烯复合材料；将制备的氧化镁/石墨烯复合材料作为抗菌剂添加到水性树脂中制备成抗菌涂料。本发明的制备方法简单、高效、产率高，产品粒径大小均一并适用于工业化生产；将氧化镁/石墨烯复合材料应用到水性树脂中制备成抗菌涂料，解决了抗菌涂料存在二次污染，依赖紫外光照杀菌的不足，有利于实现稳定持久的抗菌保护。本发明不仅提高了氧化镁基复合材料和涂料的抗菌性能，而且制备的抗菌涂料应用领域广泛，具有良好的应用前景。
Description
技术领域
本发明属于功能涂料生产技术领域，具体涉及到一种氧化镁/石墨烯抗菌涂料的制备方法。
背景技术
医院手术室、食品发酵车间、药品加工工厂等卫生要求严格场所的内墙表面以及使用频率较高的家具、家电、织物等均需要进行抗菌处理，使用抗菌涂料是简单、可行的方法之一。目前抗菌涂料中使用的抗菌剂主要包括天然抗菌剂、有机抗菌剂、金属离子抗菌剂和纳米抗菌材料，如壳聚糖、山葵、三氯卡班、吡啶硫酮锌，氧化锌，氧化铜、二氧化钛、银纳米粒子等。一些抗菌剂虽然具有高效的抗菌活性，但由于结构稳定性差、光依赖性强、生物毒性不明确等原因限制了其在实际环境中的应用。随着绿色环保理念的日益提升，开发制备工艺简便、稳定持久、广谱抗菌和环境相容性优异的抗菌剂其抗菌涂料成为当前研究的热点问题。
纳米氧化镁具有持久和广谱的抗菌活性，可以克服银系抗菌材料的成本高、易变色、稳定性差、生物毒性等问题，也可以弥补光催化抗菌材料抗菌效率低和对紫外光依赖的不足，是一种安全无毒、环境友好、有着巨大应用潜力的抗菌材料。目前已经报道了多种氧化镁结构调控方法，但如何提高其抗菌性能并且大规模制备高性能复合材料和抗菌涂料是当前迫切需要解决的问题。
发明内容
本发明的目的是提供一种氧化镁/石墨烯抗菌涂料的制备方法，即在微波水热条件下，通过助剂改性，在氧化石墨表面原位生长氢氧化镁纳米片获得复合物前驱体，再通过高温热还原得到氧化镁/石墨烯复合材料；将制备的氧化镁/石墨烯复合材料作为抗菌剂添加到水性树脂中制备成抗菌涂料。制备的抗菌涂料具有抑制细菌繁殖，改善环境卫生的功能。
本发明的技术方案：
一种氧化镁/石墨烯抗菌涂料的制备方法，步骤如下：
步骤1.氧化镁/石墨烯复合材料的制备：在40～50℃下，将浓度为0.5～1g/L的氧化石墨分散液滴加到助剂溶液中，磁力搅拌直至混合均匀；再向混合体系中滴加镁盐溶液继续搅拌20～60min，再滴加碱溶液，继续搅拌2h得到悬浊液；将悬浊液转移到微波水热釜中，在140～180℃温度下，反应15～45min，得到氢氧化镁/氧化石墨复合前驱体；将氢氧化镁/氧化石墨复合前驱体在氮气气氛中、500～650℃温度条件下，进行热还原处理，得到氧化镁/石墨烯复合材料；所述的氧化镁/石墨烯复合材料中氧化镁和石墨烯的质量比为4:1～19:1；所述的助剂在悬浊液中的浓度为0.005～0.2g/L；所述的碱控制悬浊液的pH＝8～11；
步骤2.抗菌涂料的制备，按重量百分比计：取5-20份氧化镁/石墨烯复合材料加入到60-85份水性树脂中，用分散机进行充分搅拌；再依次加入0.1-2份的分散剂和0.1-2份消泡剂，搅拌均匀；然后，加入8-15份高岭土、5-10份钛白粉和0.5-1份增稠剂，搅拌0.5-3h，即得到氧化镁/石墨烯抗菌涂料。
所述的镁盐为六水合硝酸镁(Mg(NO3)2·6H2O)、六水合氯化镁(MgCl2·6H2O)、七水合硫酸镁(MgSO4·7H2O)选取任意一种。
所述的碱为氢氧化钠(NaOH)、氨水(NH3·H2O)选取任意一种。
所述的助剂为聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物(P123)、十六烷基三甲基溴化铵(CTAB)、聚乙烯吡咯烷酮-K30(PVP)、十二烷基苯磺酸钠(SDBS)选取任意一种。
所述的水性树脂为改性聚醋酸乙烯乳液、聚丙烯酸乳液、水性聚氨酯乳液中的一种或两种以上。
所述的分散剂为硅酸钠、硅酸钾、三聚磷酸钠、六偏磷酸钠中选取任意一种。
所述的消泡剂为聚醚改性硅氧烷。
所述的增稠剂为聚丙烯酸酯、缔合型聚氨酯、甲基纤维素、羧甲基纤维素、羟乙基纤维素、羟丙基甲基纤维素选取任意一种。
本发明的效果和益处：采用微波水热法辅助原位生长制备氧化镁/石墨烯复合材料，方法简单、高效、产率高，产品粒径大小均一并适用于工业化生产；将氧化镁/石墨烯复合材料应用到水性树脂中制备成抗菌涂料，解决了抗菌涂料存在二次污染，依赖紫外光照杀菌的不足，有利于实现稳定持久的抗菌保护。本发明不仅提高了氧化镁基复合材料和涂料的抗菌性能，而且制备的抗菌涂料可以广泛应用于医院、工厂、公共交通、家用电器、航天器材、医疗器械、产品包装等方面，具有良好的应用前景。
附图说明
图1为氧化镁/石墨烯复合材料的TEM图。
具体实施方式
以下结合技术方案叙述本发明的具体实施方式。
实施例1
步骤1.制备氧化镁/石墨烯复合材料：在45℃下，取CTAB10g加入200mL去离子水中搅拌直至完全溶解，取403mL浓度为0.5g/L的氧化石墨烯分散液滴加到上述溶液中在1000r/min下搅拌30min。并在磁力搅拌下滴加200mL81.32g/L的MgCl2·6H2O溶液，继续搅拌30min后，将200mL的32g/LNaOH溶液滴加到上述溶液中继续搅拌2h，将悬浊液转移到微波水热釜中，在180℃下微波水热30min，使氢氧化镁纳米片在氧化石墨上进行原位沉积。将所得前驱体过滤，60℃下干燥8h，在氮气气氛下以2℃/min的升温速率升温到600℃煅烧2h后自然冷却到室温，即得到氧化镁:石墨烯质量比为16:1的氧化镁/石墨烯复合材料。
步骤2.制备抗菌涂料(组分按重量百分比)：改性聚醋酸乙烯乳液70份，氧化镁/石墨烯复合材料5份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土12份，钛白粉10份。
材料的抗菌性能测试：参照GBT 21866-2008、GBT 21510-2008、QB/T2591-2003(GB/T2591-2003A)的标准方法测试实施例所得的材料的抗菌效果，结果表明测定对金黄色葡萄球菌和大肠杆菌的抗菌率均大于98％。
实施例2
步骤1.制备氧化镁/石墨烯复合材料的方法与实施例1相同。
步骤2.制备抗菌涂料(组分按重量百分比)：改性聚醋酸乙烯乳液70份，氧化镁/石墨烯复合材料10份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土10份，钛白粉10份。
实施例3
步骤1.制备氧化镁/石墨烯复合材料的方法与实施例1相同。
步骤2.制备抗菌涂料(组分按重量百分比)：改性聚醋酸乙烯乳液70份，氧化镁/石墨烯复合材料20份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土8份，钛白粉10份。
实施例4
步骤1.制备氧化镁/石墨烯复合材料的方法与实施例1相同。
步骤2.制备抗菌涂料(组分按重量百分比)：聚丙烯酸乳液80份，氧化镁/石墨烯复合材料15份，硅酸钠0.5份，聚醚改性硅氧烷2份，聚丙烯酸酯2份，高岭土8份，钛白粉10份。
实施例5
步骤1.制备氧化镁/石墨烯复合材料的方法与实施例1相同。
步骤2.制备抗菌涂料(组分按重量百分比)：水性聚氨酯乳液75份，氧化镁/石墨烯复合材料5份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土15份，钛白粉8份。
实施例6
步骤1.制备氧化镁/石墨烯复合材料：在45℃下，取助剂CTAB10g加入200mL去离子水中搅拌直至完全溶解，取806mL浓度为0.5g/L的氧化石墨烯分散液滴加到上述溶液中在1000r/min下搅拌30min。并在磁力搅拌下滴加200mL浓度为102.56g/L的Mg(NO3)2·6H2O溶液，继续搅拌30min后，将200mL32g/LNaOH溶液滴加到上述溶液中继续搅拌2h，将悬浊液转移到微波水热釜中，在180℃下微波水热20min，使氢氧化镁纳米片在氧化石墨上进行原位沉积。将所得前驱体过滤，60℃下干燥8h，在氮气气氛下以2℃/min的升温速率升温到600℃煅烧2h后自然冷却到室温，即得到氧化镁:石墨烯质量比为8:1的氧化镁/石墨烯复合材料。
步骤2.制备抗菌涂料(组分按重量百分比)：改性聚醋酸乙烯乳液70份，氧化镁/石墨烯复合材料10份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土10份，钛白粉10份。
实施例7
步骤1.制备氧化镁/石墨烯复合材料的方法与实施例6相同。
步骤2.制备抗菌涂料(组分按重量百分比)：改性聚醋酸乙烯乳液70份，氧化镁/石墨烯复合材料20份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土8份，钛白粉10份。
实施例8
步骤1.制备氧化镁/石墨烯复合材料的方法与实施例6相同。
步骤2.制备抗菌涂料(组分按重量百分比)：水性聚氨酯乳液75份，氧化镁/石墨烯复合材料10份，硅酸钠0.5份，聚醚改性硅氧烷2份，缔合型聚氨酯2份，高岭土10份，钛白粉8份。
Claims (10)
1.一种氧化镁/石墨烯抗菌涂料的制备方法，其特征在于，步骤如下：
步骤1.氧化镁/石墨烯复合材料的制备：在40～50℃下，将浓度为0.5～1g/L的氧化石墨分散液滴加到助剂溶液中，磁力搅拌直至混合均匀；再向混合体系中滴加镁盐溶液继续搅拌20～60min，再滴加碱溶液，继续搅拌2h得到悬浊液；将悬浊液转移到微波水热釜中，在140～180℃温度下，反应15～45min，得到氢氧化镁/氧化石墨复合前驱体；将氢氧化镁/氧化石墨复合前驱体在氮气气氛中、500～650℃温度条件下，进行热还原处理，得到氧化镁/石墨烯复合材料；所述的氧化镁/石墨烯复合材料中氧化镁和石墨烯的质量比为4:1～19:1；所述的助剂在悬浊液中的浓度为0.005～0.2g/L；所述的碱控制悬浊液的pH＝8～11；
步骤2.抗菌涂料的制备，按重量百分比计：取5-20份氧化镁/石墨烯复合材料加入到60-85份水性树脂中，用分散机进行充分搅拌；再依次加入0.1-2份的分散剂和0.1-2份消泡剂，搅拌均匀；然后，加入8-15份高岭土、5-10份钛白粉和0.5-1份增稠剂，搅拌0.5-3h，即得到氧化镁/石墨烯抗菌涂料。
2.根据权利要求1所述的制备方法，其特征在于，所述的镁盐为六水合硝酸镁、六水合氯化镁或七水合硫酸镁。
3.根据权利要求1或2所述的制备方法，其特征在于，所述的碱为氢氧化钠或氨水。
4.根据权利要求3所述的制备方法，其特征在于，所述的助剂为聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物、十六烷基三甲基溴化铵、聚乙烯吡咯烷酮-K30或十二烷基苯磺酸钠。
5.根据权利要求1、2或4所述的制备方法，其特征在于，所述的水性树脂为改性聚醋酸乙烯乳液、聚丙烯酸乳液、水性聚氨酯乳液中的一种或两种以上。
6.根据权利要求5所述的制备方法，其特征在于，所述的分散剂为硅酸钠、硅酸钾、三聚磷酸钠或六偏磷酸钠。
7.根据权利要求6所述的制备方法，其特征在于，所述的消泡剂为聚醚改性硅氧烷。
8.根据权利要求1、2、4、6或7所述的制备方法，其特征在于，所述的增稠剂为聚丙烯酸酯、缔合型聚氨酯、甲基纤维素、羧甲基纤维素、羟乙基纤维素或羟丙基甲基纤维素。
9.根据权利要求3所述的制备方法，其特征在于，所述的增稠剂为聚丙烯酸酯、缔合型聚氨酯、甲基纤维素、羧甲基纤维素、羟乙基纤维素或羟丙基甲基纤维素。
10.根据权利要求5所述的制备方法，其特征在于，所述的增稠剂为聚丙烯酸酯、缔合型聚氨酯、甲基纤维素、羧甲基纤维素、羟乙基纤维素或羟丙基甲基纤维素。
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