CN114887667A - 一种新型的光催化空气净化材料的制备方法 - Google Patents
一种新型的光催化空气净化材料的制备方法 Download PDFInfo
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
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- BBCQSMSCEJBIRD-UHFFFAOYSA-N 3-fluorophthalic acid Chemical compound OC(=O)C1=CC=CC(F)=C1C(O)=O BBCQSMSCEJBIRD-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了一种新型的光催化空气净化材料的制备方法,包括:取4mol/L的氢氧根碱源置于烧杯中,将4mol/L的锡源溶液加入到烧杯中,搅拌后放入内村,加热,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料;取SnO2纳米材料、苯二甲酸源和锆源一起溶解在DMF和酸源的混合溶液中,然后加热保持,冷却至室温,用甲醇清洗离心,干燥得到UiO‑66‑(OH)2/SnO2复合纳米材料。本发明还提供一种新型的光催化空气净化材料,由所述的新型的光催化空气净化材料的制备方法制备而成。制得的UiO‑66‑(OH)2/SnO2复合纳米材料,具有高比表面积且结构/功能容易调节且分布有大量官能团,能够在室温下持续、快速吸附室内空气中低浓度甲醛污染物且高效杀菌性能。
Description
技术领域
本发明涉及空气污染治理技术领域,特别是涉及一种新型的光催化空气净化材料的制备方法。
背景技术
空气中污染物浓度如果达到一定有害程度,超过了环境质量标准会对人造成一定危害。室内空气污染也不容忽视,在室内空气中存在500多种挥发性物质,其中致癌物质就有20多种,致病病毒200多种。目前,危害较大的主要是甲醛、苯等有害气体,其中污染物甲醛对人体的危害具长期性、潜伏性、隐蔽性的特点,长期吸入甲醛会使人嗅觉异常,严重的甚至可能致畸、致癌风险。并且在环境问题日趋严重、病原体微生物随处可见的形势下,开发出新型多功能、安全环保的杀菌除醛材料显得尤为重要。
目前,市面上解决室内污染物常用的吸附剂有活性炭、分子筛、粘土等。杀菌材料的种类繁多,其中光催化型杀菌材料主要是二氧化钛催化剂。这些材料虽然能吸附一定浓度的甲醛,也能起到一定的杀菌效果。但是因为他们都存在比表面积不够以致于效率低、只有紫外吸收杀菌、效果差等问题,现阶段既能杀菌且除甲醛的催化剂效率低,因此,开发一种高效杀菌除醛材料具有重要意义。
发明内容
基于此,本发明的目的在于,解决市面上常见吸附剂有活性炭等材料在大多数低压条件下对空气有害气体的吸附能力较弱、且大多数催化剂杀菌效率低等问题,提供一种新型的光催化空气净化材料的制备方法。
第一方面,一种新型的光催化空气净化材料的制备方法,包括:
取4mol/L的氢氧根碱源置于烧杯中,将4mol/L的锡源溶液加入到烧杯中,搅拌后放入内村,加热,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料;
取SnO2纳米材料、苯二甲酸源和锆源一起溶解在DMF和酸源的混合溶液中,然后加热保持,冷却至室温,用甲醇清洗离心,干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
上述技术方案在一种实施方式中,取50毫升4mol/L氢氧根碱源置于烧杯中,将25毫升4mol/L的锡源溶液加入到烧杯中,搅拌1h后放入内村,在160-200℃下加热12-24h,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料。
上述技术方案在一种实施方式中,取SnO2纳米材料10g、2mmol苯二甲酸源和2mmol锆源一起溶解在DMF:酸源=1-3:1的100毫升混合溶液中,然后在110℃下保持4h,冷却至室温,用甲醇清洗离心,在80℃下干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
上述技术方案在一种实施方式中,所述氢氧根碱源为NaOH、KOH、氨水中的一种或多种。
上述技术方案在一种实施方式中,所述锡源包括氧化亚锡、氯化亚锡、四氯化锡中的一种或多种。
上述技术方案在一种实施方式中,所述苯二甲酸源包括2-氨基1,4苯二甲酸、邻苯二甲酸、3-氟邻苯二甲酸、3-氨基苯二甲酸中的一种或多种。
上述技术方案在一种实施方式中,所述锆源包括ZrCl4、ZrF4、ZrBr4、ZrI4中的一种或多种。
上述技术方案在一种实施方式中,所述酸源包括碳酸、亚硝酸、醋酸、亚硫酸中的一种或多种。
第二方面,本发明提供一种新型的光催化空气净化材料,由上述任一项所述的新型的光催化空气净化材料的制备方法制备而成。
相对于现有技术,本发明提供的一种新型的UiO-66-(OH)2/SnO2复合纳米材料光催化空气净化材料的制备方法,其原方法设备简单、条件温和,过程快速简单、低能耗、无污染,所用化学试剂廉价易得,易产业化。制得的UiO-66-(OH)2/SnO2复合纳米材料,具有高比表面积且结构/功能容易调节且分布有大量官能团,能够在室温下持续、快速吸附室内空气中低浓度甲醛污染物且高效杀菌性能。制得的UiO-66-(OH)2/SnO2复合纳米材料具有长寿命、高净化率的特点,具有良好的实用前景,适用于室内、车内及办公场所等使用,且甲醛去除率可达99.7%、杀菌率达99.9%。
为了更好地理解和实施,下面结合附图详细说明本发明。
附图说明
图1为实施例2中制备的UiO-66-(OH)2/SnO2复合纳米材料的SEM示意图。
图2为实施例5中杀菌前后效果图。
图3为实施例6中杀菌前后效果图。
图4为实施例5和实施例6中杀菌效果的对比柱状图。
具体实施方式
在本说明书中提到或者可能提到的上、下、左、右、前、后、正面、背面、顶部、底部等方位用语是相对于其构造进行定义的,它们是相对的概念。因此,有可能会根据其所处不同位置、不同使用状态而进行相应地变化。所以,也不应当将这些或者其他的方位用语解释为限制性用语。
以下示例性实施例中所描述的实施方式并不代表与本公开相一致的所有实施方式。相反,它们仅是与本公开的一些方面相一致的实施方式的例子。
在本公开使用的术语是仅仅出于描述特定实施例的目的,而非旨在限制本公开。在本公开中所使用的单数形式的“一种”、“所述”和“该”也旨在包括多数形式,除非上下文清楚地表示其他含义。还应当理解,本文中使用的术语“和/或”是指并包含一个或多个相关联的列出项目的任何或所有可能组合。
第一方面,一种新型的光催化空气净化材料的制备方法,包括:
步骤101,取4mol/L的氢氧根碱源置于烧杯中,将4mol/L的锡源溶液加入到烧杯中,搅拌后放入内村,加热,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料。
在一种实施方式中,取50毫升4mol/L氢氧根碱源置于烧杯中,将25毫升4mol/L的锡源溶液加入到烧杯中,搅拌1h后放入内村,在160-200℃下加热12-24h,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料。
可选地,所述氢氧根碱源为NaOH、KOH、氨水中的一种或多种。
可选地,所述锡源包括氧化亚锡、氯化亚锡、四氯化锡中的一种或多种。
步骤102,取SnO2纳米材料、苯二甲酸源和锆源一起溶解在DMF和酸源的混合溶液中,然后加热保持,冷却至室温,用甲醇清洗离心,干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
上述技术方案在一种实施方式中,取SnO2纳米材料10g、2mmol苯二甲酸源和2mmol锆源一起溶解在DMF:酸源=1-3:1的100毫升混合溶液中,然后在110℃下保持4h,冷却至室温,用甲醇清洗离心,在80℃下干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
可选地,所述苯二甲酸源包括2-氨基1,4苯二甲酸、邻苯二甲酸、3-氟邻苯二甲酸、3-氨基苯二甲酸中的一种或多种。
可选地,所述锆源包括ZrCl4、ZrF4、ZrBr4、ZrI4中的一种或多种。
可选地,所述酸源包括碳酸、亚硝酸、醋酸、亚硫酸中的一种或多种。
第二方面,本发明提供一种新型的光催化空气净化材料,由上述新型的光催化空气净化材料的制备方法制备而成。
实施例1
取50毫升4mol/L NaOH置于烧杯中,将25毫升4mol/L的氧化亚锡溶液加入到烧杯中,搅拌1h后放入100ml内村,在180℃下加热24h,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料。
实施例2
取实施例1中SnO2纳米材料10g、2mmol二羟基对苯二甲酸和2mmol ZrCl4一起溶解在DMF:酸源=1:1的100毫升混合溶液中,然后在110℃下保持4h,冷却至室温,用甲醇清洗离心,在80℃下干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
请参阅图1,图1为实施例2中制备的UiO-66-(OH)2/SnO2复合纳米材料的SEM示意图。
由图1可知,UiO-66-(OH)2/SnO2复合纳米材料具有多样的孔尺寸和孔环境,这种多样的孔尺寸和孔环境具备实现空气中ppm级浓度甲醛有害气体的高效捕获性能,以及高效杀菌性能。
并且,UiO-66-(OH)2/SnO2复合纳米材料具有高比表面积且结构/功能容易调节且分布有大量官能团,能够在室温下持续、快速吸附、分解室内空气中低浓度甲醛污染物且高效杀菌性能。
金属有机框架材料(Metal-Organic Frameworks,MOFs)具有比表面积大、性能可调控、紫外可见吸收等优点而广泛应用于吸附、催化科研领域。UiO-66-(OH)2MOFs材料因具有多样的孔尺寸和孔环境,能够实现空气中ppm级浓度甲醛气体的高效捕获,且紫外可见均可吸收,具有持久的光催化杀菌除醛性能,在空气污染的净化等领域展现出良好的应用潜力。
在SnO2纳米材料引入UiO-66-(OH)2MOFs纳米材料,通过将两种材料复合,将材料的光吸收拓展到了可见光范围,光催化过程可产生的活性氧自由基,具有强大杀菌除醛性能。
实施例3除醛性能测试
取实施例1中的SnO2纳米材料,室温除甲醛测试是在25℃下在一个手套箱进行的,将SnO2纳米材料1g喷涂在5*5cm的毛玻璃上,将1ppm浓度甲醛溶液通过移液枪注射在玻璃板上,开风扇,搅拌1min,使舱内空气与释放诳释放的污染物混匀后,关闭风扇,测定污染物浓度值为初始浓度,记作C1。开启制冷片,进行照射玻璃培养皿上,开启美国Interscan便携式4160-2甲醛检测仪,每隔1h记录一次数据,见表1。
表1
通过表1结果分析可知:空白对照时间,甲醛也只下降6%,而SnO2纳米材料除醛率可达84%,说明SnO2纳米材料对甲醛有一定的去除效果。
SnO2纳米材料作为光催化杀菌除醛材料,具有广谱杀菌除醛的特点,且在杀菌过程中仅作为催化剂参与反应,理论上不消耗,具有持久的杀菌除醛性能。但是SnO2纳米材料的禁带隙较宽,只能被占太阳能4%的紫外光所激发,并且半导体载流子复合率高,光量子效率低,限制了SnO2纳米材料的实际应用。
实施例4除醛性能测试
取实施例2中的UiO-66-(OH)2/SnO2复合纳米材料,室温除甲醛测试是在25℃下在一个手套箱进行的,将UiO-66-(OH)2/SnO2复合纳米材料1g喷涂在5*5cm的毛玻璃上,将1ppm浓度甲醛溶液通过移液枪注射在玻璃板上,开风扇,搅拌1min,使舱内空气与释放诳释放的污染物混匀后,关闭风扇,测定污染物浓度值为初始浓度,记作C1。开启制冷片,进行照射玻璃培养皿上,开启美国Interscan便携式4160-2甲醛检测仪,每隔1h记录一次数据,见表2。
表2
通过表2结果分析可知:空白对照时间,甲醛也只下降6%,而UiO-66-(OH)2/SnO2复合纳米材料除醛率高达99.7%,说明UiO-66-(OH)2/SnO2复合纳米材料对甲醛较好的去除效果。
实施例5杀菌性能测试
在含有E.Coli的生理盐水溶液中加入目标光催化杀菌剂(实施例1中的SnO2纳米材料),用无菌枪头吸取100μL大肠杆菌悬浮液(106CFU/mL,ATCC25922)轻轻打在杀菌材料表面,暗反应30分钟吸附平衡后,在可见光下照射1h进行细菌灭杀,依次取样后得菌悬液,将所得菌悬液依次稀释不同倍数,取50uL稀释液涂布在琼脂糖培养基上,继续在恒温培养箱培养24h,恒温培养箱中温度为37℃,培养结束后取出计数。
请参阅图2,图2为实施例5中杀菌前后效果图。其中,左侧图为使用目标光催化杀菌剂(实施例1中的SnO2纳米材料)杀菌前的菌悬液图,右侧为使用使用目标光催化杀菌剂(实施例1中的SnO2纳米材料)杀菌后的菌悬液图。
图2显示,杀菌后菌悬液图中的菌群明显缩小,表明,实施例1中的SnO2纳米材料具有一定的杀菌性能。
实施例6杀菌性能测试
在含有E.Coli的生理盐水溶液中加入目标光催化杀菌剂(实施例2中的UiO-66-(OH)2/SnO2复合纳米材料),用无菌枪头吸取100μL大肠杆菌悬浮液(106CFU/mL,ATCC25922)轻轻打在杀菌材料表面,暗反应30分钟吸附平衡后,在可见光下照射1h进行细菌灭杀,依次取样后得菌悬液,将所得菌悬液依次稀释不同倍数,取50uL稀释液涂布在琼脂糖培养基上,继续在恒温培养箱培养24h,恒温培养箱中温度为37℃,培养结束后取出计数。
请参阅图3,图3为实施例6中杀菌前后效果图。其中,左侧图为使用目标光催化杀菌剂(实施例2中的UiO-66-(OH)2/SnO2复合纳米材料)杀菌前的菌悬液图,右侧为使用使用目标光催化杀菌剂(实施例2中的UiO-66-(OH)2/SnO2复合纳米材料)杀菌后的菌悬液图。
图3显示,杀菌后菌悬液图中的菌群消失,悬液呈澄清状态,表明,实施例2中的UiO-66-(OH)2/SnO2复合纳米材料具有优秀的杀菌性能。
请参阅图4,图4为实施例5和实施例6中杀菌效果的对比柱状图。经菌悬液中的菌群进行检测,实施例1中的SnO2纳米材料杀菌率为85%,实施例2中的UiO-66-(OH)2/SnO2复合纳米材料杀菌率为99.9%。进一步佐证,实施例2中的UiO-66-(OH)2/SnO2复合纳米材料具有优秀的杀菌性能。
相对于现有技术,本发明提供的一种新型的UiO-66-(OH)2/SnO2复合纳米材料光催化空气净化材料的制备方法,其原方法设备简单、条件温和,过程快速简单、低能耗、无污染,所用化学试剂廉价易得,易产业化。制得的UiO-66-(OH)2/SnO2复合纳米材料,具有高比表面积且结构/功能容易调节且分布有大量官能团,能够在室温下持续、快速吸附室内空气中低浓度甲醛污染物且高效杀菌性能。制得的UiO-66-(OH)2/SnO2复合纳米材料具有长寿命、高净化率的特点,具有良好的实用前景,适用于室内、车内及办公场所等使用,且甲醛去除率可达99.7%、杀菌率达99.9%。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (9)
1.一种新型的光催化空气净化材料的制备方法,其特征在于,包括:
取4mol/L的氢氧根碱源置于烧杯中,将4mol/L的锡源溶液加入到烧杯中,搅拌后放入内村,加热,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料;
取SnO2纳米材料、苯二甲酸源和锆源一起溶解在DMF和酸源的混合溶液中,然后加热保持,冷却至室温,用甲醇清洗离心,干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
2.根据权利要求1所述的新型的光催化空气净化材料的制备方法,其特征在于:取50毫升4mol/L氢氧根碱源置于烧杯中,将25毫升4mol/L的锡源溶液加入到烧杯中,搅拌1h后放入内村,在160-200℃下加热12-24h,所得沉淀经多次离心洗干燥得白色粉末,即为SnO2纳米材料。
3.根据权利要求2所述的新型的光催化空气净化材料的制备方法,其特征在于:取SnO2纳米材料10g、2mmol苯二甲酸源和2mmol锆源一起溶解在DMF:酸源=1-3:1的100毫升混合溶液中,然后在110℃下保持4h,冷却至室温,用甲醇清洗离心,在80℃下干燥得到UiO-66-(OH)2/SnO2复合纳米材料。
4.根据权利要求1-3任一项所述的新型的光催化空气净化材料的制备方法,其特征在于:所述氢氧根碱源为NaOH、KOH、氨水中的一种或多种。
5.根据权利要求1-3任一项所述的新型的光催化空气净化材料的制备方法,其特征在于:所述锡源包括氧化亚锡、氯化亚锡、四氯化锡中的一种或多种。
6.根据权利要求1-3任一项所述的新型的光催化空气净化材料的制备方法,其特征在于:所述苯二甲酸源包括2-氨基1,4苯二甲酸、邻苯二甲酸、3-氟邻苯二甲酸、3-氨基苯二甲酸中的一种或多种。
7.根据权利要求1-3任一项所述的新型的光催化空气净化材料的制备方法,其特征在于:所述锆源包括ZrCl4、ZrF4、ZrBr4、ZrI4中的一种或多种。
8.根据权利要求1-3任一项所述的新型的光催化空气净化材料的制备方法,其特征在于:所述酸源包括碳酸、亚硝酸、醋酸、亚硫酸中的一种或多种。
9.一种新型的光催化空气净化材料,其特征在于:由权利要求1-8任一项所述的新型的光催化空气净化材料的制备方法制备而成。
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