CN115382578A - 一种负载MIL-100(Fe)的活性炭纤维材料的制备方法 - Google Patents
一种负载MIL-100(Fe)的活性炭纤维材料的制备方法 Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000013291 MIL-100 Substances 0.000 title claims abstract description 68
- 239000002657 fibrous material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
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- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 8
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Abstract
本发明涉及功能纤维材料制备技术领域，尤其涉及一种负载MIL‑100(Fe)的活性炭纤维材料的制备方法，具体步骤如下：步骤一、将七水合硫酸亚铁和均苯三甲酸充分混合，并用研钵研磨均匀；步骤二、将所得混合物均匀地涂覆在活性炭纤维表面，用铝箔包裹之后，用平板压烫仪进行热压处理，冷却后去除铝箔；步骤三、将所得的活性炭纤维材料分别用水和乙醇清洗，去除未反应的原料，最后烘干，即可制得负载MIL‑100(Fe)的活性炭纤维材料。本发明采用热压法，在无溶剂、无胶粘剂的条件下，将MIL‑100(Fe)负载在活性炭纤维上。另外，本发明制得的活性炭纤维材料对印染废水中的染料有很好的脱色效果，应用前景广阔。
Description
技术领域
本发明涉及功能纤维材料制备技术领域，尤其涉及一种负载MIL-100(Fe)的活性炭纤维材料的制备方法。
背景技术
活性炭纤维具有较大的比表面积，良好的力学性能，同时耐酸碱，耐高温，导电性和化学稳定性好，常被用作吸附剂或催化剂载体，广泛应用于污水处理。在活性炭纤维上负载TiO2、ZnO、Fe2O3等纳米光催化材料，利用活性炭纤维的导电性可降低纳米光催化材料在光照下所产生的空穴(h+)与光生电子(e-)复合率，提高纳米光催化材料的光催化性能。
金属有机框架(MOFs)材料是一种具有大表面积和可调节的有机连接体或金属簇的多孔材料，广泛应用于光催化、分子吸附和分离以及多孔载体。其中，铁基MOFs的应用最为广泛，因为铁是一种地球丰富的元素，价格低廉。迄今为止，MIL-53(Fe)、MIL-68(Fe)、MIL-100(Fe)、MIL-101(Fe)和MIL-88B(Fe)等几种铁基MOFs，由于它们对可见光的良好响应以及通过类Fenton途径将H2O2活化为羟基自由基(·OH)，成为了光催化领域的热门材料。此外，铁基MOFs具有高度水稳定性和低毒性。但铁基MOFs常用的制备方法为水/溶剂热法，其能耗高，而且有有机溶剂污染的风险，因此需要寻找经济、环保的制备方法。同时铁基MOFs大多数为粉末，用于废水处理存在难以回收的问题。CN108607610B一种可磁回收的Fe-MOF光催化剂的制备方法及其应用，及CN104096542A一种新型磁性Fe/C@MOF复合材料吸附剂及其制备方法，利用材料具有一定的磁性，使材料可以回收重复利用，但必须通过外加磁场来实现分离回收。
发明内容
本发明的目的是为了解决现有技术中存在的缺点，而提出的一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，不同于传统的水/溶剂热制备方法，本发明采用热压法，在无溶剂、无胶粘剂的条件下，将MIL-100(Fe)负载在活性炭纤维上，不但可以赋予活性炭纤维的吸附和光催化性能，还可以解决MIL-100(Fe)在废水处理中难以回收的问题，同时利用活性炭纤维的导电性，可以提高MIL-100(Fe)的光催化性能，制得的活性炭纤维材料对印染废水中的染料有很好的脱色效果，应用前景广阔。
为了实现上述目的，本发明采用了如下技术方案：
一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，具体步骤如下：
步骤一、将七水合硫酸亚铁和均苯三甲酸充分混合，并用研钵研磨均匀，得混合物；
步骤二、将步骤一所得混合物均匀地涂覆在活性炭纤维表面，用铝箔包裹之后，用平板压烫仪进行热压处理，冷却后去除铝箔，得活性炭纤维材料；
步骤三、将步骤二所得的活性炭纤维材料分别用去离子水和乙醇清洗，去除未反应的原料，最后烘干，即可制得负载MIL-100(Fe)的活性炭纤维材料。
优选地，在步骤一中，七水合硫酸亚铁和均苯三甲酸的摩尔比为1:1-2。
优选地，在步骤二中，活性炭纤维为活性炭纤维布或毡。
优选地，在步骤二中，热压温度为150-200℃，时间15-30min。
优选地，在步骤三中，清洗次数为2-3次，烘干温度为80-100℃。
与现有技术相比，本发明具有以下有益效果：
1、本发明采用热压法，在无溶剂、无胶粘剂的条件下，将MIL-100(Fe)负载在活性炭纤维上，制备过程中无有机溶剂污染的风险，更加绿色环保。
2、本发明制备设备简单，操作方便，耗时短。
3、本发明将MIL-100(Fe)负载在活性炭纤维上，不但可以赋予活性炭纤维的吸附和光催化性能，还可以解决MIL-100(Fe)在废水处理中难以回收的问题，同时利用活性炭纤维的导电性，可以提高MIL-100(Fe)的光催化性能。
附图说明
图1为本发明负载MIL-100(Fe)的活性炭纤维毡，作为滤布过滤活性黑KN-B染料溶液的脱色效果图；
图2为本发明负载MIL-100(Fe)的活性炭纤维毡，在1000W氙灯照射下对活性黑KN-B染料溶液的脱色效果图；
图3为本发明实施例1所制得的负载MIL-100(Fe)的活性炭纤维毡的扫描电镜照片。
具体实施方式
下面结合附图将对本发明实施例中的技术方案进行清楚、完整地描述，以使本领域的技术人员能够更好的理解本发明的优点和特征，从而对本发明的保护范围做出更为清楚的界定。本发明所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例，基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1：
参照图1、图2和图3，一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，具体步骤如下：
步骤一、将3mmol的七水合硫酸亚铁和2mmol的均苯三甲酸充分混合，并用研钵研磨均匀，得混合物；
步骤二、将步骤一所得混合物均匀地涂覆在活性炭纤维毡(4cm×10cm)表面，用铝箔包裹之后，用平板压烫仪200℃热压处理15min，冷却后去除铝箔；
步骤三、将步骤二所得的活性炭纤维毡分别用去离子水和乙醇清洗3次，去除未反应的原料，最后烘干，即可制得负载MIL-100(Fe)的活性炭纤维材料。
本实施例结果：在50mL的50mg/L的活性黑KN-B染料溶液，加入0.16mL/L的30％过氧化氢溶液，用制得的负载MIL-100(Fe)活性炭纤维材料和负载MIL-100(Fe)活性炭纤维材料作为滤布，过滤染液，测得其对活性黑KN-B染液的脱色效果如图1所示，可以看出负载MIL-100(Fe)的活性炭纤维毡比未负载MIL-100(Fe)的活性炭纤维毡对活性黑KN-B溶液的脱色率提高了42.5％。
为了考察所制得的负载MIL-100(Fe)的活性炭纤维材料的光催化性能，在50mL的50mg/L的活性黑KN-B染料溶液，加入0.16mL/L的30％过氧化氢溶液，分别加入0.1g负载MIL-100(Fe)活性炭纤维毡和未负载MIL-100(Fe)活性炭纤维毡，用1000W氙灯照射一定时间下，测得染液的脱色率如图2所示，可以看出负载MIL-100(Fe)的活性炭纤维毡比未负载MIL-100(Fe)的活性炭纤维毡对活性黑KN-B染液的脱色率明显提高。光照60min后，负载MIL-100(Fe)的活性炭纤维脱色率达到99％，比为负载的高44.7％，说明负载MIL-100(Fe)的活性碳纤维具有更好的脱色效果。
实施例2：
参照图1和图2，一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，具体步骤如下：
步骤一、将2mmol的七水合硫酸亚铁和2mmol的均苯三甲酸充分混合，并用研钵研磨均匀，得混合物；
步骤二、将步骤一所得混合物均匀地涂覆在活性炭纤维毡(4cm×10cm)表面，用铝箔包裹之后，用平板压烫仪180℃热压处理20min，冷却后去除铝箔；
步骤三、将步骤二所得的活性炭纤维毡分别用去离子水和乙醇清洗2次，去除未反应的原料，最后烘干，即可制得负载MIL-100(Fe)的活性炭纤维材料。
本实施例结果：在50mL的50mg/L的活性黑KN-B染料溶液，加入0.16mL/L的30％过氧化氢溶液，用制得的负载MIL-100(Fe)活性炭纤维材料和负载MIL-100(Fe)活性炭纤维材料作为滤布，过滤染液，测得其对活性黑KN-B染液的脱色效果如图1所示，可以看出负载MIL-100(Fe)的活性炭纤维毡比未负载MIL-100(Fe)的活性炭纤维毡对活性黑KN-B溶液的脱色率提高了40.4％。
为了考察所制得的负载MIL-100(Fe)的活性炭纤维材料的光催化性能，在50mL的50mg/L的活性黑KN-B染料溶液，加入0.16mL/L的30％过氧化氢溶液，分别加入0.1g负载MIL-100(Fe)活性炭纤维毡和未负载MIL-100(Fe)活性炭纤维毡，用1000W氙灯照射一定时间下，测得染液的脱色率如图2所示，可以看出负载MIL-100(Fe)的活性炭纤维毡比未负载MIL-100(Fe)的活性炭纤维毡对活性黑KN-B染液的脱色率明显提高。光照60min后，负载MIL-100(Fe)的活性炭纤维脱色率达到97％，比为负载的高42.4％，说明负载MIL-100(Fe)的活性碳纤维具有更好的脱色效果。
实施例3：
参照图1和图2，一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，具体步骤如下：
步骤一、将1mmol的七水合硫酸亚铁和2mmol的均苯三甲酸充分混合，并用研钵研磨均匀，得混合物；
步骤二、将步骤一所得混合物均匀地涂覆在活性炭纤维毡(4cm×10cm)表面，用铝箔包裹之后，用平板压烫仪150℃热压处理30min，冷却后去除铝箔；
步骤三、将步骤二所得的活性炭纤维毡分别用去离子水和乙醇清洗2次，去除未反应的原料，最后烘干，即可制得负载MIL-100(Fe)的活性炭纤维材料。
本实施例结果：在50mL的50mg/L的活性黑KN-B染料溶液，加入0.16mL/L的30％过氧化氢溶液，用制得的负载MIL-100(Fe)活性炭纤维材料和负载MIL-100(Fe)活性炭纤维材料作为滤布，过滤染液，测得其对活性黑KN-B染液的脱色效果如图1所示，可以看出负载MIL-100(Fe)的活性炭纤维毡比未负载MIL-100(Fe)的活性炭纤维毡对活性黑KN-B溶液的脱色率提高了37.1％。
为了考察所制得的负载MIL-100(Fe)的活性炭纤维材料的光催化性能，在50mL的50mg/L的活性黑KN-B染料溶液，加入0.16mL/L的30％过氧化氢溶液，分别加入0.1g负载MIL-100(Fe)活性炭纤维毡和未负载MIL-100(Fe)活性炭纤维毡，用1000W氙灯照射一定时间下，测得染液的脱色率如图2所示，可以看出负载MIL-100(Fe)的活性炭纤维毡比未负载MIL-100(Fe)的活性炭纤维毡对活性黑KN-B染液的脱色率明显提高。光照60min后，负载MIL-100(Fe)的活性炭纤维脱色率达到96％，比为负载的高41.4％，说明负载MIL-100(Fe)的活性碳纤维具有更好的脱色效果。
综上所述，本发明采用热压法，在无溶剂、无胶粘剂的条件下，将MIL-100(Fe)负载在活性炭纤维上，不但可以赋予活性炭纤维的吸附和光催化性能，还可以解决MIL-100(Fe)在废水处理中难以回收的问题，同时利用活性炭纤维的导电性，可以提高MIL-100(Fe)的光催化性能。该方法制备过程中无有机溶剂污染的风险，更加绿色环保；且制备设备简单，操作方便，耗时短。另外，本发明制得的活性炭纤维材料对印染废水中的染料有很好的脱色效果，应用前景广阔。
本发明中披露的说明和实践，对于本技术领域的普通技术人员来说，都是易于思考和理解的，且在不脱离本发明原理的前提下，还可以做出若干改进和润饰。因此，在不偏离本发明精神的基础上所做的修改或改进，也应视为本发明的保护范围。
Claims (5)
1.一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，其特征在于，具体步骤如下：
步骤一、将七水合硫酸亚铁和均苯三甲酸充分混合，并用研钵研磨均匀，得混合物；
步骤二、将步骤一所得混合物均匀地涂覆在活性炭纤维表面，用铝箔包裹之后，用平板压烫仪进行热压处理，冷却后去除铝箔，得活性炭纤维材料；
步骤三、将步骤二所得的活性炭纤维材料分别用去离子水和乙醇清洗，去除未反应的原料，最后烘干，即可制得负载MIL-100(Fe)的活性炭纤维材料。
2.根据权利要求1所述的一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，其特征在于，在步骤一中，七水合硫酸亚铁和均苯三甲酸的摩尔比为1:1-2。
3.根据权利要求1所述的一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，其特征在于，在步骤二中，活性炭纤维为活性炭纤维布或毡。
4.根据权利要求1所述的一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，其特征在于，在步骤二中，热压温度为150-200℃，时间15-30min。
5.根据权利要求1所述的一种负载MIL-100(Fe)的活性炭纤维材料的制备方法，其特征在于，在步骤三中，清洗次数为2-3次，烘干温度为80-100℃。
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