CN108744599A - 碘掺杂碳酸氧铋包覆的碳布材料及其制备方法与在油水分离中的应用 - Google Patents
碘掺杂碳酸氧铋包覆的碳布材料及其制备方法与在油水分离中的应用 Download PDFInfo
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- 239000004744 fabric Substances 0.000 title claims abstract description 65
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title claims abstract description 45
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- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
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- ANERHPOLUMFRDC-UHFFFAOYSA-K bismuth citrate Chemical class [Bi+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O ANERHPOLUMFRDC-UHFFFAOYSA-K 0.000 description 1
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- B01D39/086—Filter cloth, i.e. woven, knitted or interlaced material of inorganic material
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract
本发明公开了碘掺杂碳酸氧铋包覆的碳布材料及其制备方法与在油水分离中的应用，包括以下步骤，将预处理的碳布浸没在碘掺杂碳酸氧铋前驱体溶液中，水热反应，得到碘掺杂碳酸氧铋包覆的碳布材料；所述柠檬酸铋溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇。本发明通过水热法一步合成了碘掺杂碳酸氧铋包覆的碳布，具有分离乳液的功能。这种材料制备简单，原材料易得，分离效果好，循环性好，在工业污水处理和乳液分离方面具有良好的应用前景。
Description
技术领域
本发明属于功能材料技术领域，具体涉及到一种碘掺杂的碳酸氧铋包覆的碳布作为油水分离材料的制备方法与应用。
背景技术
水和油是人们赖以生存的宝贵资源，然而大量的油排入水中从而形成油水乳液，不仅造成水资源的污染同时造成宝贵的油资源浪费。近年来，碳布的应用越来越广泛。碳布具有优良的化学稳定性、耐腐蚀性、密封性、高润滑不粘性、电绝缘性和良好的抗老化耐力，但受其润湿性的限制，无法应用于实际的油水乳液分离。因此，对碳布进行合适的修饰，能使其满足分离油水乳液的要求。
发明内容
本发明的目的是提供一种碳酸氧铋包覆的碳材料的制备方法，通过水热法在碳布表面生长大量的纳米碳酸氧铋，从而制备出多功能性的复合材料，能有效分离油水乳液，可重复使用性好，可再重复性好，最主要的是产品可工业化生产，以达到治理水污染的目的。
为了达到上述目的，本发明具体技术方案如下：
碘掺杂碳酸氧铋包覆的碳布材料的制备方法，包括以下步骤，将预处理的碳布浸没在碘掺杂碳酸氧铋前驱体溶液中，水热反应，得到碘掺杂碳酸氧铋包覆的碳布材料；所述柠檬酸铋溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇。
本发明还公开了一种碘掺杂碳酸氧铋前驱体溶液，溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇。
本发明还公开了一种油水分离的方法，包括以下步骤：
（1）将预处理的碳布浸没在碘掺杂碳酸氧铋前驱体溶液中，水热反应，得到碘掺杂碳酸氧铋包覆的碳布材料；所述柠檬酸铋溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇；
（2）将待分离油水导入碘掺杂碳酸氧铋包覆的碳布材料中，完成油水分离。
上述技术方案中，室温下，在水中溶解碳酸钠粉末，再加入乙二醇，搅拌后加入柠檬酸铋粉末，搅拌至溶液呈无色透明后再加入碘化钠粉末，得到碘掺杂碳酸氧铋前驱体溶液。
优选的，柠檬酸铋、碳酸钠、碘化钠、乙二醇的质量比为5：(1.3～1.35)：3.5： (27～28)。
上述技术方案中，水热反应为在180 ℃下反应24 h，在此温度下，柠檬酸铋会发生分解，并与碳酸钠反应生成碳酸氧铋，片状的纳米碳酸氧铋生长在碳布表面。
上述技术方案中，碳布分别用丙酮、乙醇和去离子水超声清洗，再浸泡在浓硝酸中，得到预处理的碳布。硝酸活化的碳布表面产生羧基等基团，能增强碳布的反应活性，使其更易生长晶体。
上述技术方案中，水热反应进行两次，二次水热反应的条件相同，目的是使碳酸氧铋生长更完全，所得的产物具有更好的分离性能。
本发明碘掺杂碳酸氧铋包覆的碳布材料的制备方法，包括以下步骤：
（1）以柠檬酸铋为前驱体，配置一定量的碘掺杂碳酸氧铋前驱体溶液；
（2）将预处理的碳布浸没在溶液中，在反应釜中进行水热反应，反应重复两次，最后得到碘掺杂碳酸氧铋包覆的碳布材料，用于油水分离材料。
本发明还公开了根据上述制备方法制备的碘掺杂碳酸氧铋包覆的碳布材料；碘掺杂碳酸氧铋前驱体溶液或者上述碘掺杂碳酸氧铋包覆的碳布材料在油水分离中的应用。
本发明中，碳酸氧铋作为半导体光催化剂，首次在油水乳液分离领域应用，可以用于降解各种有机污染物，并具有优异的性能，且碳酸氧铋结晶的水热制备中，不同条件下的形成过程和结构不同。
本发明通过水热法一步合成了碘掺杂碳酸氧铋包覆的碳布，具有分离乳液的功能。这种材料制备简单，原材料易得，分离效果好，循环性好，在工业污水处理和乳液分离方面具有良好的应用前景。
附图说明
图1为修饰前和修饰后的碳布扫描电镜图；
图2为修饰后的碳布的润湿性侧视图；
图3为修饰后的碳布的油水乳液分离效果图；
图4为修饰后的碳布的循环测试效果图；
图5为修饰后的碳布的循环测试流量图。
具体实施方式
实施例一
碘掺杂碳酸氧铋前驱体溶液的制备，具体步骤如下：
室温下，在100毫升水中溶解1.325克碳酸钠粉末，再加入 25毫升乙二醇，搅拌20分钟；向上述溶液中加入5克柠檬酸铋，继续搅拌至溶液无色透明，最后加入3.5克碘化钠，搅拌20分钟，得到碘掺杂碳酸氧铋前驱体溶液。
碳布分别用丙酮、乙醇和去离子水超声清洗，再浸泡在浓硝酸中6小时，得到预处理的碳布，SEM图见图1。
水热法的具体操作步骤如下：
将预处理的碳布浸没在碘掺杂碳酸氧铋前驱体溶液中，然后将碘掺杂碳酸氧铋前驱体溶液和碳布转移至150 毫升的不锈钢反应釜中，在180 ℃下反应24小时，反应完后去除碳布用乙醇和去离子水清洗产物两次，之后将碳布再次放入反应釜进行二次反应，为在180℃下反应24小时，反应完后去除碳布用乙醇和去离子水清洗产物两次，得到碘掺杂碳酸氧铋包覆的碳布材料，SEM图见图1。
附图1为修饰前和修饰后的碳布的SEM图，（a）图为修饰前的碳布SEM图，（b）、（c）、（d）图为不同分辨率下的产物SEM图，由图可看出碳布上均匀负载了大量的碘掺杂的碳酸氧铋纳米片。
实施例二
碘掺杂碳酸氧铋修饰的碳布的润湿性测试
附图2为碘掺杂碳酸氧铋包覆的碳布材料在空气中呈现超亲水性，当水滴和油滴接触到碳布表面后，迅速铺展开，接触角为0°。而把碳布浸没在水下时，氯仿在碳布表面聚集成球状，接触角为154°；当碳布置于甲苯中时，水滴同样在表面聚集成球状，接触角为153°。结果表明修饰的碳布具备油水分离所需的润湿性要求，其中，（a）图为水在空气中的接触角，（b）图为甲苯在空气中的接触角，（c）图为甲苯在水下的接触角，（d）图为氯仿在水下的接触角。
实施例三
乳液分离测试，具体步骤如下：
将10毫升甲苯加入到90毫升水中，然后再加入50毫克十二烷基硫酸钠，搅拌2小时，之后使用配制好的乳液进行乳液分离测试。
取碘掺杂碳酸氧铋包覆的碳布材料装入玻璃过滤器中，然后倒入100毫升油水乳液，附图3为油水乳液分离步骤以及效果图，从图上可以看出，将乳白色的油水乳液倒入夹有修饰的碳布的玻璃过滤器后，澄清的水流入玻璃滤瓶中，说明其具有良好的乳液分离效果。
实施例四
分离效率和流量的测试，具体步骤如下：
分离效率和渗透通量：使用以下等式计算油/水乳液的分离效率：
R（％）=（1-Cp / Co）×100％
其中R（％）是排油系数，Cp和Co分别是收集的水和油/水乳液的油浓度。纯化水通过紫外可见分光光度法进行分析。通过根据以下等式计算单位时间内的渗透量来确定乳剂的通量：
Flux = V / At
其中A（cm2）是膜的有效过滤表面，V（L / m2h）是渗透物的体积，t（h）是分离时间。每次试验中倒入等量的油水乳液。
图4和图5为材料对水包甲苯和水包己烷两种乳液的循环分离效果和流量图，可以发现材料在经过多次的循环测试之后依旧保持良好的分离效果。
总结
通过以上分析，本发明通过水热法一步合成了碘掺杂碳酸氧铋包覆的碳布，具有分离乳液的功能，如果仅仅采用预处理的碳布无法有效分离，分离效率不到50%，如果不加入碘化钠，分离效率较低，大约62%。本发明材料制备简单，原材料易得，分离效果好，循环性好，在工业污水处理和乳液分离方面具有良好的应用前景。
Claims (10)
1.一种碘掺杂碳酸氧铋包覆的碳布材料的制备方法，包括以下步骤，将预处理的碳布浸没在碘掺杂碳酸氧铋前驱体溶液中，水热反应，得到碘掺杂碳酸氧铋包覆的碳布材料；所述柠檬酸铋溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇。
2.一种油水分离的方法，包括以下步骤：
（1）将预处理的碳布浸没在碘掺杂碳酸氧铋前驱体溶液中，水热反应，得到碘掺杂碳酸氧铋包覆的碳布材料；所述柠檬酸铋溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇；
（2）将待分离油水导入碘掺杂碳酸氧铋包覆的碳布材料中，完成油水分离。
3.根据权利要求1或者2所述的方法，其特征在于，室温下，在水中溶解碳酸钠粉末，再加入乙二醇，搅拌后加入柠檬酸铋粉末，搅拌至溶液呈无色透明后再加入碘化钠粉末，得到碘掺杂碳酸氧铋前驱体溶液。
4.根据权利要求1或者2所述的方法，其特征在于，水热反应为在180 ℃下反应24 h。
5.根据权利要求1或者2所述的方法，其特征在于，碳布分别用丙酮、乙醇和去离子水超声清洗，再浸泡在浓硝酸中，得到预处理的碳布。
6.根据权利要求1或者2所述的方法，其特征在于，水热反应进行两次，二次水热反应的条件相同。
7.根据权利要求1所述的方法制备的碘掺杂碳酸氧铋包覆的碳布材料。
8.碘掺杂碳酸氧铋前驱体溶液，溶液包括柠檬酸铋、碳酸钠、碘化钠、乙二醇。
9.权利要求8所述碘掺杂碳酸氧铋前驱体溶液的制备方法，其特征在于，室温下，在水中溶解碳酸钠粉末，再加入乙二醇，搅拌后加入柠檬酸铋粉末，搅拌至溶液呈无色透明后再加入碘化钠粉末，得到碘掺杂碳酸氧铋前驱体溶液。
10.权利要求8所述碘掺杂碳酸氧铋前驱体溶液或者权利要求7所述碘掺杂碳酸氧铋包覆的碳布材料在油水分离中的应用。
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