CN114195106A - 一种高比表面积氮化硼多孔材料的制备方法 - Google Patents
一种高比表面积氮化硼多孔材料的制备方法 Download PDFInfo
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Abstract
本发明为一种引入表面活性剂作为结构导向的方法来制备高比表面积氮化硼多孔材料。详细的制备方法包括以下步骤：在烧杯中放入适量硼酸，氰胺类化合物，加入适量去离子水后进行加热搅拌，待形成硼酸‑氰胺白色加和物后加入一种表面活性剂(聚环氧乙烷‑聚环氧丙烷‑聚环氧乙烷三嵌段共聚物，P123)，待水分蒸发，得到反应前驱体。将前驱体洗涤干燥处理后放入管式炉内进行两阶段煅烧即可得到氮化硼多孔材料。该方法操作简单，无毒无污染，成本较低，可大规模制备出高比表面积的氮化硼多孔材料。该发明引入三嵌段共聚物表面活性剂P123成功活化氮化硼，所得样品比表面积高，孔结构丰富，吸附性能优异，在有机染料吸附等水处理领域有着广阔的应用前景。
Description
技术领域
本发明属于水处理吸附剂制备领域，具体涉及到一种引入表面活性剂作为模板来制备氮化硼多孔材料的方法。
背景技术
氮化硼因为与石墨烯有相似的六方层状结构，又被称作“白色石墨烯”。其具有很多独特的物理和化学性质：出色的化学和热稳定性，高热导率，绝缘性，可用作润滑剂和保护涂层。而人工设计合成的氮化硼多孔材料通常具有较多的孔结构缺陷以及高比表面积，使得氮化硼多孔材料在氢气存储，污染物吸附，以及催化剂载体领域有着很广泛的应用。氮化硼多孔材料内部有着封闭或者互相贯通的孔结构，孔径尺寸可根据实际应用进行调控。孔径的分布情况，比表面积的高低，孔容积的大小，缺陷的多少，以及表面官能团都对于氮化硼多孔材料的性能有着较大的影响。
氮化硼的制备方法主要有机械剥离法、气体剥离法、软硬模板法、高温热分解法、溶剂热合成法、化学发泡法、元素置换法、化学气相沉积法等等，这些制备方法中往往存在生产成本高，操作繁琐，生产效率低下，模板难以除尽的缺点，这些问题使得在氮化硼的研究过程中难以大规模制备出纯度较高，性能优异且成本低的氮化硼多孔材料。
因此我们需要开发一种成本较低并且可以大模制备氮化硼的方法，使得能够进一步提升氮化硼多孔材料的比表面积以及吸附性能。
发明内容
本发明为氮化硼多孔材料的制备开发一条新的路径。本发明工艺简单，成本较低，可以制备出均匀的纤维带状的多孔结构，并且样品具有极高的比表面积和孔容积，在有机染料吸附实验中，对于亚甲基蓝染料有着较大的吸附值，为氮化硼材料在吸附领域开拓更远的前景。
第一方面，本发明公开了氮化硼多孔材料的制备方法，本发明的技术方案如下：
(1)将一定配比的硼酸作为硼源和氰胺类化合物作为氮源放入烧杯中，再加入适量去离子水后充分加热搅拌一定时间；
(2)待形成白色的硼酸-氰胺加和物后，加入适量的聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物(P123)表面活性剂，继续加热搅拌一定时间；
(3)待水分蒸发完之后得到含有嵌段共聚物的前驱体，进行洗涤干燥处理；
(4)将处理好的前驱体放入管式炉内在氨气气氛下升温至第一阶段温度A，保温一定时间，然后继续升温至第二阶段温度B保温一定时间，即可得到氮化硼多孔材料。
上述步骤(1)中，氮源化合物可以是三聚氰胺、二氰二胺、单氰胺、尿素(优选地，选择三聚氰胺作为氮源)。
上述步骤(1)中，硼酸和氰胺类化合物的硼氮元素的摩尔比范围为1∶(0.1-100)。
上述步骤(1)中，硼氮源原料与P123的质量比范围为1∶(0.01-72)。
上述步骤(4)中，管式炉煅烧时的保护气包括但不仅限于氮气，氩气，氦气，氖气，氨气。优选地，选择氮气和氨气。进一步优选地，选择氨气。
上述步骤(4)中，管式炉内煅烧时升温速率范围为1～100℃/min。
上述步骤(4)中，管式炉第一阶段温度A范围为500℃～800℃，保温时长包括但不仅限于1-72h。
上述步骤(4)中，管式炉第二阶段温度B范围为1100℃～1500℃，保温时长范围为1-48h。
第二方面，本申请实施方式要求保护通过上述任一方法制备出氮化硼多孔材料在吸附剂领域的应用。
本发明方法与现有技术相比，具有以下优势：
1.本发明实施方式所展示的方法，工艺简单易于制备，原料成本低且易获得，无毒无污染，可以大规模制备氮化硼多孔材料。
2.本发明实施方式所展示的制备方法通过P123作为表面活性剂，成功活化氮化硼，有效的增大了其比表面积和增加了其吸附性能。
3.本发明实施方式通过调控两个阶段的煅烧温度和时间以及升温的速率可以得到均匀稳定的介孔分布，有利于其吸附性能的提高。
4.本发明实施方式所展示的制备出的氮化硼多孔材料比表面积高达1101m2/g，总孔容积为0.607cm3/g。
5.本发明实施方式所展示的制备出的氮化硼多孔材料，用于有机染料亚甲基蓝吸附实验，吸附值达到338mg/L，在吸附剂里处于领先地位。
附图说明
图1为本发明方式实施例一得到的氮化硼多孔材料的XRD图。
图2为本发明方式实施例一得到的氮化硼多孔材料的XPS图。
图3为本发明方式实施例一得到的氮化硼多孔材料的SEM图。
图4为本发明方式实施例一得到的氮化硼多孔材料的TEM图。
图5为本发明方式实施例一得到的氮化硼多孔材料的氮气吸附脱附等温线图。
图6为本发明方式实施例一得到的氮化硼多孔材料对亚甲基蓝的吸附等温线图。
具体实施方式
结合具体实施例，对本发明进行详细说明，以下所述为本发明的解释而非限定。
实施例一：
本实施方式实施了利用硼酸作为硼源，三聚氰胺作为氮源，P123作为表面活性剂的方法，具体包括以下步骤：
(1)将4g的硼酸和4g的三聚氰胺放入烧杯内，再倒入150ml的去离子水。
(2)将上述混合物放置在搅拌机上升温至90℃，以300r/min转速搅拌，待形成白色的硼酸-氰胺加和物后，再加入6g的P123继续搅拌。
(3)充分搅拌至一段时间后，待水分蒸发完后即可得到氮化硼前驱体，即混入硼酸-三聚氰胺的嵌段共聚物。
(4)将上述前驱体取出后用去离子水洗涤干净，在80℃下干燥10h。
(5)将处理好的氮化硼前驱体放入管式炉内进行煅烧，第一阶段升温至600℃，升温速率为10℃/min，保温2h。
(6)第一阶段结束后，第二阶段升温至1300℃，升温速率不变，保温6个小时即可得到氮化硼多孔材料。
本实施方式中，通过引入表面活性剂P123的方法制备出的氮化硼多孔材料，其XRD衍射信息如图1所示，26°和43°的两个峰分别代表其(002)和(100)晶面。其XPS如图2所示，样品的主要元素为硼和氮，其中，硼氮原子比为1.26，且样品中含有较多的氧原子，说明样品的羟基化程度较高。其SEM如图3所示，可以看出大体上呈现微米级的纤维带状结构，并且纤维带的大小较为均一。TEM如图4，清晰地显示了纤维带的形貌：整体形状和SEM的观察相似；并且可以观察到在带状结构上分布着孔径大小为10-30nm的介孔。通过BET法和QSDFT法计算得到样品的比表面积高达1101m2/g，总孔容积为0.607cm3/g，N2的吸附脱附曲线如图5所示，对亚甲基蓝的吸附等温线用朗缪尔模型拟合后如图6，R2超过了0.99，对于亚甲基蓝的最大吸附值为338mg/L，在吸附剂领域处于领先地位。
实施例二：
将实施例一步骤(1)中4g的硼酸改为8g的硼酸，其他各项操作步骤与实施例一相同，所得到的氮化硼多孔材料的比表面积为501m2/g，总孔容积为0.348cm3/g。
实施例三：
将实施例一步骤(1)中三聚氰胺换成二氰二胺，其他各项操作步骤与实施例一相同，所得到的氮化硼多孔的比表面积为1086m2/g，总孔容积为0.561cm3/g。
实施例四：
将实施例一步骤(5)中管式炉内的升温速率改为20℃/min，其他各项操作步骤与实施例一相同，所得到的氮化硼多孔材料的比表面积为925m2/g，总孔容积为0.513cm3/g。
实施例五：
将实施例一步骤(5)中在管式炉内第一阶段升至的温度改为500℃，其他各项操作步骤与实施例一相同，所得到的氮化硼多孔材料的比表面积为976m2/g，总孔容积为0.504cm3/g。
实施例六：
将实施例一步骤(6)中在管式炉内第二阶段升至的温度改为1200℃，其他各项操作步骤与实施例一相同，所得到的氮化硼多孔材料的比表面积为904m2/g，总孔容积为0.463cm3/g。
Claims (8)
1.本发明为一种高比表面积氮化硼多孔材料的制备方法，其特征在于，该方法包括以下步骤：
(1)将一定配比的硼酸作为硼源和氰胺类化合物作为氮源放入烧杯中，再加入适量去离子水后充分加热搅拌一定时间；
(2)待形成白色的硼酸-氰胺加和物后，加入适量的聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物(P123)表面活性剂，继续加热搅拌一定时间；
(3)待水分蒸发完之后得到含有嵌段共聚物的前驱体，进行洗涤干燥处理；
(4)将处理好的前驱体放入管式炉内在氨气气氛下升温至第一阶段温度A，保温一定时间，然后继续升温至第二阶段温度B保温一定时间，便可得到氮化硼多孔材料。
2.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(1)中氮源化合物包括但不仅限于三聚氰胺、二氰二胺、单氰胺、尿素。
3.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(1)中的硼酸和氰胺类化合物的硼氮元素的摩尔比范围为1∶(0.1-100)。
4.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(1)中硼氮源原料与P123的质量比范围为1∶(0.01-72)。
5.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(4)中保护气包括但不仅限于氮气，氩气，氦气，氖气，氨气。
6.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(4)中管式炉内煅烧时升温速率为1～100℃/min。
7.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(4)中管式炉第一阶段温度A为500℃～800℃，第一阶段保温时长为1-72h。
8.根据权利要求1所述的一种高比表面积氮化硼多孔材料的制备方法，其特征在于，所述步骤(4)中管式炉第二阶段温度B为1100℃～1500℃，第二阶段保温时长为1-48h。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204481A (zh) * | 2013-04-17 | 2013-07-17 | 河北工业大学 | 一种用于水处理的活性氮化硼的合成方法 |
| CN109133942A (zh) * | 2018-09-17 | 2019-01-04 | 河北工业大学 | 一种高比表面积的活性氮化硼纤维的制备方法 |
| CN113860272A (zh) * | 2021-11-25 | 2021-12-31 | 南京大学 | 一种富介孔的六方氮化硼多孔材料的制备方法 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204481A (zh) * | 2013-04-17 | 2013-07-17 | 河北工业大学 | 一种用于水处理的活性氮化硼的合成方法 |
| CN109133942A (zh) * | 2018-09-17 | 2019-01-04 | 河北工业大学 | 一种高比表面积的活性氮化硼纤维的制备方法 |
| CN113860272A (zh) * | 2021-11-25 | 2021-12-31 | 南京大学 | 一种富介孔的六方氮化硼多孔材料的制备方法 |
Non-Patent Citations (3)
| Title |
|---|
| LI,J,ET AL: "Activated boron nitride as an effective adsorbent for metal ions and organic pollutants", 《SCIENTIFIC REPORTS》 * |
| WANG ,JM, ET AL: "Porous Boron Carbon Nitride Nanosheets as Efficient Metal-Free Catalysts for the Oxygen Reduction Reactions in Both Alkaline and Acidic Solutions", 《ACS ENERGY LETTERS》 * |
| 王学斌等: "发泡法制备二维材料泡沫体的进展", 《无机材料学报》 * |
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