CN109019535A - 一种应用于cs2吸附的氮化硼的制备方法 - Google Patents

一种应用于cs2吸附的氮化硼的制备方法 Download PDF

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CN109019535A
CN109019535A CN201811206241.6A CN201811206241A CN109019535A CN 109019535 A CN109019535 A CN 109019535A CN 201811206241 A CN201811206241 A CN 201811206241A CN 109019535 A CN109019535 A CN 109019535A
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boron nitride
temperature
absorption
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唐成春
王奕然
刘振亚
冀嘉伟
周正
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Hebei University of Technology
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Abstract

本发明涉及一种应用于CS2吸附的氮化硼的制备方法，该方法的步骤是：第一步、将18.9g三聚氰胺和18.55g硼酸以1:2的摩尔比混合加入到1000mL去离子水中，90℃水浴使之完全溶解后降至80℃并保温6h，随后自然降至室温得到白色絮状物，经抽滤、干燥后得到前驱体M·2B；第二步、将M·2B放入管式炉中，氮气气氛下以5℃/min的升温速率升至600℃，保温4h，随后再升温至900℃，保温4h，得到白色的活性氮化硼粉末。该方法使用两步法低温制备得到活性氮化硼，以该活性氮化硼作为吸附剂对二硫化碳表现出优秀的吸附性能。

Description

一种应用于CS2吸附的氮化硼的制备方法
技术领域
本发明涉及功能材料领域，尤其涉及一种应用于CS2吸附的氮化硼的制备方法。
背景技术
二硫化碳纯品为无色,有折射的流动性液体,具有芳香气味,带甜味与氯仿相似。工业品为黄色液体,具有烂萝卜的难闻气味。易挥发且靠近地面累积,是典型的工业化学毒物。二硫化碳广泛用于冶金、农药、橡胶、粘胶纤维等工业领域。常用作溶解剂及制造粘胶纤维,石蜡,玻璃纸和四氯化碳及石油精制等,工业上用作粮食熏蒸杀虫剂和除草剂。由于其沸点低、挥发性强、毒性大,因此在生产和使用过程中易散发于空气中,对环境和人体造成严重的污染和危害。在工业中，少量甚至微量二硫化碳的存在还会使催化剂中毒，对催化剂的寿命和使用具有极大影响。
二硫化碳气体的处理主要有两种方法口。一种是冷凝法。因为二硫化碳沸点低,只有46.3℃,可以采用冷凝回收.另一种较成熟的方法是吸附分离法，由于工业废气中的二硫化碳在大多数情况下浓度较低,而且其本身又是化纤行业重要的原料,因此适宜于用吸附法来治理回收利用。常用的吸附剂包括活性炭，硅胶等，而活性氮化硼在此方面的应用并没有报导。
发明内容
本发明的目的是，提供一种应用于CS2吸附的氮化硼的制备方法。该方法使用两步法低温制备得到活性氮化硼，以该活性氮化硼作为吸附剂，分别采用静态、动态吸附实验，证明了其对二硫化碳优秀的吸附性能。
为实现上述目的，本发明采用如下的技术方案：
一种应用于CS2吸附的氮化硼的制备方法，该方法的步骤是：
第一步、将18.9g三聚氰胺和18.55g硼酸以1:2的摩尔比混合加入到1000mL去离子水中，90℃水浴使之完全溶解后降至80℃并保温6h，随后自然降至室温得到白色絮状物，经抽滤、干燥后得到前驱体M·2B；
第二步、将M·2B放入管式炉中，氮气气氛下以5℃/min的升温速率升至600℃，保温4h，随后再升温至900℃，保温4h，得到白色的活性氮化硼(p-BN)粉末。
与现有技术相比，本发明的有益效果在于：
本发明方法合成温度更低，与高温合成氮化硼(1500-2000℃)相比，结晶度较低，更有利于作为吸附剂应用于CS2的吸附。
附图说明
附图1为本发明方法制备得到的活性氮化硼的XRD图谱。
附图2为实施例1中活性氮化硼的TEM图像。
附图3为p-BN低温吸附-脱附等温线。
附图4 p-BN孔体积和特征孔径分布曲线。
附图5为实施例1的动态吸附实验的结果图。
附图6为实施例2的静态吸附实验的对比结果图。
具体实施方式
下面结合实施例和附图对本发明做进一步详细的描述，需要说明的是如下实施例仅对本发明进行解释说明，不能限制本发明的保护范围。
本发明应用于CS2吸附的氮化硼的制备方法，该方法的步骤是：
第一步、将18.9g三聚氰胺和18.55g硼酸以1:2的摩尔比混合加入到1000mL去离子水中，90℃水浴使之完全溶解后降至80℃并保温6h，随后自然降至室温得到白色絮状物，经抽滤、干燥后得到前驱体M·2B；
第二步、将M·2B放入管式炉中，氮气气氛下以5℃/min的升温速率升至600℃，保温4h，随后再升温至900℃，保温4h，得到白色的活性氮化硼(p-BN)粉末。
本发明方法合成的p-BN用X射线衍射分析(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)和N2吸附-脱附等表征方法分析其组成和结构。
实施例1
本实施例采用上述方法制备得到的采用活性氮化硼进行动态吸附实验，并用称重法测量吸附前后吸附剂重量差。
取容积为1L的实验瓶，称取1g氮化硼放入其中，留出进气口和出气口，将实验瓶密封完好。通入浓度为500ppm的二硫化碳气体，稀释气为氮气，气体流速100sccm。待达到吸附时间，取出吸附剂称重。进行多次不同时间的吸附实验，得到结果如图5所示。由图5可知，所制得的氮化硼对二硫化碳气体的饱和吸附量516mg/g。
实施例2
本实施例采用上述方法制备得到的采用活性氮化硼采用静态吸附实验，并称重法测量吸附前后吸附剂重量差。取容积1升的实验瓶，将浓度为500ppm的二硫化碳标准使用液加入瓶内，让其在静止状态下充分挥发，吸附时间固定为24h，然后称重法测定吸附前后的质量。
本实施例同时采用商业级氮化硼纳米片(BNNS)和氮化硼纳米球(BNSS)作为吸附剂进行对比静态吸附实验，结果如图6所示。
从图6中可以看出，p-BN的吸附效果最好，远远高于BNNS和BNSS由此可见，p-BN具有优良的吸附性能，在脱除气体中二硫化碳方面具有潜在的应用前景。
由上述实施例可以看出，本发明方法制备得到的活性氮化硼对二硫化碳气体具有优异的吸附性能。此外，本发明方法可在较低温度下制备，制备方法简单易行，适用于大规模工业生产。
本发明未述及之处适用于现有技术。

Claims (1)

1.一种应用于CS2吸附的氮化硼的制备方法，该方法的步骤是：
第一步、将18.9g三聚氰胺和18.55g硼酸以1:2的摩尔比混合加入到1000mL去离子水中，90℃水浴使之完全溶解后降至80℃并保温6h，随后自然降至室温得到白色絮状物，经抽滤、干燥后得到前驱体M·2B；
第二步、将M·2B放入管式炉中，氮气气氛下以5℃/min的升温速率升至600℃，保温4h，随后再升温至900℃，保温4h，得到白色的活性氮化硼粉末。
CN201811206241.6A 2018-10-17 2018-10-17 一种应用于cs2吸附的氮化硼的制备方法 Withdrawn CN109019535A (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110386593A (zh) * 2019-07-04 2019-10-29 北京科技大学 非晶前驱体诱导合成球状氮化硼（bn）纳米粉体的方法
CN110629323A (zh) * 2019-10-14 2019-12-31 河北工业大学 一种有机溶剂辅助合成具有高长径比多孔氮化硼纤维的方法
CN112316567A (zh) * 2020-10-19 2021-02-05 江苏大学 一种纳米纤维过滤薄膜及其制备方法和装置

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110386593A (zh) * 2019-07-04 2019-10-29 北京科技大学 非晶前驱体诱导合成球状氮化硼（bn）纳米粉体的方法
CN110629323A (zh) * 2019-10-14 2019-12-31 河北工业大学 一种有机溶剂辅助合成具有高长径比多孔氮化硼纤维的方法
CN110629323B (zh) * 2019-10-14 2021-11-16 河北工业大学 一种有机溶剂辅助合成具有高长径比多孔氮化硼纤维的方法
CN112316567A (zh) * 2020-10-19 2021-02-05 江苏大学 一种纳米纤维过滤薄膜及其制备方法和装置

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