CN110668407A - 一种棒状六方氮化硼泡沫的制备方法及其丙烷氧化脱氢应用 - Google Patents
一种棒状六方氮化硼泡沫的制备方法及其丙烷氧化脱氢应用 Download PDFInfo
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Abstract
本发明公开了一种棒状六方氮化硼泡沫的制备方法及其丙烷氧化脱氢应用,涉及材料科学技术和石油化工领域。本发明提出了一种棒状六方氮化硼泡沫的制备方法,利用了三聚氰胺和硼酸水解聚合反应。干燥的前驱体在氨气中退后之后,生成的六方氮化硼为白色泡沫状固体。这个泡沫由孔孔(约100 nm尺寸)相连的棒状六方氮化硼架构而成。这种孔结构有利于气体的流通和扩散,具有很好的作为多相催化剂的潜力。棒状六方氮化硼泡沫表现了优异的丙烷脱氢性能。本发明方法简单,产率高,有利于大规模的工业生产,具备显著的经济和社会效益。
Description
技术领域
本发明公开了一种棒状六方氮化硼泡沫的制备方法及其丙烷氧化脱氢应用,涉及材料科学技术和石油化工领域。
背景技术
材料的形貌和结构对其性质和应用的影响显著。泡沫材料具有低密度、大比表面积、多孔、较高的负载容量等性质,在隔热、气体传感、能源和催化领域有广泛的应用。最近,六方氮化硼被发现具有优异的短链烷烃氧化脱氢性能。然而,其作为氧化脱氢催化剂时常常是粉末状态,在塞流式反应器中容易造成大的压降,影响反应底物和产物的外扩散,存在催化反应难以控制的现象。因此,在反应前往往需要造粒以降低气阻,这增加了催化剂的制备流程,影响效率。所以,开发一种低气阻的、容易控制反应的六方氮化硼材料作为烷烃氧化脱氢催化剂具有重要意义。
发明内容
本发明的目的在于提供一种简便的、高效率的、低成本的制备六方氮化硼泡沫材料的方法,并将其用于丙烷氧化脱氢反应。本发明利用硼酸和三聚氰胺为原料,制备水凝胶前躯体,在高危焙烧前真空冻干的泡沫前驱体,最终得到了棒状六方氮化硼泡沫材料。将该材料用于丙烷氧化脱氢制丙烯反应,表现了优异的催化性能。该方法操作简便,成本低廉,具有大规模的商品化生产前景,对于其它泡沫材料的制备和应用具有借鉴意义。
为实现上述目的,本发明采用如下技术方案:
一种棒状六方氮化硼泡沫的制备方法,具体包括以下步骤:
具体包括以下步骤:
(1)将三聚氰胺溶于100 mL含硼酸的沸水中,呈无色透明状态,冷却至室温,水溶液凝结成白色的水凝胶;
(2)真空直至冻干白色水凝胶,得到白色泡沫前驱体;
(3)将其置于管式炉中进行高温退火,自然冷却,得到白色泡沫样品。
进一步地,所述三聚氰胺与硼酸的摩尔比1:2。
进一步地,所述真空冻干条件为:-20℃。
进一步地,所述高温退火是在氨气气氛条件下进行的。
进一步地,所述高温退火具体条件为:程序控温,升温速率5 ℃/min,在800℃退火5h。
所述制备方法得到的棒状六方氮化硼泡沫用于催化丙烷脱氢制备丙烯作为反应催化剂。
本发明的有益效果在于:
(1)开发了一种制备棒状六方氮化硼泡沫材料的方法。
(2)得到了优异的丙烷氧化脱氢制备丙烯的性能。
(3)对拓展六方氮化硼泡沫材料具有借鉴意义。
附图说明
图1为棒状六方氮化硼的制备过程示意图。
图2为实例1制备的棒状六方氮化硼泡沫的X射线粉末衍射(XRD)图。
图3为实例1制备的棒状六方氮化硼泡沫的X射线光电子能谱(XPS)。
图4为实例1制备的棒状六方氮化硼泡沫的扫描电镜(SEM)图。
图5中a、b为实例1制备的磷酸硼空心球泡沫材料的TEM图,c图为HRTEM图,d图为HADDF图,e、f图对应于d图位置的B和N的元素分布图。
图6中a为实例1制备的棒状六方氮化硼泡沫催化丙烷脱氢制丙烯的转化率和选择性图,图中b为其和商品化片状六方氮化硼的性能对比图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
本发明制备步骤如下:
将一定量的三聚氰胺加入硼酸的沸水溶液中,溶解透明,自然冷却至室温,出现水凝胶。将水凝胶真空冻干干燥,置于氧化铝坩埚。在氨气气氛下,以5 oC/min升温,到800 oC保温5 h,然后自然冷却,得到白色泡沫样品,即棒状六方氮化硼泡沫材料。
实施例1
硼酸2.47 g溶于100 mL超纯水中,煮沸,将2.50 g三聚氰胺分多次加入,完全溶解至透明,然后自然冷却至室温,析出白色水凝胶。将白色水凝胶真空-20℃直至冻干,转移至坩埚,置于管式炉中。在氨气气氛下,流速80 mL/min,以5℃/min升温,到800℃保温5h,然后自然冷却,得到白色泡沫样品,即棒状六方氮化硼泡沫材料。
取30 mg泡沫材料置于U型管中,两端以石英棉固定。通入反应气(丙烷6 mL/min,氧气3 mL/min,氮气11 mL/min),升高到550℃进行反应,色谱在线分析。(其照片、制备过程示意图如图1所示,晶型结构、组分分别如图2、3所示,扫描电子显微镜图如图4所示、透射电子显微镜如图5所示、丙烷氧化脱氢性能如图6所示)。
本发明制备得到的棒状六方氮化硼泡沫材料的实物图和制备过程示意图如图1所示,白色材料呈泡沫状,很蓬松,能稳稳的置于毛刷上。经XRD表征(图2),位于26.0o和42.7o的衍射峰分别代表的是六方氮化硼的(002)、(101)晶面的特征衍射。XPS表征(图3)中发现,六方氮化硼泡沫中含有B、C、N和O元素,还有部分的C残留在样品中。图4为样品的扫描电镜图,从图可知泡沫材料在微观上呈现棒状结构材料,在棒上还有很多的额尺寸约100 nm的孔存在。TEM图(图5)可以看出这些孔都是相互连通的,这对于催化丙烷氧化脱氢具有促进作用。图6中a为棒状六方氮化硼催化丙烷氧化脱氢制丙烯的活性图,丙烷的转化率约为20~30%之间,丙烯的选择性在65~70%,同时丙烯加上乙烯的转化率为85~90%之间,这体现了良好的丙烷转化率和丙烯选择性。对比商品化的片状氮化硼(图6中b),本发明制备的棒状六方氮化硼具有明显的更好的性能,这与我们制备的棒状六方氮化硼泡沫孔孔相连的特殊结构有关。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (7)
1.一种棒状六方氮化硼泡沫的制备方法,其特征在于:以硼酸和三聚氰胺为原料,利用聚合的硼酸和三聚氰胺前驱体,在高温退火过程中生成多孔棒状六方氮化硼泡沫。
2.根据权利要求1所述的一种棒状六方氮化硼泡沫的制备方法,其特征在于:具体包括以下步骤:
(1)将三聚氰胺溶于100 mL含硼酸的沸水中,呈无色透明状态,冷却至室温,水溶液凝结成白色的水凝胶;
(2)真空直至冻干白色水凝胶,得到白色泡沫前驱体;
(3)将其置于管式炉中进行高温退火,自然冷却,得到白色泡沫样品。
3.根据权利要求2所述的一种棒状六方氮化硼泡沫的制备方法,其特征在于:所述三聚氰胺与硼酸的摩尔比1:2。
4.根据权利要求2所述的一种棒状六方氮化硼泡沫的制备方法,其特征在于:所述真空冻干条件为:-20℃。
5.根据权利要求2所述的一种棒状六方氮化硼泡沫的制备方法,其特征在于:
所述高温退火是在氨气气氛条件下进行的。
6.根据权利要求2所述的一种棒状六方氮化硼泡沫的制备方法,其特征在于:
所述高温退火具体条件为:程序控温,升温速率5 ℃/min,在800℃退火5h。
7.一种如权利要求1~6任一项方法得到的棒状六方氮化硼泡沫在催化丙烷脱氢制备丙烯上的应用。
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