CN108298957A - 一种三维立体纳米材料的制备方法 - Google Patents

一种三维立体纳米材料的制备方法 Download PDF

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CN108298957A
CN108298957A CN201810115392.4A CN201810115392A CN108298957A CN 108298957 A CN108298957 A CN 108298957A CN 201810115392 A CN201810115392 A CN 201810115392A CN 108298957 A CN108298957 A CN 108298957A
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Abstract

本发明公开了一种三维立体纳米材料的制备方法,将三氧化二硼、二氧化钛、硅酸四丁酯、无水乙醇、碳酸氢钠溶液、对苯二胺混合,置于超声反应装置中,调节pH值为4‑6,常温超声10‑20min得分散均匀的混合液A;将混合液A置于密封的反应釜中,控制压力为0.15‑0.20MPa,在120‑140℃下保温反应8‑12h,待反应完毕冷却至室温得到混合胶体;将混合胶体、1‑甲基‑2‑吡咯烷酮、糠醇和柠檬酸三丁酯混合,在温度40‑50℃搅拌至均匀状态;将所得产物放入马弗炉中,以速率1‑3℃/min升温至100‑150℃,保持20‑40min;以速率3‑5℃/min升温至300‑350℃保持1‑3h;以速率1‑3℃/min升温至500‑600℃,保持反应2‑5h,待冷却后即可得到所述三维立体纳米材料。

Description

一种三维立体纳米材料的制备方法
技术领域
本发明属于纳米材料领域,特别涉及一种三维立体纳米材料的制备方法。
背景技术
多孔固体材料由于其孔道结构和大比表面积,在吸附、催化、过滤、离子交换等方面具有广阔的应用前景。人们把孔道尺寸在2nm以下的物质称为微孔材料(microporousmaterials),代表性物质是分子筛;孔道尺寸范围在2~50nm间的材料称为介孔材料(mesoporous materials),代表性物质是M41S系列的中孔分子筛;孔道尺寸范围在50nm以上的物质称为大孔材料(macroporous materials),如阳极化多孔氧化铝模板等。在这类材料的合成中,模板剂需要通过高温氧化去除,而介孔孔道由无定型孔壁构筑而成,因此孔道容易坍塌,同时得到的介孔材料粉末容易在焙烧过程中烧结,因此介孔材料具有较低的热稳定性与水热稳定性,大大地限制其合成与工业应用。如何获得具有高的热稳定性的多孔材料已成为多孔材料研究领域具有挑战性的课题之一。
随着纳米科技的发展,人们开始将多孔材料制成一维纳米结构,这类材料既具有多孔材料的特征又具有一维纳米结构的特征,表现出许多优良的特性。例如,用多孔纳米线制成的气体传感器与相应单晶纳米线制成的气体传感器相比,具有更高的灵敏性,然而现有制备方法中制得的多孔纳米结构都没有经历高温的热处理过程,且多为一维纳米材料,其热稳定性仍然没有得到很好地改善,分散性较差。
发明内容
针对现有技术中传统纳米材料存在的上述不足,本发明的目的是提供一种三维立体纳米材料的制备方法,以提高纳米材料的耐高温性和分散性能,且可有效衰减噪音。
为实现本发明目的技术方案如下:
一种三维立体纳米材料的制备方法,包括如下步骤:
S1:将5-8份三氧化二硼、3-5份二氧化钛、4-8份硅酸四丁酯、15-25份无水乙醇、8-12份碳酸氢钠溶液、3-7份对苯二胺混合,置于超声反应装置中,调节pH值为4-6,常温超声10-20min得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.15-0.20MPa,在120-140℃下保温反应8-12h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、4-9份1-甲基-2-吡咯烷酮、10-20份糠醇和8-15份柠檬酸三丁酯混合,在温度40-50℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率1-3℃/min升温至100-150℃,保持20-40min;以速率3-5℃/min升温至300-350℃保持1-3h;以速率1-3℃/min升温至500-600℃,保持反应2-5h,待冷却后即可得到所述三维立体纳米材料。
优选的,步骤S1中所述将7份三氧化二硼、4份二氧化钛、6份硅酸四丁酯、20份无水乙醇、10份碳酸氢钠溶液、5份对苯二胺混合。
优选的,步骤S1中所述pH值为5.5,超声功率为3500W,超声15min。
优选的,步骤S2中所述控制压力为0.18MPa,在130℃下保温反应10h。
优选的,步骤S3中所述1-甲基-2-吡咯烷酮7份、糠醇15份和柠檬酸三丁酯12份,温度控制为45℃。
优选的,步骤S4中所述以速率2℃/min升温至120℃,保持25min;以速率4℃/min升温至330℃保持1.5h;以速率2℃/min升温至550℃,保持反应3h。
上述任意一条所述制备方法制备得到的三维立体纳米材料。
本发明与现有技术相比,其有益效果为:
本发明所述一种三维立体纳米材料的制备方法,以三氧化二硼、二氧化钛、硅酸四丁酯等成分制成混合胶体,随后与1-甲基-2-吡咯烷酮、糠醇等在马弗炉中经程序升温反应最终得到三维立体状的纳米材料,改善了现有技术中一维纳米材料的不足之处。本发明制备工艺简单,所得到的纳米材料具有良好的耐高温和分散性能,且对于噪声衰减效果显著。
具体实施方式
以下结合实施例对本发明作进一步的说明。
实施例1
S1:将5份三氧化二硼、3份二氧化钛、4份硅酸四丁酯、15份无水乙醇、12份碳酸氢钠溶液、3份对苯二胺混合,置于超声反应装置中,调节pH值为4,常温超声10min,超声功率为3500W,得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.15MPa,在120℃下保温反应8h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、4份1-甲基-2-吡咯烷酮、10份糠醇和8份柠檬酸三丁酯混合,在温度40℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率1℃/min升温至100℃,保持20min;以速率3℃/min升温至300℃保持1h;以速率1℃/min升温至500℃,保持反应2h,待冷却后即可得到所述三维立体纳米材料。
实施例2
S1:将8份三氧化二硼、5份二氧化钛、8份硅酸四丁酯、25份无水乙醇、8份碳酸氢钠溶液、7份对苯二胺混合,置于超声反应装置中,调节pH值为6,常温超声20min,超声功率为3500W,得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.20MPa,在140℃下保温反应12h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、9份1-甲基-2-吡咯烷酮、20份糠醇和15份柠檬酸三丁酯混合,在温度50℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率3℃/min升温至150℃,保持40min;以速率5℃/min升温至350℃保持3h;以速率3℃/min升温至600℃,保持反应5h,待冷却后即可得到所述三维立体纳米材料。
实施例3
S1:将6份三氧化二硼、3份二氧化钛、7份硅酸四丁酯、18份无水乙醇、10份碳酸氢钠溶液、5份对苯二胺混合,置于超声反应装置中,调节pH值为4.5,常温超声12min得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.17MPa,在130℃下保温反应9h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、8份1-甲基-2-吡咯烷酮、17份糠醇和13份柠檬酸三丁酯混合,在温度45℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率2℃/min升温至120℃,保持25min;以速率4℃/min升温至330℃保持1.5h;以速率1℃/min升温至550℃,保持反应3h,待冷却后即可得到所述三维立体纳米材料。
实施例4
S1:将7份三氧化二硼、5份二氧化钛、5份硅酸四丁酯、22份无水乙醇、12份碳酸氢钠溶液、6份对苯二胺混合,置于超声反应装置中,调节pH值为5.5,常温超声18min得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.20MPa,在125℃下保温反应11h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、5份1-甲基-2-吡咯烷酮、14份糠醇和10份柠檬酸三丁酯混合,在温度48℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率3℃/min升温至140℃,保持35min;以速率5℃/min升温至305℃保持2.5h;以速率2℃/min升温至600℃,保持反应4h,待冷却后即可得到所述三维立体纳米材料。
实施例5
S1:将7份三氧化二硼、4份二氧化钛、6份硅酸四丁酯、20份无水乙醇、10份碳酸氢钠溶液、5份对苯二胺混合,置于超声反应装置中,调节pH值为5.5,常温超声15min,超声功率3500W,得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.18MPa,在130℃下保温反应10h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、7份1-甲基-2-吡咯烷酮、15份糠醇和12份柠檬酸三丁酯混合,在温度45℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率2℃/min升温至120℃,保持25min;以速率4℃/min升温至330℃保持1.5h;以速率2℃/min升温至550℃,保持反应3h,待冷却后即可得到所述三维立体纳米材料。
经检测,各个实施例所述三维立体纳米材料的性能如下:
试验 耐高温(℃) 衰减损失(%) 耐冲击强度(MPa)
实施例1 610 48 18
实施例2 625 51 22
实施例3 620 53 20
实施例4 635 52 23
实施例5 650 55 25
本发明不限于这里的实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (7)

1.一种三维立体纳米材料的制备方法,其特征在于,包括如下步骤:
S1:将5-8份三氧化二硼、3-5份二氧化钛、4-8份硅酸四丁酯、15-25份无水乙醇、8-12份碳酸氢钠溶液、3-7份对苯二胺混合,置于超声反应装置中,调节pH值为4-6,常温超声10-20min得分散均匀的混合液A;
S2:将步骤S1中所述混合液A置于密封的反应釜中,控制压力为0.15-0.20MPa,在120-140℃下保温反应8-12h,待反应完毕冷却至室温得到混合胶体;
S3:将步骤S2混合胶体、4-9份1-甲基-2-吡咯烷酮、10-20份糠醇和8-15份柠檬酸三丁酯混合,在温度40-50℃搅拌至均匀状态;
S4:将步骤S3中所得产物放入马弗炉中,以速率1-3℃/min升温至100-150℃,保持20-40min;以速率3-5℃/min升温至300-350℃保持1-3h;以速率1-3℃/min升温至500-600℃,保持反应2-5h,待冷却后即可得到所述三维立体纳米材料。
2.根据权利要求1所述的一种三维立体纳米材料的制备方法,其特征在于,步骤S1中所述将7份三氧化二硼、4份二氧化钛、6份硅酸四丁酯、20份无水乙醇、10份碳酸氢钠溶液、5份对苯二胺混合。
3.根据权利要求1所述的一种三维立体纳米材料的制备方法,其特征在于,步骤S1中所述pH值为5.5,超声功率为3500W,超声15min。
4.根据权利要求1所述的一种三维立体纳米材料的制备方法,其特征在于,步骤S2中所述控制压力为0.18MPa,在130℃下保温反应10h。
5.根据权利要求1所述的一种三维立体纳米材料的制备方法,其特征在于,步骤S3中所述1-甲基-2-吡咯烷酮7份、糠醇15份和柠檬酸三丁酯12份,温度控制为45℃。
6.根据权利要求1所述的一种三维立体纳米材料的制备方法,其特征在于,步骤S4中所述以速率2℃/min升温至120℃,保持25min;以速率4℃/min升温至330℃保持1.5h;以速率2℃/min升温至550℃,保持反应3h。
7.根据权利要求1-6任意一条所述制备方法制备得到的三维立体纳米材料。
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