CN101518728B - 一种整体式高比表面积多孔吸附剂及其制备方法 - Google Patents

一种整体式高比表面积多孔吸附剂及其制备方法 Download PDF

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CN101518728B
CN101518728B CN2009100817806A CN200910081780A CN101518728B CN 101518728 B CN101518728 B CN 101518728B CN 2009100817806 A CN2009100817806 A CN 2009100817806A CN 200910081780 A CN200910081780 A CN 200910081780A CN 101518728 B CN101518728 B CN 101518728B
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何静
安哲
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Beijing University of Chemical Technology
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Abstract

一种整体式高比表面积多孔吸附剂及其制备方法，属于多孔吸附剂技术领域。该吸附剂具有整体式自支撑金属氧化物骨架结构，比表面积高且孔径分布均匀。吸附材料涵盖可由金属硝酸盐经热分解转变而得的金属氧化物，包括Co3O4、In2O3、ZnO、Cr2O3、NiO。方法经由手性硅基材料，模板导向合成整体式自支撑孔状结构吸附材料。优点在于，吸附剂吸附量大，可吸附气体包括氢气、一氧化碳、乙炔等，可吸附溶剂包括酮、醛、醚等，或者作为特种吸附剂吸附大分子极性有机污染物及特定气体分子。

Description

一种整体式高比表面积多孔吸附剂及其制备方法
技术领域
本发明属于多孔吸附剂技术领域，特别涉及一种整体式高比表面积多孔吸附剂及其制备方法，这种吸附剂具有整体式的自支撑结构及高的比表面积。
背景技术
吸附材料是当今科学研究的热点，其应用范围十分广泛，如用于特种气瓶材料的整体填充式吸附剂、能源存储吸附剂、水体及大气净化吸附剂等。目前用作吸附剂的材料主要有硅酸盐材料、分子筛材料、金属骨架材料及孔状结构金属氧化物材料等。
基于特种气瓶材料的整体填充式吸附剂的迫切需求，吸附剂材料的制备主要面临两个巨大挑战。一方面，材料缺乏整体式结构，孔状结构三维有序度差；另一方面，材料的比表面积有待提高，孔径分布不均匀。针对以上两个科学难点，我们提出了一种经由手性硅基材料模板导向合成整体式自支撑孔状结构吸附材料的方法，所得吸附剂材料比表面积较高，孔径分布均匀。
发明内容
本发明的目的在于提供一种整体式高比表面积多孔吸附剂及其制备方法，所得吸附材料比表面积大、孔径分布均匀，同时工艺简单、成本较低。
本发明提供的一种整体式高比表面积多孔吸附剂，该吸附剂具有整体式自支撑金属氧化物骨架结构；该吸附剂具有高比表面积的多孔金属氧化物骨架结构。金属氧化物吸附剂孔径在2～4nm，比表面积在50～200m2/g。
所得吸附剂组成为金属氧化物并涵盖可由金属硝酸盐经热分解转变而得的金属氧化物，包括四氧化三钴(Co3O4)、三氧化二铟(In2O3)、氧化锌(ZnO)、三氧化二铬(Cr2O3)及氧化镍(NiO)。
本发明的整体式多孔吸附剂的制备方法如下：
(1)氧化硅模板的制备
将十六烷基三甲基溴化铵、硅酸钠、均三甲苯、乙酸乙酯、及去离子水按摩尔比0.12～0.50∶0.15～0.50∶0.18～1.0∶0.3～3.0∶1000依次均匀混合，于15-40℃温度条件下晶化10～48小时，分离、洗涤、干燥得到固体粉末。
将浓硝酸、双氧水按摩尔比2.0～4.0∶4.0～6.0与所得固体粉末均匀混合，微波辐射下，分别控制压力1.0～1.5Mpa、温度100～250℃去除十六烷基三甲基溴化铵，分离、洗涤、干燥得到前体硅模板。
(2)整体式吸附剂的制备
将金属硝酸盐溶液与所得前体均匀混合0.5～10小时，所得混合物于50～150℃下预烘干，所得固体于400～600℃中焙烧得到固体粉末。
将2mol/L NaOH溶液与所得固体粉末均匀混合0.5-3.0小时，去除前体硅模板，分离、洗涤、干燥得到吸附剂。
步骤(2)中，所得金属氧化物吸附剂孔径在2～4nm可调，比表面积在50～200m2/g可调。
本发明的整体式吸附剂吸附量大，可吸附气体包括氢气、一氧化碳、乙炔等，可吸附溶剂包括酮、醛、醚等，或者作为特种吸附剂吸附大分子极性有机污染物及特定气体分子。工艺简单、成本较低，可将特种气瓶材料的整体填充式吸附剂进一步推向实用化。
附图说明
图1为整体式自支撑多孔四氧化三钴吸附剂的高分辨透射电镜图。
图2为整体式自支撑多孔三氧化二铟吸附剂的高分辨透射电镜图。
具体实施方式
实施例1
a.将0.002mol十六烷基三甲基溴化铵、0.002mol硅酸钠、0.004mol均三甲苯、0.003mol乙酸乙酯、及150mL去离子水依次均匀混合，置于30℃水浴静置10小时；
b.反应结束后，产物离心，用去离子水洗涤5次，浆液于25℃真空干燥箱干燥得到白色粉末；
c.取0.3334g白色粉末，加入0.023mol浓硝酸，0.034mol双氧水(30％)，混合均匀，微波照射条件下，分别控制压力和温度不超过1.3Mpa和180℃，反应2min；
d.待温度压力降至常温常压后取出，将反应液离心后弃去上清液，洗涤至pH＝7。浆液于25℃干燥得到手性氧化硅模板；
e.将0.1g手性二氧化硅分散至1mL 0.8mol/mL的硝酸钴溶液中，25℃搅拌0.5小时，所得混合液80℃干燥1小时，所得固体放入瓷坩锅置于马福炉中，从室温加热至450℃，保温7小时，自然降至室温；
f.所得固体置于2mol/L氢氧化钠溶液中，25℃搅拌2小时去除硅基模板，离心洗涤至pH＝7，25℃干燥得整体式自支撑多孔四氧化三钴吸附剂。
实施例2
a.将0.002mol十六烷基三甲基溴化铵、0.002mol硅酸钠、0.004mol均三甲苯、0.003mol乙酸乙酯、及150mL去离子水依次均匀混合，置于30℃水浴静置10小时；
b.反应结束后，产物离心，用去离子水洗涤5次，浆液于25℃真空干燥箱干燥得到白色粉末；
c.取0.3334g白色粉末，加入0.023mol浓硝酸，0.034mol双氧水(30％)，混合均匀，微波照射条件下，分别控制压力和温度不超过1.3Mpa和180℃，反应2min；
d.待温度压力降至常温常压后取出，将反应液离心后弃去上清液，洗涤至pH＝7。浆液于25℃干燥得到手性氧化硅模板；
e.将0.1g手性二氧化硅前体分散至0.8mL 0.8mol/mL的硝酸铟溶液中，25℃搅拌1小时，所得混合液80℃干燥1小时，所得固体放入瓷坩锅置于马福炉中，从室温加热至450℃，保温6小时，自然降至室温；
f.所得固体置于2mol/L氢氧化钠溶液中，25℃搅拌2小时去除硅基模板，离心洗涤至pH＝7，25℃干燥得整体式手性自支撑多孔三氧化二铟吸附剂。
实施例3
将实施例1和实施例2所得整体式手性自支撑多孔四氧化三钴及三氧化二铟吸附剂进行氮气吸脱付实验，其比表面和孔径数据见下表一。
表一 整体式手性自支撑多孔四氧化三钴及三氧化二铟吸附剂孔结构参数

Claims (1)

1.一种整体式高比表面积多孔吸附剂的制备方法，其特征在于，工艺步骤为：
(1)氧化硅模板的制备
将十六烷基三甲基溴化铵、硅酸钠、均三甲苯、乙酸乙酯及去离子水按摩尔比0.12～0.50∶0.15～0.50∶0.18～1.0∶0.3～3.0∶1000依次均匀混合，于15-40℃温度条件下晶化10～48小时，分离、洗涤、干燥得到固体粉末；
将浓硝酸、双氧水按摩尔比2.0～4.0∶4.0～6.0与所得固体粉末均匀混合，微波辐射下，分别控制压力1.0～1.5Mpa、温度100～250℃去除十六烷基三甲基溴化铵，分离、洗涤、干燥得到前体硅模板；
(2)整体式吸附剂的制备
将金属硝酸盐溶液与所得前体均匀混合0.5～10小时，所得混合物于50～150℃下烘干，所得固体于400～600℃焙烧得到固体粉末；
将2mol/LNaOH溶液与所得固体粉末均匀混合0.5-3.0小时，去除前体硅模板，分离、洗涤、干燥，得到吸附剂；
所述的吸附剂具有整体式自支撑金属氧化物骨架结构；组成为金属氧化物并涵盖由金属硝酸盐经热分解转变而得的金属氧化物；金属氧化物吸附剂孔径在2～4nm，比表面积在50～200m2/g。
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