CN106167400A - 一种高比表面积的纳米多孔陶瓷材料的制备方法及得到的产品和应用 - Google Patents
一种高比表面积的纳米多孔陶瓷材料的制备方法及得到的产品和应用 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 71
- 239000011148 porous material Substances 0.000 claims abstract description 36
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 7
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- 229910001385 heavy metal Inorganic materials 0.000 claims description 21
- 150000002500 ions Chemical class 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001723 curing Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
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- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 17
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- 238000009826 distribution Methods 0.000 description 4
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提出了一种高比表面积的纳米多孔陶瓷材料的制备方法,包括以下步骤:①取5~50W%的纳米氧化铝、50~80W%的气相白碳黑、1~10W%的添加剂、5~50W%的造孔剂混匀,成型;②升温至900~1300℃脱造孔剂,烧结固化,得纳米多孔陶瓷材料,制备成本低,制备的得到的纳米多孔陶瓷材料产品具有高比表面积,机械强度高,为产品的进一步应用提供了更好的基础。
Description
技术领域
本发明涉及多孔材料的制备及应用领域,特别是具有大比表面积的多孔陶瓷材料的制备方法,本发明还涉及大比表面积的多孔陶瓷材料及其应用。
背景技术
多孔材料相对于普通材料而言,它的质量轻、密度比较小、比表面积较大等优异的物理化学性能使它越来越多地被人们所认识和发展。这里所说的多孔材料根据其孔径分布一般分为大孔材料、介孔材料(孔径在2~50nm)和微纳孔材料。通过特定工艺设计出富含纳米孔道结构的多孔材料可以极大地增加材料的比表面积,使材料获得更多的与外界物质发生相互作用的界面,进一步拓宽多孔材料的应用领域。如目前应用较广的活性炭材料、分子筛系列多孔材料等都具有巨大的比表面积,在工业上广泛用来作为吸附材料或者催化剂。但这样的材料作为吸附材料吸附选择性差,吸附后脱附再生困难,作为催化剂因对其结构和性能的进一步设计途径有限而限制了它的应用。
在维持吸附材料巨大比表面积的同时,要赋予多孔材料更广泛的应用,一种有效的途径就是在多孔材料的表面设计特定的化学功能基团,这样的设计人为控制多孔材料对不同物质吸附的选择性,或者人为控制多孔材料作为催化剂对不同反应的催化选择性。然而进行这样的设计需要多孔材料具有合适的孔径尺寸,通常可操作的孔径应大于5nm。介孔材料为这种设计提供了可能。如介孔分子筛经过表面分子设计后,对污水中汞离子的吸附就具有极高的吸附容量。介孔分子筛经过表面分子设计后制成的催化剂具有高的催化活性并可以循环使用。
然而,要推广介孔材料在相关领域的应用出现了问题,主要是该类材料制备成本高、介孔材料本身因孔壁较薄致使其强度较低(如当前的SBA、MCM系列介孔分子筛)。发展制备成本低、机械强度高、孔径分布在介孔尺度的多孔陶瓷材料可以解决上面这两类问题。陶瓷材料另一方面的优点在于其本身具有很强的环境适应性(如耐酸、耐碱、耐高温等),这一方面远优于有机多孔泡沫材料,进一步拓宽了该类材料在工业领域的应用前景。
鉴于多孔陶瓷材料广阔的应用前景,已经发展了一系列的多孔陶瓷制备方法,不同制备方法制备的多孔材料具有不同的孔隙率和微观孔结构。如模板法可以制备出孔隙率25~95%,孔径10um~3mm的多孔陶瓷;添加造孔剂法可以制备出孔隙率20~90%,孔径1um~700um的多孔陶瓷;发泡法可以制备孔隙率40~97%,孔径10um~1.2mm的多孔陶瓷;溶胶-凝胶法可以制备出纳米级孔道结构、大比表面积的硅基多孔陶瓷,但生产效率低、成本较高。太原理工大学马非2012年的博士论文《重金属离子吸附材料的制备及性能研究》描述了一类通过烧结方法获得微米级孔道多孔材料的方法,并用于开展吸附重金属离子的研究。但微米级的孔道结构致使材料的比表面积较低,材料吸附重金属离子的容量较小。
发明内容
本发明提出一种高比表面积的纳米多孔陶瓷材料的制备方法,制备成本低,制备的得到的纳米多孔陶瓷材料产品具有高比表面积,机械强度高,为产品的进一步应用提供了更好的基础。
本发明的技术方案是这样实现的:
一种高比表面积的纳米多孔陶瓷材料的制备方法,包括以下步骤:
①取5~50W%的纳米氧化铝、50~80W%的气相白碳黑、1~10W%的添加剂、5~50W%的造孔剂混匀,成型;
②采用程序升温至900~1300℃脱造孔剂,烧结固化,得纳米多孔陶瓷材料;
优选的,选用的原材料所述纳米氧化铝、所述白碳黑、均为纳米级的颗粒或溶胶,所述造孔剂也为纳米级尺寸均匀的材料,所述添加剂包括粘结剂、助熔剂,如PVA,氧化镁等。
优选的,步骤②中,烧结固化过程使用助溶剂实现均匀、低温烧结,降低烧结成本。
一种高比表面积的纳米多孔陶瓷材料,采用所述高比表面积的纳米多孔陶瓷材料的制备方法制备得到。
进一步,所述高比表面积的纳米多孔陶瓷材料的孔径范围分布在5~100nm,比表面积在20~500m2/g范围。
所述高比表面积的纳米多孔陶瓷材料在重金属离子吸附材料或异相催化材料中的应用。
一种制备重金属离子吸附材料或异相催化材料的方法,采用所述高比表面积的纳米多孔陶瓷材料,并包括步骤:
(1)对所述高比表面积的纳米多孔陶瓷材料进行前期预处理;
(2)然后对所述高比表面积的纳米多孔陶瓷材料进行表面功能化改性,设计成重金属离子吸附材料或异相催化材料。
其中,所述前期预处理为使用0.5~10W%双氧水、0.1~5W%硝酸在50~80℃条件下对所述高比表面积的纳米多孔陶瓷材料进行前期预处理10min~2h,80~150℃烘干。
所述表面功能改性包括:A:将能和重金属离子发生较强配位的有机功能基团密集地接枝在所述高比表面积的纳米多孔陶瓷材料表面,获得重金属离子吸附材料;或B:将能和催化活性金属离子发生较强配位的有机功能基团密集地接枝在所述高比表面积的纳米多孔陶瓷材料表面,发展异相催化材料。
本发明的所述高比表面积的纳米多孔陶瓷材料的制备方法,制备成本低,适于工业推广,同时,制得的高比表面积的纳米多孔陶瓷材料优势明显,具有高比表面积,机械强度高,具有更好的工业应用。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。
图1为本发明高比表面积的纳米多孔陶瓷材料的制备方法以及应用方法流程示意图;
图2为本发明实施例得到的高比表面积的纳米多孔陶瓷材料的孔分布情况;
图3为实施例2中不同氧化镁添加剂加入的孔隙率和比表面积;
图4为产品照片;
图5为产品照片。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
高比表面积的纳米多孔陶瓷材料的制备,步骤如下:
①取35W%的纳米氧化铝、50W%的气相白碳黑、5W%的粘结剂、10W%的造孔剂混匀,成型。
②程序升温至1200℃烧结固化,脱造孔剂,降温得高比表面积的纳米多孔陶瓷材料。高比表面积的纳米多孔陶瓷材料的孔分布情况见图2所示。
实施例2
高比表面积的纳米多孔陶瓷材料的制备方,步骤如下:
①取20W%的纳米氧化铝、65W%的气相白碳黑、4W%的粘结剂、1W%的氧化镁、10W%的造孔剂混匀,成型。
②程序升温至1000℃烧结固化,脱造孔剂,降温得高比表面积的纳米多孔陶瓷材料。不同氧化镁添加剂加入的孔隙率和比表面积见图3所示。
实施例3
高比表面积的纳米多孔陶瓷材料的制备和应用工艺,步骤如下:
①取20W%的铝溶胶、66W%的气相白碳黑、3W%的粘结剂、1W%的烧结助剂、10W%的造孔剂混匀,成型;
②程序升温至1000℃烧结固化,脱造孔剂,降温得纳米多孔陶瓷材料。
③使用2%双氧水、1%硝酸在60℃条件下对高比表面积的纳米多孔陶瓷材料进行前期预处理0.5h,120℃烘干备用。
④对步骤③得到的高比表面积的纳米多孔陶瓷材料经乙醇、KH560、催化剂改性,获得富含巯基的多孔陶瓷材料。经巯基改性的多孔陶球,其表面及陶球内部都呈现不易被水润湿的特性,见图4所示。
⑤将富含巯基的多孔陶瓷材料经氢氧化钠溶液处理,以改善巯基改性多孔陶瓷材料的亲水性特征,即得用于水体、淤泥重金属污染治理的重金属离子吸附材料。
实施例4
高比表面积的纳米多孔陶瓷材料的制备方法和应用,步骤如下:
①取35W%的纳米氧化铝、50W%的气相白碳黑、5W%的添加剂、10W%的造孔剂混匀,成型。
②程序升温至1100℃烧结固化,脱造孔剂,降温得纳米多孔陶瓷材料。
③使用2%双氧水、0.1%硝酸在80℃条件下对纳米多孔陶瓷材料进行前期预处理1h,150℃烘干备用。
④对步骤③得到的纳米多孔陶瓷经乙醇、KH550、催化剂改性,获得富含氨基的多孔陶瓷材料,即得重金属离子吸附材料。
实施例5
一种具有高比表面积的纳米多孔陶瓷材料的制备方法及其应用,步骤如下:
①取实施例3所得重金属离子吸附材料吸附含汞污水中的重金属离子Hg2+,汞的吸附容量达~50mg/g;
②使用10mol/L的盐酸浸泡①中吸附Hg2+的多孔陶瓷材料,实现重金属离子吸附材料的再生。
实施例6
一种具有高比表面积的纳米多孔陶瓷材料的制备方法及其应用,步骤如下:
①取35W%的纳米氧化铝、50W%的气相白碳黑、5W%的添加剂、10W%的造孔剂混匀,成型;
②程序升温至1000℃烧结固化,脱造孔剂,降温得纳米多孔陶瓷材料;
③使用2%双氧水、0.5%硝酸在80℃条件下对纳米多孔陶瓷材料进行前期预处理2h,120℃烘干备用。
④对步骤③得到的纳米多孔陶瓷经乙醇、KH550、催化剂改性,获得富含氨基的多孔陶瓷材料。
利用表面氨基化学接枝强金属离子配体(如:卡宾类配体),制备异相催化剂。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种高比表面积的纳米多孔陶瓷材料的制备方法,其特征在于,包括以下步骤:
①取5~50W%的纳米氧化铝、50~80W%的气相白碳黑、1~10W%的添加剂、5~50W%的造孔剂混匀,成型;
②升温至900~1300℃脱造孔剂,烧结固化,得纳米多孔陶瓷材料。
2.如权利要求1中所述高比表面积的纳米多孔陶瓷材料的制备方法,其特征在于:选用的原材料所述纳米氧化铝、所述白碳黑、均为纳米级的颗粒或溶胶,所述造孔剂也为纳米级尺寸均匀的材料,所述添加剂包括粘结剂、助熔剂。
3.如权利要求1中所述高比表面积的纳米多孔陶瓷材料的制备方法,其特征在于:步骤②中,烧结固化过程使用助溶剂实现均匀、低温烧结。
4.一种高比表面积的纳米多孔陶瓷材料,其特征在于:采用权利要求1-3中任一所述高比表面积的纳米多孔陶瓷材料的制备方法制备得到。
5.如权利要求4中所述高比表面积的纳米多孔陶瓷材料,其特征在于:所述高比表面积的纳米多孔陶瓷材料的孔径范围分布在5~100nm,比表面积在20~500m2/g范围。
6.如权利要求4或5中所述高比表面积的纳米多孔陶瓷材料在重金属离子吸附材料或异相催化材料中的应用。
7.一种制备重金属离子吸附材料或异相催化材料的方法,其特征在于,采用权利要求4或5中所述高比表面积的纳米多孔陶瓷材料,并包括步骤:
(1)对所述高比表面积的纳米多孔陶瓷材料进行前期预处理;
(2)然后对所述高比表面积的纳米多孔陶瓷材料进行表面功能化改性,设计成重金属离子吸附材料或异相催化材料。
8.如权利要求8中所述制备重金属离子吸附材料或异相催化材料的方法,其特征在于:所述前期预处理为使用0.5~10W%双氧水、0.1~5W%硝酸在50~80℃条件下对所述高比表面积的纳米多孔陶瓷材料进行前期预处理10min~2h,80~150℃烘干。
9.如权利要求8中所述制备重金属离子吸附材料或异相催化材料的方法,其特征在于:表面功能改性包括:A:将能和重金属离子发生较强配位的有机功能基团密集地接枝在所述高比表面积的纳米多孔陶瓷材料表面,获得重金属离子吸附材料;或B:将能和催化活性金属离子发生较强配位的有机功能基团密集地接枝在所述高比表面积的纳米多孔陶瓷材料表面,发展异相催化材料。
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CN110193382A (zh) * | 2019-05-08 | 2019-09-03 | 兰州大学 | 利用凹凸棒制备孔隙度可调的网眼陶瓷催化剂载体的方法 |
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