CN108311146B - 一种石墨烯/银/二氧化钛/氧化锰复合材料及其制备方法 - Google Patents
一种石墨烯/银/二氧化钛/氧化锰复合材料及其制备方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 79
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 19
- 229910001923 silver oxide Inorganic materials 0.000 title abstract description 12
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- 238000000354 decomposition reaction Methods 0.000 claims abstract description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 229910016978 MnOx Inorganic materials 0.000 claims description 5
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- 229940071125 manganese acetate Drugs 0.000 claims description 4
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- 239000011702 manganese sulphate Substances 0.000 claims description 4
- 235000007079 manganese sulphate Nutrition 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 4
- 229940071536 silver acetate Drugs 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 3
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229960001841 potassium permanganate Drugs 0.000 claims description 3
- 150000003608 titanium Chemical class 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 18
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
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- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种石墨烯/银/二氧化钛/氧化锰复合材料及其制备方法。用于可见光分解挥发性有机化合物与臭氧的石墨烯复合材料,由石墨烯、银、二氧化钛和氧化锰组成,锰与石墨烯的质量比为(0.05~0.2):1,银与石墨烯的质量比为(0.05~0.2):1,钛元素与石墨烯的质量比为(0.05~0.3):1。本发明的石墨烯复合材料具有更高分解有机化合物与臭氧的能力,同时可以实现可见光分解,是一种非常有前景的环境治理方面的材料,可进一步治理室内外的空间环境,并实现环境的改善。
Description
技术领域
本发明属于复合材料制备领域,具体涉及一种应用于可见光分解挥发性有机化合物与臭氧的石墨烯/银/二氧化钛/氧化锰复合材料制备方法。
背景技术
环境中存在大量的挥发性有机化合物(VOC)已经引起人们的广泛关注。甲醛(HCHO)是建筑物装修材料散发到室内空气中的主要污染物之一, 它既是一种致癌物,同时,在很低浓度其就能引发过敏症状的刺激剂。而一氧化氮(NO)、二氧化氮(NO2)和二氧化硫(SO2)等也是主要的室外空气污染物。因此在室内外实现HCHO、NO、NO2、SO2等的分解对人们的健康具有重要的意义。除了上述的一些气体,臭氧(O3)这种具有强氧化性能的物质也逐渐显现了对人们的新危害,研究表明当O3的浓度为0.11ppm时,人呼吸2小时后的肺活量会减少20%;当O3的浓度为1-2 ppm时,人类在该环境中超过2时间后,通常会发生思维紊乱。世界卫生组织制定了的安全标准是:8小时工作环境下允许的最大浓度应低于0.1ppm。鉴于上述的存在的问题,只有采取有效的办法去解决这些室内外存在的气体才能有效的保证人们的身心健康。
目前,在一些研究和商业过程中,通常采用二氧化钛(TiO2)作为HCHO、NO2、NO、SO2以及O3等气体的分解材料,其通常制备为液体或者涂层去实现室内外环境的净化。将其制备成纳米级能更好的TiO2展现其催化能力,不过小尺寸将会使得其出现团聚而降低其催化性能。纳米银(Ag)是另外一种用于HCHO、NO2、NO、SO2、O3等催化降解的物质,不过其在应用过程中同样会出现团聚,而难于满足实际的应用。并且目前在环境应用过程中,更趋向于可见光的条件下进行。
石墨烯是一种具有巨大的比表面积,能有效的抑制负载的材料的团聚,促使材料(如TiO2, Ag)展现更大的性能;同时,石墨烯本身具有很好的吸附能力,有益于更好的吸附空气中的有害物质。如果对TiO2, Ag材料实行掺杂可开发在可见光条件快速HCHO、NO2、NO、SO2、O3等有害气体的材料。因此,在本部分的研究中,探索了一种以石墨烯作为基础材料,通过水热和共沉淀以及光分解的方法制备一种能在可见光条件下实现高效分解环境中有害气体的石墨烯/银/二氧化钛/氧化锰的复合材料。
发明内容
为了克服现有材料的本身存在的单一性能,以及实现制备材料在可见光条件的多功能性,本发明的目的在于提供一种在可见光条件下实现挥发性有机化合物与臭氧分解的石墨烯复合材料及其制备方法,该方法工艺简单、操作容易、生产成本低廉。
为实现上述目的,本发明采用的技术方案如下:
一种用于可见光分解挥发性有机化合物与臭氧的石墨烯复合材料,由石墨烯、银、二氧化钛和氧化锰组成,锰与石墨烯的质量比为(0.05~0.2):1,银与石墨烯的质量比为(0.05~0.2):1,钛元素与石墨烯的质量比为(0.05~0.3):1。
上述石墨烯复合材料的制备方法,包括以下步骤:
1)将石墨烯和锰源在水和乙醇的混合溶液中,然后进行水热反应,将反应物进行分离得到中间体石墨烯/MnOx;2)将上述制备的中间体分散在水溶液中,然后加入银源、钛源和无机碱,然后进行90℃加热反应,后经过分离、干燥和煅烧得到粉末状复合材料;3)经过紫外光照后得到最终的石墨烯复合材料。
在上述石墨烯复合材料的制备方法中,所述步骤1)中石墨烯为氧化石墨烯或直接超声分散的非氧化石墨烯。
在上述石墨烯复合材料的制备方法中,所述步骤1)中的锰源为硫酸锰、醋酸锰、高锰酸钾或者硝酸锰。
在上述石墨烯复合材料的制备方法中,所述步骤2)中的银源为硝酸银、醋酸银或者草酸银。
在上述石墨烯复合材料的制备方法中,所述步骤2)中的钛源为氯钛盐、有机钛盐或者纳米二氧化钛。
在上述石墨烯复合材料的制备方法中,所述步骤2)中的无机碱为氨水、碱金属碳酸盐或者碱金属强碱。
在上述石墨烯复合材料的制备方法中,所述步骤2)中的煅烧需要保护性气氛,保护性气氛为氮气或者氩气。
在上述石墨烯复合材料的制备方法中,所述步骤2)中煅烧的时间为1~8h。
与现有技术相比,本发明具有如下有益效果:
本发明的石墨烯复合材料具有更高分解有机化合物与臭氧的能力,同时可以实现可见光分解,是一种非常有前景的环境治理方面的材料,可进一步治理室内外的空间环境,并实现环境的改善。
本发明采用通过水热法结合共沉淀和光化学实现石墨烯/银/二氧化钛/氧化锰复合材料的制备,该材料可在可见光条件下实现挥发性有机化合物与臭氧的快速分解;本发明的制备方法简单、操作容易、生产成本低廉,有利于人居环境的改善。
附图说明
图1为石墨烯/银/二氧化钛/氧化锰复合材料样品的SEM图。
具体实施方式
下面结合实施例对本发明作进一步说明。
一种应用于可见光分解挥发性有机化合物与臭氧的石墨烯/银/二氧化钛/氧化锰复合材料的制备方法,包括以下步骤:
1)将石墨烯(氧化石墨烯或直接超声分散的非氧化石墨烯)和锰源(硫酸锰、醋酸锰、高锰酸钾或者硝酸锰)在水和乙醇的混合溶液中,然后进行水热反应并分离得到中间体(石墨烯/MnOx)。
2)将上述制备的中间体分散在水溶液中然后加入银源(硝酸银或者醋酸银)、钛源(氯钛盐、有机钛盐或者纳米二氧化钛)和无机碱(氨水、碱金属碳酸盐或者碱金属强碱),然后进行90℃加热反应,然后经过分离和干燥,然后在400~600℃保护气氛下(氮气或氩气)煅烧1~8小时,得到粉末状复合材料;
3)将上述的制备的材料经过紫外光照后得到最终的石墨烯/银/二氧化钛/氧化锰复合材料。
实施例1
一种应用于可见光分解挥发性有机化合物与臭氧的石墨烯复合材料的制备方法,包括以下步骤:
1)按照复合材料中石墨烯与其它反应物的比例中将1g的氧化石墨烯,0.2g的高锰酸钾在水和乙醇的混合溶液中均匀混合,然后进行水热反应,将制备的石墨烯/MnO2进行分离得到中间体。
2)将上述制备的石墨烯/MnO2再次分散在水溶液中,然后加入0.15g硝酸银并搅拌分散,随后加入0.2g的三氯化钛的水溶液,并搅拌均匀,将溶液升温到90℃,随后滴加氢氧化钠溶液(其中氢氧化钠的比反应计算量稍多),控制反应的时间为2小时,然后冷却到室温并经过抽滤,然后在真空干燥箱中80℃干燥12小时,将干燥的粉体进行烧结,在500℃保护性气氛下烧结,烧结时间为2h。
3)将上述烧结的材料进行紫外光分解处理,处理时间为30分钟,然后得到石墨烯/银/二氧化钛/氧化锰复合材料。制备的样品SEM图见图1。
实施例2
一种应用于可见光分解挥发性有机化合物与臭氧的石墨烯复合材料的制备方法,包括以下步骤:
1)按照复合材料中石墨烯与其它反应物的比例中将1g的再膨胀制备的石墨烯,0.1g的硫酸锰在水和乙醇的混合溶液中均匀混合,然后进行水热反应,然后将制备的石墨烯/MnOx进行分离得到中间体。
2)将上述制备的石墨烯/MnOx再次分散在水溶液中,然后加入0.2g硝酸银并搅拌分散,随后加入0.15 g的三氯化钛的水溶液,并搅拌均匀,将溶液升温到85℃,随后滴加氨水(其中氨水的比反应计算量稍微过量),控制反应的时间为2小时,然后冷却到室温并经过抽滤,然后在真空干燥箱中80℃干燥12小时,将干燥的粉体进行烧结,在550℃保护性气氛下烧结,烧结时间为2h。
3)将上述烧结的材料进行紫外光分解处理,处理时间为30分钟,然后得到石墨烯/银/二氧化钛/氧化锰复合材料。
实施例3
一种应用于可见光分解挥发性有机化合物与臭氧的石墨烯复合材料的制备方法,包括以下步骤:
1)按照复合材料中石墨烯与其它反应物的比例中将1g的再膨胀制备的石墨烯,0.12g的醋酸锰在水和乙醇的混合溶液中均匀混合,然后进行水热反应,然后将制备的石墨烯/MnO2进行分离得到中间体。
2)将上述制备的石墨烯/MnO2再次分散在水溶液中,然后加入0.15g醋酸银并搅拌分散,随后加入0.2g的钛酸丁酯的水溶液,并搅拌均匀,将溶液升温到90℃,随后滴加氢氧化钾溶液(其中氢氧化钾的比反应计算量稍多),控制反应的时间为2小时,然后冷却到室温并经过抽滤,然后在真空干燥箱中80℃干燥12小时,将干燥的粉体进行烧结,在450℃保护性气氛下烧结,烧结时间为2h。
3)将上述烧结的材料进行紫外光分解处理,处理时间为60分钟,然后得到石墨烯/银/二氧化钛/氧化锰复合材料。
Claims (8)
1.一种用于可见光分解挥发性有机化合物与臭氧的石墨烯复合材料的制备方法,其特征在于,由石墨烯、银、二氧化钛和氧化锰组成,锰与石墨烯的质量比为(0.05~0.2):1,银与石墨烯的质量比为(0.05~0.2):1,钛元素与石墨烯的质量比为(0.05~0.3):1。
制备方法包括以下步骤:
1)将石墨烯和锰源在水和乙醇的混合溶液中,然后进行水热反应,将反应物进行分离得到中间体石墨烯/MnOx;2)将上述制备的中间体分散在水溶液中,然后加入银源、钛源和无机碱,然后进行90℃加热反应,后经过分离、干燥和煅烧得到粉末状复合材料;3)经过紫外光照后得到最终的石墨烯复合材料。
2.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤1)中石墨烯为氧化石墨烯或直接超声分散的非氧化石墨烯。
3.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤1)中的锰源为硫酸锰、醋酸锰、高锰酸钾或者硝酸锰。
4.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤2)中的银源为硝酸银、醋酸银或者草酸银。
5.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤2)中的钛源为氯钛盐、有机钛盐或者纳米二氧化钛。
6.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤2)中的无机碱为氨水、碱金属碳酸盐或者碱金属强碱。
7.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤2)中的煅烧需要保护性气氛,保护性气氛为氮气或者氩气。
8.根据权利要求1所述的石墨烯复合材料的制备方法,其特征在于,所述步骤2)中煅烧的时间为1~8h。
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