CN111774052A - 高熔点稀有金属元素修饰氧化铈纳米棒及其制备与应用 - Google Patents
高熔点稀有金属元素修饰氧化铈纳米棒及其制备与应用 Download PDFInfo
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- CN111774052A CN111774052A CN202010566882.3A CN202010566882A CN111774052A CN 111774052 A CN111774052 A CN 111774052A CN 202010566882 A CN202010566882 A CN 202010566882A CN 111774052 A CN111774052 A CN 111774052A
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- Prior art keywords
- cerium oxide
- rare metal
- salt
- cerium
- point rare
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 title abstract description 9
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 55
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 55
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- 239000007789 gas Substances 0.000 claims description 7
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- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 5
- -1 cerium ions Chemical class 0.000 claims description 5
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- 150000002751 molybdenum Chemical class 0.000 claims description 4
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- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 4
- 150000003657 tungsten Chemical class 0.000 claims description 4
- 229930195735 unsaturated hydrocarbon Natural products 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
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- 239000002912 waste gas Substances 0.000 claims description 4
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 3
- MFWFDRBPQDXFRC-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;vanadium Chemical group [V].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O MFWFDRBPQDXFRC-LNTINUHCSA-N 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- XZLABTOOVBNJCD-UHFFFAOYSA-D O.[Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O Chemical group O.[Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XZLABTOOVBNJCD-UHFFFAOYSA-D 0.000 claims description 2
- XFHGGMBZPXFEOU-UHFFFAOYSA-I azanium;niobium(5+);oxalate Chemical compound [NH4+].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XFHGGMBZPXFEOU-UHFFFAOYSA-I 0.000 claims description 2
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- ARVBXAKTGHWMTM-UHFFFAOYSA-N molybdenum;pentane-2,4-dione Chemical group [Mo].CC(=O)CC(C)=O ARVBXAKTGHWMTM-UHFFFAOYSA-N 0.000 claims description 2
- 239000012716 precipitator Substances 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
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- 239000003054 catalyst Substances 0.000 abstract description 67
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 20
- 229910052801 chlorine Inorganic materials 0.000 description 20
- 239000002957 persistent organic pollutant Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
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- 238000005303 weighing Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
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- 229910000510 noble metal Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
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- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
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- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
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- 239000001569 carbon dioxide Substances 0.000 description 3
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- Physics & Mathematics (AREA)
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- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
本发明公开了一种高熔点稀有金属元素修饰氧化铈纳米棒及其制备与应用,属于催化材料技术与应用领域。制备方法为将铈盐溶解得到铈盐溶液,再加入沉淀剂和结构导向剂,然后加热进行晶化,得到氧化铈纳米棒前驱体,洗涤干燥后进行焙烧,得到氧化铈纳米棒,加入高熔点稀有金属元素形成的盐后进行焙烧,得到高熔点稀有金属元素修饰的氧化铈纳米棒。本发明制得的催化剂用于卤代烃催化燃烧时,起燃温度低,完全燃烧温度低。在空速为30000ml·g‑1·h‑1,氯代烃浓度为1000ppm条件下,可在小于350℃时将其完全燃烧。同时,该类催化剂还具备很高的稳定性,在催化燃烧氯苯时,300℃下能保持50小时不失活。本发明中的催化剂制备方法简单易于操作,制备的催化剂活性高、稳定性强。
Description
技术领域
本发明属于催化材料技术与应用领域,更具体地,涉及一种高熔点稀有金属元素修饰氧化铈纳米棒及其制备方法与应用。
背景技术
近年来,我国工业化与城市化的快速发展导致空气污染增加,严重影响了区域和全球气候以及人类身体健康。大气污染问题有大部分是由有机污染物带来的,特别是各种含氯有机污染物,联合国环境项目国际条约中有12个列为首位的持久性的有机污染物都是含氯的有机化合物,这些物质几乎都具有麻醉作用、遗传毒理的“三致”效应(致突变-致癌-致畸),严重危害环境与人类健康。然而产生这些含氯污染物的过程都涉及到我国的国计民生,如制药、石化、化工、纺织印染等行业,他们无法从源头上消除污染物,这就要求采用适当手段来消除这类化合物带来的污染,催化燃烧法作为一种低能耗、适用范围广、高效的消除技术,具有广阔的应用前景。含氯有机化合物大致可以分为芳香烃氯化物,如氯苯、二氯苯;氯代脂肪烃类化合物,如氯乙烯、三氯乙烯等不饱和氯代脂肪烃和二氯甲烷、二氯乙烷等不饱和氯代脂肪烃,其中比较具有代表性的物质为氯苯、二氯乙烷、三氯乙烯。
目前,用于氯代有机污染物催化燃烧消除的催化剂以负载型贵金属(活性组分为Pt、Pd、Rh、Ru等贵金属)、固体酸催化剂和非贵金属氧化物型催化剂。负载贵金属催化剂被誉为工业催化剂的"维他命",对于含氯有机污染物的催化燃烧具有很好的催化性能,但贵金属具有价格昂贵、易氯中毒失活以及容易生成毒性更强的多氯代副产物等缺点。固体酸催化剂主要是指质子型分子筛催化剂,虽然其水热稳定性好,但其反应活性低、易积碳失活加上在消除含氯污染物过程中容易结构坍塌而受到限制使用。非贵金属氧化物催化剂因其相对良好的催化活性以及丰度高、价格低廉,是一类广泛研究的催化剂,但是目前很难运用于工业化。现有技术中采用的钒钛催化剂用于氯代烃的催化燃烧,具有一定的活性,但是因为钒的毒性而受到限制。我国是稀土大国,其中氧化铈用于氯代有机污染物催化燃烧具有很高的初始活性,但极易失活。开发高稳定活性的催化剂仍是目前研究与实际应用的热点。
发明内容
本发明解决了现有技术中氯代烃催化燃烧的催化剂活性受限、稳定性不高以及产生毒性的技术问题,提供一种高效高熔点稀有金属元素修饰氧化铈纳米棒及其制备方法与用于氯代有机污染物催化燃烧的应用。
根据本发明的第一方面,提供了一种高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,包括以下步骤:
(1)将铈盐溶解到有机醇中,得到铈盐溶液;向所述铈盐溶液中加入沉淀剂和结构导向剂,然后加热进行晶化,得到氧化铈纳米棒前驱体;所述沉淀剂用于在晶化过程中使铈离子生成沉淀物,所述结构导向剂用于使该沉淀物定向排列以形成棒状结构;
(2)将步骤(1)得到的氧化铈纳米棒前驱体洗涤干燥后进行焙烧,得到氧化铈纳米棒;
(3)向步骤(2)得到的氧化铈纳米棒中加入高熔点稀有金属元素形成的盐,充分混匀后进行焙烧,得到高熔点稀有金属元素修饰的氧化铈纳米棒。
优选地,步骤(1)中所述加热的温度为140℃~180℃,所述晶化的时间为24~48小时。
优选地,步骤(1)中所述沉淀剂为尿素或六次甲基四氨,所述结构导向剂为苯甲醇或苯乙醇;所述铈盐为水合硝酸铈或醋酸铈;所述有机醇为甲醇、乙醇或异丙醇;所述铈盐溶液中铈盐的浓度为0.05mol/L~0.25mol/L;所述铈盐、沉淀剂和结构导向剂的物质的量之比为1:(2-6):(1-6)。
优选地,步骤(2)中所述焙烧的温度为400℃~550℃,时间为3h~6h;步骤(3)中所述焙烧的温度为400℃~550℃,时间为3h~6h。
优选地,步骤(3)中得到高熔点稀有金属元素修饰的氧化铈纳米棒中稀有金属的质量分数为0.5%~5%。
优选地,步骤(3)中所述高熔点稀有金属元素形成的盐为钨盐、钼盐、钒盐或铌盐;
优选地,所述钨盐为钨酸钠或钨酸铵;所述钼盐为乙酰丙酮钼或钼酸铵;所述钒盐为乙酰丙酮钒或偏钒酸钠;所述铌盐为水合草酸铌或草酸铌铵。
按照本发明的另一方面,提供了任一所述方法制备得到的高熔点稀有金属元素修饰的氧化铈纳米棒。
按照本发明的另一方面,提供了高熔点稀有金属元素修饰的氧化铈纳米棒用于含有卤代烃的废气催化燃烧的应用。
优选地,所述卤代烃为氯代烃;
优选地,所述氯代烃为氯代饱和烃、氯代不饱和烃或氯代芳烃;
优选地,所述氯代饱和烃为二氯乙烷;所述氯代不饱和烃为三氯乙烯;所述氯代芳烃为氯苯。
优选地,所述含有卤代烃的废气中卤代烃的体积占0.05%~5%;所述催化燃烧时的反应压力为0.1Mpa~0.5Mpa,温度为100℃~400℃。
总体而言,通过本发明所构思的以上技术方案与现有技术相比,主要具备以下的技术优点:
(1)本发明采用高熔点稀有金属元素修饰氧化铈纳米棒制备催化剂,本发明中的催化剂对卤代有机污染物催化燃烧具有很高的催化活性和稳定性,本发明中的催化剂用于氯代有机污染物,尤其是氯苯催化燃烧反应时,在高空速低浓度的条件下,起燃温度低,完全转化温度低。
(2)采用本发明的方法,在空气中,在较低的反应温度下,在催化剂的存在下,可长时间稳定地将废气中的含氯有机污染物转化成为二氧化碳、水和氯化氢,催化剂的活性不降低。
(3)本发明提供的催化剂具有制备工艺简单、价格低廉、催化活性高、抗氯中毒能力强、寿命长等特点;技术路线方便实用,可以广泛用于造纸、制药、制革、洗涤中的含氯有机污染物的催化燃烧消除。
(4)在本发明催化剂存在下,采用作为氧化剂的空气带入反应器,使含氯有机污染物在催化剂的作用下完全燃烧,将含氯有机污染物转化成为二氧化碳、水和氯化氢或氯气。完全燃烧尾气可以采用稀碱溶液吸收(氯化氢/氯气等酸性气体被吸收)后放空,排放的气体都是合乎环境要求的产物。
(5)本发明制得的催化剂用于含氯有机污染物,尤其是氯苯催化燃烧时,采用空气作为氧化剂,起燃温度低,完全燃烧温度低。在空速为30000ml·g-1·h-1,氯苯浓度为1000ppm条件下,可在300℃将氯苯完全燃烧。每克所述复合氧化物催化剂每小时催化含有氯代烃的废气为5L~60L。同时,该催化剂还具备很高的稳定性,在300℃下能保持50小时不失活。本发明所述的催化剂制备方法简单易于操作,制备的催化剂活性、稳定性兼具。
(6)本发明高熔点稀有金属元素修饰氧化铈纳米棒制备催化剂,氧化铈纳米棒作为载体,浸渍高熔点稀有金属盐后,经过干燥和煅烧后得到高熔点稀有金属元素修饰的氧化铈纳米棒。本方法制备的氧化铈纳米棒是典型的一维材料,具有丰富的孔结构,较大的比表面积,主要暴露高活性的<110>和<100>晶面且储放氧性能佳。
(7)本发明制备的催化剂以氧化铈纳米棒为催化活性成分、以高熔点稀有金属元素作为助剂,在保持氧化还原性能的同时,促进催化剂的酸性,使其有利于C-Cl键的断裂,促进Cl转移,从而提高催化含氯有机污染物的反应活性。
(8)本发明制备的高熔点稀有金属元素修饰氧化铈纳米棒催化剂,经改性后的催化剂具有合适的氧化还原性能、合适的酸性。高熔点稀有金属的负载量为1wt.%~5wt.%,负载后高熔点稀有金属元素在氧化铈纳米棒上高度分散,有效阻断Cl物种对氧化铈纳米棒的毒害作用,同时保证氧化铈纳米棒优异的氧化还原性能,从而达到比较好的催化效果。
(9)本发明制备得到的高熔点稀有金属元素修饰氧化铈纳米棒,高熔点稀有金属氧化物高度分散在催化剂的表面,在保持氧化铈纳米棒优越性能的同时,能够增加氧化铈纳米棒的酸性,促进催化剂对C-Cl键的断裂,同时促进Cl物种转移,催化剂用于含氯有机污染物的催化燃烧活性与稳定性兼具。
附图说明
图1是本发明氧化铈纳米棒扫描电镜图。
图2是本发明高熔点稀有金属元素铌修饰氧化铈纳米棒后透射电镜图。
图3是本发明所制备的2wt.%Nb-CeO2-R和CeO2-R的XRD图。
图4是本发明高熔点稀有金属元素铌修饰氧化铈纳米棒后用于氯苯催化燃烧效果图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。此外,下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1:称取4.34g的Ce(NO3)3·6H2O溶于100mL的甲醇中,搅拌1小时,随后依次加入1.8g尿素和1.08g苯甲醇,在180℃下晶化24h,待冷却后抽滤、洗涤后在110℃干燥12小时,500℃焙烧4小时,制得氧化铈纳米棒;如图1所示,本发明所制备的氧化铈为明显的棒状结构,一定数量的氧化铈纳米棒团聚在一起。量取0.11g二水合钨酸钠并溶于2mL去离子水中,称取2g的氧化铈纳米棒置于坩埚中,将上述钨酸钠溶液加入氧化铈纳米棒中,用玻璃棒反复搅拌至混合均匀。自然蒸干后放入110℃烘箱过夜烘干,400℃焙烧4小时,制得3wt.%W-CeO2-R(其中CeO2-R为氧化铈纳米棒)催化剂,并测试该催化剂对氯苯的催化作用。
实施例2:按照实施例1同样的方法,制得氧化铈纳米棒;量取0.16g钼酸铵并溶于2mL去离子水中,称取2g的氧化铈纳米棒置于坩埚中,将上述钨酸钠溶液加入氧化铈纳米棒中,用玻璃棒反复搅拌至混合均匀。自然蒸干后放入110℃烘箱过夜烘干,400℃焙烧4小时,制得4wt.%Mo-CeO2-R催化剂,并测试该催化剂对氯苯的催化作用。
实施例3:按照实施例1同样的方法,制得氧化铈纳米棒;量取0.16g偏钒酸钠并溶于2mL去离子水中,称取2g的氧化铈纳米棒置于坩埚中,将上述钨酸钠溶液加入氧化铈纳米棒中,用玻璃棒反复搅拌至混合均匀。自然蒸干后放入110℃烘箱过夜烘干,400℃焙烧4小时,制得2.5wt.%V-CeO2-R催化剂,并测试该催化剂对氯苯的催化作用。
实施例4:按照实施例1同样的方法,制得氧化铈纳米棒;量取0.29g草酸铌溶于2mL去离子水中,称取2g的氧化铈纳米棒置于坩埚中,将上述钨酸钠溶液加入氧化铈纳米棒中,用玻璃棒反复搅拌至混合均匀。自然蒸干后放入110℃烘箱过夜烘干,400℃焙烧4小时,制得2wt.%Nb-CeO2-R催化剂,并测试该催化剂对氯苯的催化作用。如图2所示,高熔点稀有金属元素Nb修饰CeO2-R后,催化剂的形貌没有任何改边,仍然保持原有的棒状结构。图3所示的是CeO2-R和2wt.%Nb-CeO2-R的XRD图,由图可以发现,CeO2-R呈典型的立方萤石结构,用2wt.%Nb修饰后,催化剂保持原来的晶型,没有发现铌氧化物的特征衍射峰,表明铌氧化物高度分散在氧化铈纳米棒的表面。
实施例5:按照实施例4同样的方法,调变草酸铌的含量,制得1wt.%Nb-CeO2-R催化剂,并测试该催化剂对氯苯的催化作用。
实施例6:按照实施例4同样的方法,调变草酸铌的含量,制得3wt.%Nb-CeO2-R催化剂,并测试该催化剂对氯苯的催化作用。
实施例7:按照实施例4同样的方法,调变草酸铌的含量,制得5wt.%Nb-CeO2-R催化剂,并测试该催化剂对氯苯的催化作用。
实施例8
按照实施例4同样的方法,制得2wt.%Nb-CeO2-R催化剂,并测试该催化剂对二氯乙烷的催化作用。
实施例9
按照实施例4同样的方法,制得2wt.%Nb-CeO2-R催化剂,并测试该催化剂对三氯乙烯的催化作用。
实施例10
将实施例4制备得到的催化剂,每克催化剂每小时处理废气量为30L,反应压力为0.1MPa,反应温度维持在300℃,氯苯的浓度为1000ppm,使用空气为氧化性气体,空气为干空气,在实施例4催化剂2wt.%Nb-CeO2-R上,在100小时内氯苯的转化率维持在90%左右,未见催化剂失活,如图4所示。
对比例1
按照实施例1同样的方法,称取4.34g的Ce(NO3)3·6H2O溶于100mL的甲醇中,搅拌1小时,随后依次加入1.8g尿素和1.08g苯甲醇,在180℃下晶化24h,待冷却后抽滤、洗涤后在110℃干燥12小时,500℃焙烧4小时,制得氧化铈纳米棒,制得氧化铈纳米棒催化剂,并测试该催化剂对氯苯的催化作用。
结果分析:
所有实施例催化剂的含氯有机物污染物催化燃烧活性评价在固定床微反应器(内径4mm石英)中进行,催化剂的用量为100mg,温度采用K型热电偶自动控制。含氯有机物污染物采用美国Stoelting公司的100系列KDS100型微量注射泵注射进入汽化室,然后与空气混合进入反应器进行燃烧。总流量采用质量流量计控制,含氯有机物污染物的浓度控制在1000ppm。反应压力为0.1Mpa,含氯有机物污染物的转化率与反应温度的关系见下表,表中T10%、T50%、T90%分别为转化率达到10%、50%、90%时所需的反应温度。主要反应产物为二氧化碳、水、氯化氢和氯气。
本领域的技术人员容易理解,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、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,其特征在于,包括以下步骤:
(1)将铈盐溶解到有机醇中,得到铈盐溶液;向所述铈盐溶液中加入沉淀剂和结构导向剂,然后加热进行晶化,得到氧化铈纳米棒前驱体;所述沉淀剂用于在晶化过程中使铈离子生成沉淀物,所述结构导向剂用于使该沉淀物定向排列以形成棒状结构;
(2)将步骤(1)得到的氧化铈纳米棒前驱体洗涤干燥后进行焙烧,得到氧化铈纳米棒;
(3)向步骤(2)得到的氧化铈纳米棒中加入高熔点稀有金属元素形成的盐,充分混匀后进行焙烧,得到高熔点稀有金属元素修饰的氧化铈纳米棒。
2.如权利要求1所述的高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,其特征在于,步骤(1)中所述加热的温度为140℃~180℃,所述晶化的时间为24~48小时。
3.如权利要求1所述的高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,其特征在于,步骤(1)中所述沉淀剂为尿素或六次甲基四氨,所述结构导向剂为苯甲醇或苯乙醇;所述铈盐为水合硝酸铈或醋酸铈;所述有机醇为甲醇、乙醇或异丙醇;所述铈盐溶液中铈盐的浓度为0.05mol/L~0.25mol/L;所述铈盐、沉淀剂和结构导向剂的物质的量之比为1:(2-6):(1-6)。
4.如权利要求1所述的高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,其特征在于,步骤(2)中所述焙烧的温度为400℃~550℃,时间为3h~6h;步骤(3)中所述焙烧的温度为400℃~550℃,时间为3h~6h。
5.如权利要求1所述的高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,其特征在于,步骤(3)中得到高熔点稀有金属元素修饰的氧化铈纳米棒中稀有金属的质量分数为0.5%~5%。
6.如权利要求1所述的高熔点稀有金属元素修饰氧化铈纳米棒的制备方法,其特征在于,步骤(3)中所述高熔点稀有金属元素形成的盐为钨盐、钼盐、钒盐或铌盐;
优选地,所述钨盐为钨酸钠或钨酸铵;所述钼盐为乙酰丙酮钼或钼酸铵;所述钒盐为乙酰丙酮钒或偏钒酸钠;所述铌盐为水合草酸铌或草酸铌铵。
7.如权利要求1~6任一所述方法制备得到的高熔点稀有金属元素修饰的氧化铈纳米棒。
8.如权利要求7所述的高熔点稀有金属元素修饰的氧化铈纳米棒用于含有卤代烃的废气催化燃烧的应用。
9.如权利要求8所述的应用,其特征在于,所述卤代烃为氯代烃;
优选地,所述氯代烃为氯代饱和烃、氯代不饱和烃或氯代芳烃;
优选地,所述氯代饱和烃为二氯乙烷;所述氯代不饱和烃为三氯乙烯;所述氯代芳烃为氯苯。
10.如权利要求8所述的应用,其特征在于,所述含有卤代烃的废气中卤代烃的体积占0.05%~5%;所述催化燃烧时的反应压力为0.1Mpa~0.5Mpa,温度为100℃~400℃。
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