CN106378143A - 铁铈复合氧化物催化剂的制备方法 - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- ZGMCLEXFYGHRTK-UHFFFAOYSA-N [Fe].[Ce] Chemical compound [Fe].[Ce] ZGMCLEXFYGHRTK-UHFFFAOYSA-N 0.000 title abstract 4
- 239000000243 solution Substances 0.000 claims abstract description 26
- 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 abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 5
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000001988 toxicity Effects 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 3
- 239000012716 precipitator Substances 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000003546 flue gas Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical class [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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Abstract
本发明公开一种铁铈复合氧化物催化剂的制备方法，包含以下步骤：（1）配制0.7mol/L的硝酸铈硝酸溶液；（2）将相同浓度的硝酸铁和硝酸铈溶液混合，搅拌；（3）以碳酸氢铵和氨水为原料，制得沉淀剂溶液；（4）将步骤（3）得到的沉淀剂溶液滴加到步骤（2）的混合溶液中，搅拌10min，过滤，并用去离子水洗涤至滤液的pH=7，真空干燥，置于马弗炉中在空气氛围下400℃焙烧5h，然后在氮气氛围下300℃焙烧2h，即得到铁铈复合氧化物催化剂。本发明操作简单，制备的催化剂形状呈球形，粒径较小，比表面积大，分散性好，毒性小，脱硝活性高。
Description
技术领域
本发明属于催化剂的制备领域，具体涉及一种铁铈复合氧化物催化剂的制备方法。
背景技术
与燃煤火电厂烟气再燃脱硝相比，选择性催化还原具有脱硝效率高，脱硝后烟气中氮氧化物浓度易满足严格的NOx国家排放标准等优点。
目前，应用在工业上的脱硝技术主要是选择性催化还原法(SCR)，该法主要以NH3为还原剂，选择性地将废气中的氮氧化物还原为N2，而V2O5-WO3(MoO3)/TiO2催化剂为最广泛的工业应用催化剂，但其存在以下几个主要缺点：活性组分钒有剧毒，易对人类和环境造成危害；由于催化剂脱硝窗口窄及温度偏高(300-400℃)，需要将其布置于脱硫塔和除尘器之前；在温度高时,烟气中SO2容易被氧化为SO3，从而将尾部烟道腐蚀。因此，需要开发低反应温度、更高SCR脱硝活性的催化剂。
发明内容
针对现有技术存在的缺陷，本发明提供一种铁铈复合氧化物催化剂的制备方法，操作简单，制备的催化剂分散性好，毒性小，脱硝活性高。
本发明是通过以下技术方案实现的。
铁铈复合氧化物催化剂的制备方法，包含以下步骤：
（1）用硝酸溶解碳酸铈，配制0.7mol/L的硝酸铈溶液；
（2）将相同浓度的硝酸铁和硝酸铈溶液按硝酸铁和硝酸铈的摩尔比为1:9的比例混合，搅拌2h；
（3）按摩尔比1:1称取碳酸氢铵和氨水，溶于二者质量综合4倍的蒸馏水中，制得沉淀剂溶液；
（4）将步骤（3）得到的沉淀剂溶液滴加到步骤（2）的混合溶液中，搅拌10min，过滤，并用去离子水洗涤至滤液的pH=7，真空干燥，置于马弗炉中在空气氛围下400℃焙烧5h，然后在氮气氛围下300℃焙烧2h，即得到铁铈复合氧化物催化剂。
优选地，上述步骤（2）中搅拌的条件为：先在500rpm的转速下搅拌1h，再与2000rpm的转速下搅拌1h。
优选地，上述步骤（4）中，步骤（3）得到的沉淀剂溶液和步骤（2）的混合溶液的质量比为1:4。
优选地，上述步骤（4）中，真空干燥的条件为在105℃下干燥4h。
本发明的优点：
本发明提供一种铁铈复合氧化物催化剂的制备方法，操作简单，制备的催化剂形状呈球形，粒径较小，比表面积大，分散性好，毒性小，脱硝活性高。
具体实施方式
实施例1
铁铈复合氧化物催化剂的制备方法，包含以下步骤：
（1）用硝酸溶解碳酸铈，配制0.7mol/L的硝酸铈溶液；
（2）将相同浓度的硝酸铁和硝酸铈溶液按硝酸铁和硝酸铈的摩尔比为1:9的比例混合，搅拌2h；
（3）按摩尔比1:1称取碳酸氢铵和氨水，溶于二者质量综合4倍的蒸馏水中，制得沉淀剂溶液；
（4）将步骤（3）得到的沉淀剂溶液滴加到步骤（2）的混合溶液中，步骤（3）得到的沉淀剂溶液和步骤（2）的混合溶液的质量比为1:4，搅拌10min，过滤，并用去离子水洗涤至滤液的pH=7，真空干燥，置于马弗炉中在空气氛围下400℃焙烧5h，然后在氮气氛围下300℃焙烧2h，即得到铁铈复合氧化物催化剂。
实施例2
铁铈复合氧化物催化剂的制备方法，包含以下步骤：
（1）用硝酸溶解碳酸铈，配制0.7mol/L的硝酸铈溶液；
（2）将相同浓度的硝酸铁和硝酸铈溶液按硝酸铁和硝酸铈的摩尔比为1:9的比例混合，搅拌2h，搅拌的条件为：先在500rpm的转速下搅拌1h，再与2000 rpm的转速下搅拌1h；
（3）按摩尔比1:1称取碳酸氢铵和氨水，溶于二者质量综合4倍的蒸馏水中，制得沉淀剂溶液；
（4）将步骤（3）得到的沉淀剂溶液滴加到步骤（2）的混合溶液中，步骤（3）得到的沉淀剂溶液和步骤（2）的混合溶液的质量比为1:4，搅拌10min，过滤，并用去离子水洗涤至滤液的pH=7，真空干燥，真空干燥的条件为在105℃下干燥4h，置于马弗炉中在空气氛围下400℃焙烧5h，然后在氮气氛围下300℃焙烧2h，即得到铁铈复合氧化物催化剂。
Claims (4)
1.铁铈复合氧化物催化剂的制备方法，其特征在于：包含以下步骤：
（1）用硝酸溶解碳酸铈，配制0.7mol/L的硝酸铈溶液；
（2）将相同浓度的硝酸铁和硝酸铈溶液按硝酸铁和硝酸铈的摩尔比为1:9的比例混合，搅拌2h；
（3）按摩尔比1:1称取碳酸氢铵和氨水，溶于二者质量综合4倍的蒸馏水中，制得沉淀剂溶液；
（4）将步骤（3）得到的沉淀剂溶液滴加到步骤（2）的混合溶液中，搅拌10min，过滤，并用去离子水洗涤至滤液的pH=7，真空干燥，置于马弗炉中在空气氛围下400℃焙烧5h，然后在氮气氛围下300℃焙烧2h，即得到铁铈复合氧化物催化剂。
2.根据权利要求1所述的铁铈复合氧化物催化剂的制备方法，其特征在于：步骤（2）中搅拌的条件为：先在500rpm的转速下搅拌1h，再与2000 rpm的转速下搅拌1h。
3.根据权利要求1所述的铁铈复合氧化物催化剂的制备方法，其特征在于：步骤（4）中，步骤（3）得到的沉淀剂溶液和步骤（2）的混合溶液的质量比为1:4。
4.根据权利要求1所述的铁铈复合氧化物催化剂的制备方法，其特征在于：步骤（4）中，真空干燥的条件为在105℃下干燥4h。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112495386A (zh) * | 2020-12-07 | 2021-03-16 | 山东公用同太环保科技有限公司 | 一种铈铜铁三元复合氧化物催化剂及制备方法和应用 |
| CN112934217A (zh) * | 2021-02-01 | 2021-06-11 | 河北工业大学 | 一种多级孔道复合金属氧化物及其制备方法和应用 |
| CN113398939A (zh) * | 2021-03-29 | 2021-09-17 | 上海中船临港船舶装备有限公司 | 用于VOCs治理的铁铈复合氧化物催化剂及制备方法 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112495386A (zh) * | 2020-12-07 | 2021-03-16 | 山东公用同太环保科技有限公司 | 一种铈铜铁三元复合氧化物催化剂及制备方法和应用 |
| CN112934217A (zh) * | 2021-02-01 | 2021-06-11 | 河北工业大学 | 一种多级孔道复合金属氧化物及其制备方法和应用 |
| CN112934217B (zh) * | 2021-02-01 | 2022-06-14 | 河北工业大学 | 一种多级孔道复合金属氧化物及其制备方法和应用 |
| CN113398939A (zh) * | 2021-03-29 | 2021-09-17 | 上海中船临港船舶装备有限公司 | 用于VOCs治理的铁铈复合氧化物催化剂及制备方法 |
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Application publication date: 20170208 |