CN112138658B - Preparation method of integral catalyst for purifying tank tail gas - Google Patents
Preparation method of integral catalyst for purifying tank tail gas Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 41
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000919 ceramic Substances 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 33
- 238000000576 coating method Methods 0.000 claims abstract description 33
- WLLURKMCNUGIRG-UHFFFAOYSA-N alumane;cerium Chemical group [AlH3].[Ce] WLLURKMCNUGIRG-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000746 purification Methods 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000013543 active substance Substances 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims abstract description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 45
- 239000010970 precious metal Substances 0.000 claims description 41
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 23
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 21
- 229960000583 acetic acid Drugs 0.000 claims description 16
- 239000012362 glacial acetic acid Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 239000011268 mixed slurry Substances 0.000 claims description 13
- 238000011068 loading method Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 10
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 239000011149 active material Substances 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 7
- 235000006408 oxalic acid Nutrition 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 229910052878 cordierite Inorganic materials 0.000 claims description 5
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical group [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 7
- 239000000779 smoke Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- 239000004071 soot Substances 0.000 description 9
- 229930195733 hydrocarbon Natural products 0.000 description 6
- 150000002430 hydrocarbons Chemical class 0.000 description 6
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 5
- 229910052863 mullite Inorganic materials 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 210000001508 eye Anatomy 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- B01D53/34—Chemical or biological purification of waste gases
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- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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Abstract
Description
技术领域Technical field
本发明涉及坦克尾气净化催化剂技术，具体的说是一种用于坦克尾气净化整体式催化剂的制备方法。The invention relates to tank exhaust gas purification catalyst technology, specifically a preparation method of an integral catalyst for tank exhaust gas purification.
背景技术Background technique
坦克是具有直射火力、越野能力和装甲防护力的履带式装甲战斗车辆，是现代陆上作战的主要武器之一，有“陆战之王”的美称。坦克通常采用大功率柴油机作为动力系统，具备低转速扭矩大，扭矩范围宽，大冷热温差下能正常使用，持续高负荷运转时间长等特点。坦克尾气是一种由多种组分组成的混合物，主要包括烃类化合物(HC)、氮氧化合物(NOx)以及碳烟颗粒物(soot)。其中，NOx会对人体的眼睛、呼吸系统及中枢神经系统等带来永久损害，并且NOx还是形成酸雨的主要原因；HC为燃油不完全燃烧产物，具有毒性、易燃易爆性和致癌作用等特性，并且HC在日照条件下极易与NOx发生光化学反应，是产生光化学烟雾二次污染的罪魁祸首；碳烟颗粒物直径通常为0.01～10微米，在大气中存留时间久、输运距离长，容易造成大范围的污染，此外，碳烟颗粒物还具有很强的致癌效果，其随呼吸进入人体肺部后极易聚集在肺泡等部位，进而导致呼吸系统疾病、心脏疾病甚至导致癌症。Tanks are tracked armored combat vehicles with direct firepower, cross-country capabilities and armor protection. They are one of the main weapons in modern land combat and are known as the "King of Land Warfare". Tanks usually use high-power diesel engines as the power system, which have the characteristics of large low-speed torque, wide torque range, normal use under large hot and cold temperature differences, and long continuous high-load operation time. Tank exhaust is a mixture composed of multiple components, mainly including hydrocarbons (HC), nitrogen oxides ( NOx ) and soot particles (soot). Among them, NO x can cause permanent damage to the human body's eyes, respiratory system and central nervous system, and NO x is also the main cause of acid rain; HC is a product of incomplete combustion of fuel and is toxic, flammable, explosive and carcinogenic. and other properties, and HC is easily photochemically reacted with NO The distance is long and it is easy to cause large-scale pollution. In addition, soot particles also have a strong carcinogenic effect. After they enter the human lungs with breathing, they can easily accumulate in the alveoli and other parts of the lungs, leading to respiratory diseases, heart diseases and even cancer. .
在坦克尾气排气管路上安装尾气净化装置是一种有效而经济的后处理技术，它通常采用过滤器等手段将坦克尾气中碳烟颗粒物进行拦截捕集，使其聚集在净化装置中，但是当碳烟颗粒物积累到一定程度后，会导致尾气背压的增加，影响发动机正常排气，必须用燃烧等手段将其除去，以保住尾气正常的背压，从而实现净化装置再生。如果将催化剂涂覆在过滤器表面，通过催化作用既能将HC氧化成无毒害的CO2，又可以将NO氧化成NO2，并进一步利用NO2较强的氧化能力在低温实现捕集聚集的碳烟颗粒物氧化，就可以实现坦克尾气污染物的有效净化。因此，开发经济高效的坦克尾气净化催化剂有着重要意义的，目前未见有关文献报道。Installing an exhaust purification device on the tank exhaust exhaust pipeline is an effective and economical post-processing technology. It usually uses filters and other means to intercept and capture the soot particles in the tank exhaust and collect them in the purification device. However, When soot particles accumulate to a certain extent, they will increase the back pressure of the exhaust gas and affect the normal exhaust of the engine. They must be removed by combustion and other means to maintain the normal back pressure of the exhaust gas and achieve regeneration of the purification device. If a catalyst is coated on the surface of the filter, HC can be oxidized into non-toxic CO 2 through catalysis, and NO can be oxidized into NO 2 , and the strong oxidation ability of NO 2 can be further used to achieve capture and accumulation at low temperatures. By oxidizing the soot particles, the tank exhaust pollutants can be effectively purified. Therefore, it is of great significance to develop an economical and efficient tank exhaust gas purification catalyst, but there are currently no relevant literature reports.
发明内容Contents of the invention
为了解决上述问题，本发明提供了一种原料安全、制备步骤简单，经济性好，且净化效果好的坦克尾气净化整体式催化剂及制备方法。In order to solve the above problems, the present invention provides an integrated catalyst for tank exhaust gas purification with safe raw materials, simple preparation steps, good economy, and good purification effect, and a preparation method.
为了达到上述目的，本发明是通过以下技术方案来实现的：In order to achieve the above objects, the present invention is achieved through the following technical solutions:
本发明是一种用于坦克尾气净化整体式催化剂的制备方法，催化剂包括载体、粘结涂层和活性物，载体为预处理后的蜂窝陶瓷过滤体，粘结涂层为铝溶胶涂层，活性物为负载贵金属Pt的铈铝混合氧化物；催化剂的制备步骤如下：The invention is a preparation method for an integral catalyst for tank exhaust gas purification. The catalyst includes a carrier, a bonding coating and an active substance. The carrier is a pretreated honeycomb ceramic filter body, and the bonding coating is an aluminum sol coating. The active material is a cerium-aluminum mixed oxide supporting the precious metal Pt; the preparation steps of the catalyst are as follows:
(1)制备载体：将蜂窝陶瓷过滤体置于质量分数为5％～15％的草酸溶液中，加热至85～95℃，预处理6～24h，然后烘干，获得预处理后的蜂窝陶瓷过滤体；(1) Preparation of carrier: Place the honeycomb ceramic filter body in an oxalic acid solution with a mass fraction of 5% to 15%, heat to 85 to 95°C, pretreat for 6 to 24 hours, and then dry to obtain the pretreated honeycomb ceramics filter body;
(2)制备铝溶胶；以拟薄水铝石为铝源，冰醋酸为解胶剂，将拟薄水铝石溶解于去离子水后，加入冰醋酸充分搅拌，获得铝溶胶；(2) Prepare aluminum sol; use pseudo-boehmite as the aluminum source and glacial acetic acid as the deglueing agent. After dissolving the pseudo-boehmite in deionized water, add glacial acetic acid and stir thoroughly to obtain the aluminum sol;
(3)制备活性物：将氧化铝粉末与氧化铈粉末研磨混合，获得混合氧化物粉末；采用等体积浸渍法将适量硝酸铂Pt(NO3)4或氯铂酸H2PtCl6负载到上述混合氧化物粉末上，获得前驱体样品；将所得前驱体样品于120℃烘干1小时，再于500℃煅烧2小时，获得负载贵金属Pt的铈铝混合氧化物；(3) Preparation of active materials: Grind and mix alumina powder and cerium oxide powder to obtain mixed oxide powder; use an equal volume impregnation method to load an appropriate amount of platinum nitrate Pt(NO 3 ) 4 or chloroplatinic acid H 2 PtCl 6 onto the above On the mixed oxide powder, a precursor sample is obtained; the obtained precursor sample is dried at 120°C for 1 hour, and then calcined at 500°C for 2 hours to obtain a cerium-aluminum mixed oxide loaded with precious metal Pt;
(4)制备浆液：将步骤(3)制备的负载贵金属Pt的铈铝混合氧化物加入到步骤(2)制备的铝溶胶中，搅拌混合均匀，加入去离子水，室温陈化，得到混合浆液；(4) Prepare slurry: Add the precious metal Pt-loaded cerium-aluminum mixed oxide prepared in step (3) to the aluminum sol prepared in step (2), stir and mix evenly, add deionized water, and age at room temperature to obtain a mixed slurry. ;
(5)制备整体式催化剂：采用真空抽提法或浸渍法，将混合浆液涂覆在预处理后的蜂窝陶瓷过滤体表面，再将涂覆有混合浆液涂的蜂窝陶瓷过滤体于120℃烘干，在500℃煅烧2小时，重复上述涂覆、烘干、焙烧流程，直至涂覆量达到50g/L以上，获得整体式催化剂。(5) Preparation of monolithic catalyst: Use vacuum extraction method or impregnation method to coat the mixed slurry on the surface of the pretreated honeycomb ceramic filter, and then bake the honeycomb ceramic filter coated with the mixed slurry at 120°C. Dry, calcine at 500°C for 2 hours, and repeat the above coating, drying, and roasting processes until the coating amount reaches more than 50g/L to obtain a monolithic catalyst.
本发明的进一步改进在于：步骤(1)中的蜂窝陶瓷过滤体为壁流式结构，其中，堇青石或莫来石中的一种为蜂窝陶瓷过滤体的主要成分。A further improvement of the present invention is that the honeycomb ceramic filter body in step (1) has a wall flow structure, in which one of cordierite or mullite is the main component of the honeycomb ceramic filter body.
本发明的进一步改进在于：步骤(2)中所加去离子水质量为拟薄水铝石质量的10～20倍，所加冰醋酸质量为拟薄水铝石质量的1～1.5倍。A further improvement of the present invention is that the mass of deionized water added in step (2) is 10-20 times the mass of pseudo-boehmite, and the mass of glacial acetic acid added is 1-1.5 times the mass of pseudo-boehmite.
本发明的进一步改进在于：步骤(3)中氧化铝粉末与氧化铈粉末质量比为3:1～5:1，贵金属Pt负载量为混合氧化物总质量的0.5％～2％。A further improvement of the present invention is that in step (3), the mass ratio of aluminum oxide powder to cerium oxide powder is 3:1 to 5:1, and the loading amount of precious metal Pt is 0.5% to 2% of the total mass of the mixed oxide.
本发明的进一步改进在于：步骤(4)中负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为5:1～20:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的5～20倍，陈化时间为6～12h。A further improvement of the present invention is that in step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with precious metal Pt to the aluminum sol is 5:1 to 20:1, and the mass of the added deionized water is the cerium-aluminum mixed oxide loaded with precious metal Pt. The total mass of oxide and aluminum sol is 5 to 20 times, and the aging time is 6 to 12 hours.
本发明的有益效果是：通过本发明制备的整体式催化剂不仅具有良好的碳烟颗粒氧化去除能力，还能实现尾气中CO、HCs和NOx的有效净化。The beneficial effects of the present invention are: the integrated catalyst prepared by the present invention not only has good soot particle oxidation removal capabilities, but can also achieve effective purification of CO, HC s and NO x in the exhaust gas.
附图说明Description of the drawings
图1是本发明制备的坦克尾气净化整体式催化剂截面示意图。Figure 1 is a schematic cross-sectional view of the integrated catalyst for tank exhaust gas purification prepared by the present invention.
具体实施方式Detailed ways
下面对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。The invention is further described below. The following examples are only used to illustrate the technical solutions of the present invention more clearly, but cannot be used to limit the scope of protection of the present invention.
本发明是一种用于坦克尾气净化整体式催化剂的制备方法，催化剂包括载体1、粘结涂层2和活性物3，载体1为预处理后的蜂窝陶瓷过滤体，粘结涂层2为铝溶胶涂层，活性物3为负载贵金属Pt的铈铝混合氧化物；催化剂的制备步骤如下：The invention is a preparation method for an integral catalyst for tank exhaust gas purification. The catalyst includes a carrier 1, a bonding coating 2 and an active substance 3. The carrier 1 is a pretreated honeycomb ceramic filter body, and the bonding coating 2 is Aluminum sol coating, active material 3 is cerium-aluminum mixed oxide supporting precious metal Pt; the preparation steps of the catalyst are as follows:
(1)制备载体：将蜂窝陶瓷过滤体置于质量分数为5％～15％的草酸溶液中，加热至85～95℃,预处理6～24h，然后烘干，获得预处理后的蜂窝陶瓷过滤体；其中，蜂窝陶瓷过滤体为壁流式结构，其中，堇青石或莫来石中的一种为蜂窝陶瓷过滤体的主要成分：(1) Preparation of carrier: Place the honeycomb ceramic filter body in an oxalic acid solution with a mass fraction of 5% to 15%, heat to 85 to 95°C, pretreat for 6 to 24 hours, and then dry to obtain the pretreated honeycomb ceramic Filter body; wherein, the honeycomb ceramic filter body has a wall flow structure, in which one of cordierite or mullite is the main component of the honeycomb ceramic filter body:
(2)制备铝溶胶；以拟薄水铝石为铝源，冰醋酸为解胶剂，将拟薄水铝石溶解于去离子水后，加入冰醋酸充分搅拌，获得铝溶胶；其中，所加去离子水质量为拟薄水铝石质量的10～20倍，所加冰醋酸质量为拟薄水铝石质量的1～1.5倍；(2) Prepare aluminum sol; use pseudo-boehmite as the aluminum source and glacial acetic acid as the deglueing agent. After dissolving the pseudo-boehmite in deionized water, add glacial acetic acid and stir thoroughly to obtain the aluminum sol; where, The mass of deionized water added is 10 to 20 times the mass of pseudo-boehmite, and the mass of glacial acetic acid added is 1 to 1.5 times the mass of pseudo-boehmite;
(3)制备活性物：将氧化铝粉末与氧化铈粉末研磨混合，获得混合氧化物粉末；采用等体积浸渍法将适量硝酸铂Pt(NO3)4或氯铂酸H2PtCl6负载到上述混合氧化物粉末上，获得前驱体样品；将所得前驱体样品于120℃烘干1小时，再于500℃煅烧2小时，获得负载贵金属Pt的铈铝混合氧化物；其中，氧化铝粉末与氧化铈粉末质量比为5:1～3:1，贵金属Pt负载量为混合氧化物总质量的0.5％～2％；(3) Preparation of active materials: Grind and mix alumina powder and cerium oxide powder to obtain mixed oxide powder; use an equal volume impregnation method to load an appropriate amount of platinum nitrate Pt(NO 3 ) 4 or chloroplatinic acid H 2 PtCl 6 onto the above On the mixed oxide powder, a precursor sample was obtained; the obtained precursor sample was dried at 120°C for 1 hour, and then calcined at 500°C for 2 hours to obtain a cerium-aluminum mixed oxide loaded with precious metal Pt; wherein, the alumina powder and oxide The mass ratio of cerium powder is 5:1 to 3:1, and the loading of precious metal Pt is 0.5% to 2% of the total mass of the mixed oxide;
(4)制备浆液：将步骤(3)制备的负载贵金属Pt的铈铝混合氧化物加入到步骤(2)制备的铝溶胶中，搅拌混合均匀，加入去离子水，室温陈化6h，得到混合浆液；其中，负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为20:1～5:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的5～20倍，陈化时间为6～12h。(4) Preparation of slurry: Add the cerium-aluminum mixed oxide loaded with precious metal Pt prepared in step (3) to the aluminum sol prepared in step (2), stir and mix evenly, add deionized water, and age at room temperature for 6 hours to obtain a mixture Slurry; wherein, the mass ratio of the cerium-aluminum mixed oxide loaded with precious metal Pt to the aluminum sol is 20:1 to 5:1, and the mass of the added deionized water is the total mass of the cerium-aluminum mixed oxide loaded with precious metal Pt and the aluminum sol. 5 to 20 times, and the aging time is 6 to 12 hours.
(5)制备整体式催化剂：采用真空抽提法或浸渍法，将混合浆液涂覆在预处理后的蜂窝陶瓷过滤体表面，再将涂覆有混合浆液涂的蜂窝陶瓷过滤体于120℃烘干，在500℃煅烧2小时，重复上述涂覆、烘干、焙烧流程，直至涂覆量达到50g/L以上，获得整体式催化剂。(5) Preparation of monolithic catalyst: Use vacuum extraction method or impregnation method to coat the mixed slurry on the surface of the pretreated honeycomb ceramic filter, and then bake the honeycomb ceramic filter coated with the mixed slurry at 120°C. Dry, calcine at 500°C for 2 hours, and repeat the above coating, drying, and roasting processes until the coating amount reaches more than 50g/L to obtain a monolithic catalyst.
实施例1Example 1
本发明是一种用于坦克尾气净化整体式催化剂的制备方法，催化剂包括载体、粘结涂层和活性物，载体为预处理后的蜂窝陶瓷过滤体，粘结涂层为铝溶胶涂层，活性物为负载贵金属Pt的铈铝混合氧化物；催化剂的制备步骤如下：The invention is a preparation method for an integral catalyst for tank exhaust gas purification. The catalyst includes a carrier, a bonding coating and an active substance. The carrier is a pretreated honeycomb ceramic filter body, and the bonding coating is an aluminum sol coating. The active material is a cerium-aluminum mixed oxide supporting the precious metal Pt; the preparation steps of the catalyst are as follows:
(1)制备载体：蜂窝陶瓷过滤体为壁流式结构，堇青石为主要成分，将蜂窝陶瓷过滤体置于质量分数为5％的草酸溶液中，加热至85℃,预处理6h，然后烘干，获得预处理后的蜂窝陶瓷过滤体；(1) Preparation of carrier: The honeycomb ceramic filter body has a wall flow structure, and cordierite is the main component. The honeycomb ceramic filter body is placed in an oxalic acid solution with a mass fraction of 5%, heated to 85°C, pretreated for 6 hours, and then baked Dry to obtain the pretreated honeycomb ceramic filter body;
(2)制备铝溶胶：以拟薄水铝石为铝源，冰醋酸为解胶剂，将拟薄水铝石溶解于去离子水后，加入冰醋酸充分搅拌，获得铝溶胶；其中，所加去离子水质量为拟薄水铝石质量的10倍，所加冰醋酸质量为拟薄水铝石质量的1倍；(2) Preparation of aluminum sol: Use pseudo-boehmite as the aluminum source and glacial acetic acid as the deglueing agent. After dissolving the pseudo-boehmite in deionized water, add glacial acetic acid and stir thoroughly to obtain the aluminum sol; where, The mass of deionized water added is 10 times the mass of pseudo-boehmite, and the mass of glacial acetic acid added is 1 times the mass of pseudo-boehmite;
(3)制备活性物：将氧化铝粉末与氧化铈粉末研磨混合，获得混合氧化物粉末；采用等体积浸渍法将适量硝酸铂Pt(NO3)4或氯铂酸H2PtCl6负载到上述混合氧化物粉末上，获得前驱体样品；将所得前驱体样品于120℃烘干1小时，再于500℃煅烧2小时，获得负载贵金属Pt的铈铝混合氧化物；其中，氧化铝粉末与氧化铈粉末质量比为5:1，贵金属Pt负载量为混合氧化物总质量的0.5％；(3) Preparation of active materials: Grind and mix alumina powder and cerium oxide powder to obtain mixed oxide powder; use an equal volume impregnation method to load an appropriate amount of platinum nitrate Pt(NO 3 ) 4 or chloroplatinic acid H 2 PtCl 6 onto the above On the mixed oxide powder, a precursor sample was obtained; the obtained precursor sample was dried at 120°C for 1 hour, and then calcined at 500°C for 2 hours to obtain a cerium-aluminum mixed oxide loaded with precious metal Pt; wherein, the alumina powder and oxide The mass ratio of cerium powder is 5:1, and the loading amount of precious metal Pt is 0.5% of the total mass of the mixed oxide;
(4)制备浆液：将步骤(3)制备的负载贵金属Pt的铈铝混合氧化物加入到步骤(2)制备的铝溶胶中，搅拌混合均匀，加入去离子水，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的10倍，室温陈化6h，得到混合浆液；其中，负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为20:1；(4) Prepare slurry: Add the cerium-aluminum mixed oxide loaded with precious metal Pt prepared in step (3) to the aluminum sol prepared in step (2), stir and mix evenly, and add deionized water. The mass of the added deionized water is The total mass of cerium-aluminum mixed oxide and aluminum sol loaded with precious metal Pt is 10 times, and aged at room temperature for 6 hours to obtain a mixed slurry; where the mass ratio of cerium-aluminum mixed oxide loaded with precious metal Pt to aluminum sol is 20:1;
(5)制备整体式催化剂：采用真空抽提法，将混合浆液涂覆在预处理后的蜂窝陶瓷过滤体表面，再将涂覆有混合浆液涂的蜂窝陶瓷过滤体于120℃烘干，在500℃煅烧2小时，重复上述涂覆、烘干、焙烧流程3次，涂覆量为52g/L，获得整体式催化剂。(5) Preparation of monolithic catalyst: Use vacuum extraction method to coat the mixed slurry on the surface of the pretreated honeycomb ceramic filter, and then dry the honeycomb ceramic filter coated with the mixed slurry at 120°C. Calculate at 500°C for 2 hours, repeat the above coating, drying, and roasting processes three times. The coating amount is 52g/L to obtain a monolithic catalyst.
实施例2Example 2
与实施例1区别在于：制备步骤(1)的蜂窝陶瓷过滤体的主要成分为莫来石；步骤(3)贵金属Pt负载量为混合氧化物总质量的0.75％；步骤(4)中负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为15:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的5倍，室温陈化时间为6h；步骤(5)采用真空抽提法，将混合浆液涂覆在预处理后的蜂窝陶瓷过滤体表面，再将涂覆有混合浆液涂的蜂窝陶瓷过滤体于120℃烘干，在500℃煅烧2小时，重复上述涂覆、烘干、焙烧流程3次，涂覆量为53g/L。The difference from Example 1 is that: the main component of the honeycomb ceramic filter in the preparation step (1) is mullite; the loading amount of the precious metal Pt in the step (3) is 0.75% of the total mass of the mixed oxide; the precious metal is loaded in the step (4) The mass ratio of Pt's cerium-aluminum mixed oxide and aluminum sol is 15:1, the mass of deionized water added is 5 times the total mass of the cerium-aluminum mixed oxide and aluminum sol loaded with precious metal Pt, and the room temperature aging time is 6 hours; Step (5) uses the vacuum extraction method to coat the mixed slurry on the surface of the pretreated honeycomb ceramic filter, and then dry the honeycomb ceramic filter coated with the mixed slurry at 120°C and calcine at 500°C for 2 hours, repeat the above coating, drying, and roasting processes three times, and the coating amount is 53g/L.
实施例3Example 3
与实施例1区别在于：步骤(1)将蜂窝陶瓷过滤体置于质量分数为8％的草酸溶液中，加热至90℃,预处理12h；步骤(2)中所加去离子水质量为拟薄水铝石质量的12倍，所加冰醋酸质量为拟薄水铝石质量的1.2倍；步骤(3)中贵金属Pt负载量为混合氧化物总质量的1％；步骤(4)中负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为12:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的8倍，室温陈化时间为8h；步骤(5)采用真空抽提法，重复涂覆、烘干、焙烧流程3次，涂覆量为55g/L。The difference from Example 1 is that: in step (1), the honeycomb ceramic filter body is placed in an oxalic acid solution with a mass fraction of 8%, heated to 90°C, and pretreated for 12 hours; in step (2), the mass of deionized water added is 12 times the mass of boehmite, and the mass of glacial acetic acid added is 1.2 times the mass of pseudo-boehmite; the loading of precious metal Pt in step (3) is 1% of the total mass of the mixed oxide; the loading in step (4) The mass ratio of the cerium-aluminum mixed oxide of precious metal Pt to the aluminum sol is 12:1. The mass of deionized water added is 8 times the total mass of the cerium-aluminum mixed oxide and aluminum sol loaded with precious metal Pt. The aging time at room temperature is 8 hours. ; Step (5) uses the vacuum extraction method, repeats the coating, drying, and roasting processes three times, and the coating amount is 55g/L.
实施例4Example 4
与实施例3的区别在于：步骤(1)的蜂窝陶瓷过滤体的主要成分为莫来石；步骤(3)中氧化铝粉末与氧化铈粉末质量比为4.5:1，贵金属Pt负载量为混合氧化物总质量的1.25％；步骤(4)中负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为10:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的12倍，室温陈化时间为8h；步骤(5)重复涂覆、烘干、焙烧流程3次，涂覆量为58g/L。The difference from Example 3 is that: the main component of the honeycomb ceramic filter in step (1) is mullite; in step (3), the mass ratio of alumina powder to cerium oxide powder is 4.5:1, and the loading amount of precious metal Pt is mixed 1.25% of the total mass of the oxide; in step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with precious metal Pt to the aluminum sol is 10:1, and the mass of deionized water added is 10:1. 12 times the total mass of the aluminum sol, and the room temperature aging time is 8 hours; step (5) repeats the coating, drying, and roasting process three times, and the coating amount is 58g/L.
实施例5Example 5
与实施例3的区别在于：步骤(1)将蜂窝陶瓷过滤体置于质量分数为10％的草酸溶液中，加热至90℃,预处理18h；步骤(2)中所加去离子水质量为拟薄水铝石质量的15倍，所加冰醋酸质量为拟薄水铝石质量的1.3倍；步骤(3)中氧化铝粉末与氧化铈粉末质量比为4:1，贵金属Pt负载量为混合氧化物总质量的1.5％；步骤(4)中负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为8:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的15倍，室温陈化时间为10h；步骤(5)中粘结涂层的涂覆量为59g/L。The difference from Example 3 is that: in step (1), the honeycomb ceramic filter body is placed in an oxalic acid solution with a mass fraction of 10%, heated to 90°C, and pretreated for 18 hours; the mass of deionized water added in step (2) is 15 times the mass of pseudo-boehmite, and the mass of glacial acetic acid added is 1.3 times the mass of pseudo-boehmite; in step (3), the mass ratio of alumina powder to cerium oxide powder is 4:1, and the loading amount of precious metal Pt is 1.5% of the total mass of the mixed oxide; in step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with precious metal Pt to the aluminum sol is 8:1, and the mass of the added deionized water is the cerium-aluminum mixed oxide loaded with precious metal Pt It is 15 times the total mass of the aluminum sol, and the aging time at room temperature is 10 hours; the coating amount of the bonding coating in step (5) is 59g/L.
实施例6Example 6
与实施例5的区别在于：步骤(1)蜂窝陶瓷过滤体的主要成分为莫来石，步骤(2)中所加去离子水质量为拟薄水铝石质量的15倍，所加冰醋酸质量为拟薄水铝石质量的1.4倍；步骤(3)中氧化铝粉末与氧化铈粉末质量比为3.5:1，贵金属Pt负载量为混合氧化物总质量的1.75％；步骤(4)中负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为7:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的18倍，室温陈化时间为10h.The difference from Example 5 is that: the main component of the honeycomb ceramic filter in step (1) is mullite, the mass of deionized water added in step (2) is 15 times the mass of pseudo-boehmite, and the glacial acetic acid added The mass is 1.4 times the mass of pseudo-boehmite; in step (3), the mass ratio of alumina powder to cerium oxide powder is 3.5:1, and the precious metal Pt loading is 1.75% of the total mass of the mixed oxide; in step (4) The mass ratio of the cerium-aluminum mixed oxide loaded with precious metal Pt to aluminum sol is 7:1. The mass of deionized water added is 18 times the total mass of the cerium-aluminum mixed oxide loaded with precious metal Pt and aluminum sol. The room temperature aging time is 10h.
实施例7Example 7
与实施例6相比，步骤(1)蜂窝陶瓷过滤体的主要成分为堇青石，将蜂窝陶瓷过滤体置于质量分数为15％的草酸溶液中，加热至95℃,预处理24h；步骤(2)中所加去离子水质量为拟薄水铝石质量的20倍，所加冰醋酸质量为拟薄水铝石质量的1.5倍；步骤(3)中氧化铝粉末与氧化铈粉末质量比为3:1，贵金属Pt负载量为混合氧化物总质量的2％；步骤(4)负载贵金属Pt的铈铝混合氧化物与铝溶胶的质量比为5:1，所加去离子水质量为负载贵金属Pt的铈铝混合氧化物与铝溶胶总质量的20倍，室温陈化时间为12h；步骤(5)中粘结涂层的涂覆量为64g/L。Compared with Example 6, the main component of the honeycomb ceramic filter body in step (1) is cordierite. The honeycomb ceramic filter body is placed in an oxalic acid solution with a mass fraction of 15%, heated to 95°C, and pretreated for 24 hours; step ( The mass of deionized water added in 2) is 20 times the mass of pseudo-boehmite, and the mass of glacial acetic acid added is 1.5 times the mass of pseudo-boehmite; the mass ratio of alumina powder to cerium oxide powder in step (3) is 3:1, and the loading amount of precious metal Pt is 2% of the total mass of the mixed oxide; the mass ratio of the cerium-aluminum mixed oxide and aluminum sol loaded with precious metal Pt in step (4) is 5:1, and the mass of deionized water added is The total mass of the cerium-aluminum mixed oxide and aluminum sol loaded with precious metal Pt is 20 times, and the room temperature aging time is 12 hours; the coating amount of the bonding coating in step (5) is 64g/L.
模拟尾气净化测试Simulated exhaust gas purification test
所制备整体式催化剂置于模拟碳烟再生发生器上进行碳烟上载，上载量为10g/L，在模拟坦克尾气条件下(在10％O2+1000ppmNO+800ppmC3H6，平衡气为N2，空速为100000h-1)进行尾气净化测试，结果如下：The prepared integrated catalyst was placed on a simulated soot regeneration generator for soot uploading. The loading amount was 10g/L. Under simulated tank exhaust conditions (10% O 2 +1000ppmNO+800ppmC 3 H 6 , the balance gas was N 2 , the airspeed is 100000h -1 ) for exhaust gas purification test, the results are as follows:
实车排气烟度测试Real vehicle exhaust smoke test
将所制备整体式催化实施例7封装后，安装于某型坦克车辆顶部，根据《非道路移动柴油机排气烟度限值及测量方法》(GB36886-2018)要求，进行实车排气烟度测试，结果如下：After the prepared integrated catalytic Example 7 was packaged, it was installed on the top of a certain type of tank vehicle. According to the requirements of "Non-road Mobile Diesel Engine Exhaust Smoke Limits and Measurement Methods" (GB36886-2018), the actual vehicle exhaust smoke was measured. Test, the results are as follows:
以上仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变形，这些改进和变形也应视为本发明的保护范围。The above are only the preferred embodiments of the present invention. It should be pointed out that for those of ordinary skill in the art, several improvements and deformations can be made without departing from the technical principles of the present invention. These improvements and deformations should also be considered. regarded as the protection scope of the present invention.
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