CN113546613A - 一种铝溶胶的制备方法及用途 - Google Patents
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 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 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 6
- 241000264877 Hippospongia communis Species 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 6
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 6
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- 239000012798 spherical particle Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims 3
- 238000000034 method Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229910052878 cordierite Inorganic materials 0.000 description 21
- 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 compound [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 description 21
- 230000002378 acidificating effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000011833 salt mixture Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- -1 aluminum ions Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 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 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
本发明提供了一种铝溶胶的制备方法及用途,属于催化剂制备领域。本发明所述的铝溶胶,配制了含有铝盐酸性溶液的溶胶,用于成型载体的涂覆,解决了成型催化剂工业生产中活性氧化铝载体单次负载量少的难题。本发明中配制的铝溶胶可以实现单次负载量可控和氧化铝均匀涂覆且稳定的特点,提高了催化剂的生产效率,节约了生产能耗和生产成本。
Description
技术领域
本发明属于催化剂制备领域,尤其是涉及一种铝溶胶的制备方法及其在催化剂生产过程中的应用。
技术背景
堇青石粉、莫来石粉、刚玉粉和氧化铝粉是常见的载体原材料,具有热膨胀系数小,抗热震性能好,升温快,耐热冲击性好等优点,广泛应用于制造成型载体,可形成耐高温、机械强度高、传热效率高的各种形状的载体基材。
虽然这些基材存在其特有的优势,但是成型后载体基材的比表面积减小,孔结构会出现坍塌,不利于活性相的负载,导致催化剂整体活性较低。因此,迫切需要开发一种配制方便、成本低廉的溶胶作为第二载体的前驱体涂层。目前,最常见的涂覆溶胶为铝溶胶,其具备铝盐原料来源广泛、成本低等优点,煅烧后形成的γ-Al2O3具有比表面积大,孔结构丰富,孔径分布广等优势。但是传统铝溶胶中的固含量较低,单次涂覆量不能满足要求。
发明内容
有鉴于此,本发明旨在配制一种固含量较高的铝溶胶,以克服现有技术中单次涂覆量较低的问题。
为达到上述目的,本发明的技术方案是这样实现的:
一种铝溶胶的制备方法,包括如下步骤,
1)将至少一种铝盐粉料加入水中,混合后得到确定固含量的铝盐悬浮液;
本步骤中是以拟薄水铝石为主要组分,硝酸铝、硫酸铝、氯化铝和异丙醇铝等铝盐作为辅助,均匀混合,得到铝盐混料。
2)量取一定体积的水、65%浓硝酸和36.5%盐酸,配制浓度为1~3mol/L HNO3+1~3mol/L HCl的酸性水溶液。
3)将得到铝盐悬浊液逐滴加入2)中的酸性水溶液,得到固含量为>0~40%的铝溶胶。
本发明铝溶胶用于成型载体的涂覆制备催化剂。成型载体形状包括且不限于球型颗粒、圆柱状、椭圆状、蜂窝状、棱柱状。涂覆方法包括且不限于等体积浸渍、过量浸渍和喷淋。
与现有技术相比,本发明的有益技术效果是:
本发明铝溶胶具备铝含量高、形态稳定等特点。铝溶胶中的酸溶液可以阻止铝离子水解沉淀形成固体,从而保证铝溶胶可以稳定存在一段时间。铝溶胶还可以根据所需的γ-Al2O3涂覆量控制铝含量,单次的涂覆γ-Al2O3的最大量可达到20%,大幅提高了γ-Al2O3的涂覆效率和催化剂的生产效率。
附图说明
图1为三个实施例的γ-Al2O3单次负载质量百分比,负载基材为蜂窝状堇青石。
具体实施方式
除有定义外,以下实施例中所用的技术术语具有与本发明所属领域技术人员普遍理解的相同含义。以下实施例中所用的试验试剂,如无特殊说明,均为常规生化试剂;所述实验方法,如无特殊说明,均为常规方法。
下面结合实施例来详细说明本发明。
实施例1
固含量10%铝溶胶的制备
分别称取80g拟薄水铝石、10g硝酸铝、5g硫酸铝、2g氯化铝和3g异丙醇铝充分混合,得到铝盐混料。量取50ml 65%HNO3、68.5ml 36.5%HCl和990ml充分混合,得到1mol/LHNO3+2mol/L HCl的酸性混合溶液。将400g水和100g铝盐混料混合,得到铝盐悬浊液。之后在铝盐悬浊液中逐滴加入500g酸性混合溶液,得到固含量10%铝溶胶。
将150g蜂窝状堇青石完全浸渍,放置于固含量10%铝溶胶中4h,取出后干燥并煅烧,称重后得到4.7wt%γ-Al2O3/堇青石载体。
实施例2
分别称取150g拟薄水铝石、20g硝酸铝、10g硫酸铝、15g氯化铝和5g异丙醇铝充分混合,得到铝盐混料。量取104.8ml 65%HNO3、72.2ml 36.5%HCl和990ml充分混合,得到2mol/L HNO3+2mol/L HCl的酸性混合溶液。将300g水和200g铝盐混料混合,得到铝盐悬浊液。之后在铝盐悬浊液中逐滴加入500g酸性混合溶液,得到固含量20%铝溶胶。
将150g蜂窝状堇青石完全浸渍,放置于固含量20%铝溶胶中4h,取出后干燥并煅烧,称重后得到9.2wt%γ-Al2O3/堇青石载体。
实施例3
分别称取200g拟薄水铝石、80g硝酸铝、10g硫酸铝、5g氯化铝和5g异丙醇铝充分混合,得到铝盐混料。量取166.5ml 65%HNO3、76.3ml 36.5%HCl和990ml充分混合,得到1mol/L HNO3+2mol/L HCl的酸性混合溶液。将200g水和300g铝盐混料混合,得到铝盐悬浊液。之后在铝盐悬浊液中逐滴加入500g酸性混合溶液,得到固含量30%铝溶胶。
将150g蜂窝状堇青石完全浸渍,放置于固含量30%铝溶胶中4h,取出后干燥并煅烧,称重后得到15.1wt%γ-Al2O3/堇青石载体。
附图1示出了本发明制备得到的三种固含量铝溶胶的负载效果。如图所示可知,随着铝溶胶固含量的增加,堇青石负载后的γ-Al2O3含量逐渐增加。
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,作出的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种铝溶胶的制备方法,包括如下步骤,
1)将至少一种铝盐粉料加入水中,混合后得到确定固含量的铝盐悬浮液;
2)将一定比例的浓硝酸、盐酸和水混合,搅拌均匀后得到酸性溶液;
3)根据铝盐悬浮液的固含量,确定所需酸性溶液的体积,将酸性溶液逐滴缓慢加入铝盐悬浮液,配制成铝溶胶。
2.根据权利要求1所述的铝溶胶的制备方法,其特征在于:铝盐粉料包括但不限于硝酸铝、硫酸铝、拟薄水铝石、异丙醇铝、氯化铝的粉料。
3.根据权利要求1所述的铝溶胶的制备方法,其特征在于:至少一种铝盐是指硝酸铝、硫酸铝、拟薄水铝石、异丙醇铝、氯化铝中的任意一种或其组合。
4.根据权利要求1所述的铝溶胶的制备方法,其特征在于:浓硝酸和盐酸的用量比为1mol/L:1-3mol/L。
5.根据权利要求1所述的铝溶胶的制备方法,其特征在于:所得铝溶胶中固含量为>0~40%。
6.一种铝溶胶,其特征在于:通过权利要求1-5任一项方法制备得到。
7.一种权利要求6所述的铝溶胶的用途,其特征在于:所述的铝溶胶用于成型载体的涂覆制备催化剂。
8.根据权利要求7所述的铝溶胶的用途,其特征在于:所述的成型载体形状包括且不限于球型颗粒、圆柱状、椭圆状、蜂窝状、棱柱状。
9.根据权利要求7所述的铝溶胶的用途,其特征在于:涂覆方法包括且不限于等体积浸渍、过量浸渍和喷淋。
10.一种催化剂,其特征在于:是将权利要求6的铝溶胶涂覆在成型载体上得到。
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH10236820A (ja) * | 1996-12-26 | 1998-09-08 | Asahi Glass Co Ltd | アルミナゾル及びアルミナ水和物粉末の製造方法及び記録媒体 |
CN104353400A (zh) * | 2014-11-12 | 2015-02-18 | 山东恒通晶体材料有限公司 | 一种高纯度、高固含量透明铝溶胶的制备方法 |
CN112973771A (zh) * | 2021-02-25 | 2021-06-18 | 西南化工研究设计院有限公司 | 含有分子筛和氧化铝的球形催化剂载体及其制备和应用 |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH10236820A (ja) * | 1996-12-26 | 1998-09-08 | Asahi Glass Co Ltd | アルミナゾル及びアルミナ水和物粉末の製造方法及び記録媒体 |
CN104353400A (zh) * | 2014-11-12 | 2015-02-18 | 山东恒通晶体材料有限公司 | 一种高纯度、高固含量透明铝溶胶的制备方法 |
CN112973771A (zh) * | 2021-02-25 | 2021-06-18 | 西南化工研究设计院有限公司 | 含有分子筛和氧化铝的球形催化剂载体及其制备和应用 |
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Application publication date: 20211026 |