CN111545209A - 基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法 - Google Patents
基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法 Download PDFInfo
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 23
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 23
- 239000002135 nanosheet Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000010949 copper Substances 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000011592 zinc chloride Substances 0.000 claims description 15
- 235000005074 zinc chloride Nutrition 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 5
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009903 catalytic hydrogenation reaction Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- -1 zinc aluminate Chemical class 0.000 description 1
Classifications
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- 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
- B01J23/80—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 zinc, cadmium or mercury
-
- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
- C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
- C07C29/153—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the catalyst used
- C07C29/154—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the catalyst used containing copper, silver, gold, or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
- C07C2523/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36 with zinc, cadmium or mercury
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
本发明公开一种基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法,获得催化活性和稳定性优良的Cu/ZnO纳米催化剂，并且所用原料药剂安全易得，用于二氧化碳催化加氢制甲醇，在较低温度425℃下表现出较高的催化反应活性，CO2转化率达到83％以上，CO产率达到31％以上，CH3OH产率达到52％以上，可用于绿色环保新能源的开发与应用。
Description
技术领域
本发明属于化工领域，涉及一种基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法。
背景技术
水煤气(WGS)变换反应已经研究了近一个世纪，工艺比较成熟。而逆水煤气变换反应(RWGS)可以利用丰富而廉价的二氧化碳作为碳源，利用RWGS反应生成的一氧化碳作为中间产物，采用F-T合成法制备烯烃；也可以利用RWGS生产乙醇。目前广泛应用于生产甲醇的CAMERE法，其中高温下的RWGS反应是其关键步骤，一氧化碳的转化率越高对甲醇的合成就越有利。因此高稳定性的催化剂对CAMERE反应至关重要。
传统的RWGS催化剂主要包括铝酸锌催化剂、Pt/CeO2催化剂、铜基催化剂和锰基催化剂等。上述催化剂主要采用沉淀法制备氧化铁催化剂，主要包括原料溶解混合、中和、热煮、洗涤、过滤、干燥和焙烧几个步骤。由于RWGS属于多相反应，因此要求催化剂具有复杂的化学组成和特殊的物理结构。采用不同的制备方法，催化剂的化学组成相同，但是物理结构有差异，催化效果差异较大。上述沉淀法制备氧化铁催化剂，制备的氧化铁催化剂粒径不均匀，分散度低，催化效果差。因此利用氧化铜纳米片作为模板，制备铁系催化剂的方法日益流行。但是上述方法需要最后将铜元素去除，防止催化干扰，造成成本提高。
发明内容
为了克服上述缺陷，本发明目的在于提供一种基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法，该方法制备的催化剂成本较低，活性分组均匀分布。
为了实现发明目的，本发明采取的技术方案如下：
一种基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法，其特征在于包括如下步骤：
1)将硬模板氧化铜纳米片与去离子水混合，质量比为1：1000—1：2000，然后在30-60r/min的转速下搅拌2-5h，使硬模板氧化铜纳米片充分的分散在去离子水中；
2)将溶液加热至50-80℃，在此温度下，在30-60r/min的转速下加入与硬模板氧化铜纳米片相同摩尔数的氯化锌，使其完全溶解在溶液中；
3)搅拌2-5h后，发生如下反应：
ZnCl2+CuO→CuCl2+ZnO。同时溶液的颜色从黑色逐渐变为灰色。然后通过过滤分离沉淀，并用过量去离子水清洗以去除未反应的锌离子；
4)用去离子水冲洗剩余的灰色样品，最后真空干燥并压碎，得到Cu/ZnO催化剂。
采用本方法可获得如下有益效果：获得催化活性和稳定性优良的Cu/ZnO纳米催化剂，并且所用原料药剂安全易得，用于二氧化碳催化加氢制甲醇，在较低温度425℃下表现出较高的催化反应活性，CO2转化率达到83％以上，CO产率达到31％以上，CH3OH产率达到52％以上，可用于绿色环保新能源的开发与应用。
具体实施方式
下面结合具体实施例进行说明：
实施例1
1.将800mg硬模板氧化铜纳米片与800ml去离子水混合，然后在30r/min的转速下搅拌2h，使硬模板氧化铜纳米片充分的分散在去离子水中。
2.将溶液加热至50℃，在此温度下，在30r/min的转速下加入与硬模板氧化铜纳米片相同摩尔数的氯化锌，使其完全溶解在溶液中。
3.搅拌2h后，发生如下反应：
ZnCl2+CuO→CuCl2+ZnO。同时溶液的颜色从黑色逐渐变为灰色。然后通过过滤分离沉淀，并用过量去离子水清洗以去除未反应的锌离子。
4.用去离子水冲洗剩余的灰色样品，最后真空干燥并压碎，得到氧化铁催化剂。
材料在较低温度425℃下表现出较高的催化反应活性，CO2转化率83.6％，CO产率31.2％，CH3OH产率52.4％，可用于绿色环保新能源的开发与应用。
实施例2
1.将500mg硬模板氧化铜纳米片与500ml去离子水混合，然后在50r/min的转速下搅拌3h，使硬模板氧化铜纳米片充分的分散在去离子水中。
2.将溶液加热至40℃，在此温度下，在40r/min的转速下加入与硬模板氧化铜纳米片相同摩尔数的氯化锌，使其完全溶解在溶液中。
3.搅拌3h后，发生如下反应：
ZnCl2+CuO→CuCl2+ZnO。同时溶液的颜色从黑色逐渐变为灰色。然后通过过滤分离沉淀，并用过量去离子水清洗以去除未反应的锌离子。
4.用去离子水冲洗剩余的灰色样品，最后真空干燥并压碎，得到氧化铁催化剂。
材料在较低温度425℃下表现出较高的催化反应活性，CO2转化率83.8％，CO产率31.6％，CH3OH产率52.2％，可用于绿色环保新能源的开发与应用。
实施例3
1.将1200mg硬模板氧化铜纳米片与1200ml去离子水混合，然后在60r/min的转速下搅拌5h，使硬模板氧化铜纳米片充分的分散在去离子水中。
2.将溶液加热至80℃，在此温度下，在60r/min的转速下加入与硬模板氧化铜纳米片相同摩尔数的氯化锌，使其完全溶解在溶液中。
3.搅拌5h后，发生如下反应：
ZnCl2+CuO→CuCl2+ZnO。同时溶液的颜色从黑色逐渐变为灰色。然后通过过滤分离沉淀，并用过量去离子水清洗以去除未反应的锌离子。
4.用去离子水冲洗剩余的灰色样品，最后真空干燥并压碎，得到氧化铁催化剂。
材料在较低温度425℃下表现出较高的催化反应活性，CO2转化率83.2％，CO产率31.4％，CH3OH产率52.3％，可用于绿色环保新能源的开发与应用。
Claims (1)
1.一种基于硬模板氧化铜纳米片合成Cu/ZnO催化剂的方法，其特征在于包括如下步骤：
1)将硬模板氧化铜纳米片与去离子水混合，质量比为1：1000—1：2000，然后在30-60r/min的转速下搅拌2-5h，使硬模板氧化铜纳米片充分的分散在去离子水中；
2)将溶液加热至50-80℃，在此温度下，在30-60r/min的转速下加入与硬模板氧化铜纳米片相同摩尔数的氯化锌，使其完全溶解在溶液中；
3)搅拌2-5h后，发生如下反应：
ZnCl2+CuO→CuCl2+ZnO；同时溶液的颜色从黑色逐渐变为灰色，然后通过过滤分离沉淀，并用过量去离子水清洗以去除未反应的锌离子；
4)用去离子水冲洗剩余的灰色样品，最后真空干燥并压碎，得到Cu/ZnO催化剂。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390640A (zh) * | 2002-07-30 | 2003-01-15 | 复旦大学 | 一种合成甲醇及二甲醚的纳米铜锌铝催化剂及其制备方法 |
| CN107043319A (zh) * | 2016-02-05 | 2017-08-15 | 株式会社模范 | 制备甲醇的方法 |
| CN107185543A (zh) * | 2017-06-05 | 2017-09-22 | 衢州学院 | 一种用于二氧化碳加氢合成甲醇的催化剂及其制备与应用 |
| CN107952437A (zh) * | 2017-11-09 | 2018-04-24 | 华南理工大学 | 用于二氧化碳加氢合成甲醇的Cu/二氧化钛纳米片催化剂及其制备方法 |
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- 2020-04-30 CN CN202010364012.8A patent/CN111545209A/zh active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390640A (zh) * | 2002-07-30 | 2003-01-15 | 复旦大学 | 一种合成甲醇及二甲醚的纳米铜锌铝催化剂及其制备方法 |
| CN107043319A (zh) * | 2016-02-05 | 2017-08-15 | 株式会社模范 | 制备甲醇的方法 |
| CN107185543A (zh) * | 2017-06-05 | 2017-09-22 | 衢州学院 | 一种用于二氧化碳加氢合成甲醇的催化剂及其制备与应用 |
| CN107952437A (zh) * | 2017-11-09 | 2018-04-24 | 华南理工大学 | 用于二氧化碳加氢合成甲醇的Cu/二氧化钛纳米片催化剂及其制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 王伊强等: "《普通化学》", 30 June 2003, 中国农业出版社 * |
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Application publication date: 20200818 |