CN114349591A - High-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide - Google Patents
High-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide Download PDFInfo
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- CN114349591A CN114349591A CN202011085748.8A CN202011085748A CN114349591A CN 114349591 A CN114349591 A CN 114349591A CN 202011085748 A CN202011085748 A CN 202011085748A CN 114349591 A CN114349591 A CN 114349591A
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- carbon dioxide
- catalyst
- ethane
- reaction
- ethylene
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 239000003054 catalyst Substances 0.000 title claims abstract description 77
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 54
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 54
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000005977 Ethylene Substances 0.000 title claims abstract description 43
- 230000001590 oxidative effect Effects 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000004005 microsphere Substances 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 10
- 238000005470 impregnation Methods 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 10
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000012495 reaction gas Substances 0.000 description 18
- 238000006356 dehydrogenation reaction Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
Abstract
The invention belongs to the technical field of chemical catalysts, and relates to a high-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide. The catalyst takes silicon dioxide microspheres as a carrier and vanadium as an active component, and the content of the active component is 0.5-3 wt%. The preparation method is that an ammonium metavanadate solution is introduced into the silicon dioxide microsphere powder by using an impregnation method, and the silicon dioxide microsphere powder is dried, formed into small balls and then roasted to obtain the catalyst. The invention greatly reduces the reaction temperature for preparing ethylene from ethane and reduces the reaction energy consumption; the catalyst has simple preparation method and low cost, and has higher ethane conversion rate and ethylene selectivity in the reaction of preparing ethylene by oxidizing ethane with carbon dioxide.
Description
Technical Field
The invention belongs to the technical field of chemical catalysts, and particularly relates to a high-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide.
Background
The ethylene industry is the core industry of the petrochemical industry, and ethylene products account for over 70 percent of petrochemical products. Ethylene yield is one of the important indicators for the state of the petrochemical industry, and the production thereof is mainly from the cracking process of naphtha or light oil at present. With the increasing shortage of petroleum resources, the dehydrogenation of ethane, which is abundant and cheap, to prepare ethylene has attracted more and more attention.
Although the preparation of ethylene by ethane dehydrogenation is industrialized, the reaction temperature is basically over 850 ℃ due to the limitation of thermodynamic equilibrium conversion rate, and the energy consumption is particularly high. Therefore, the mild oxidant carbon dioxide is introduced into the reaction system to form a feasible experimental scheme, the deep oxidation of ethane is not generated, and the selectivity of the product ethylene can be ensured; meanwhile, partial energy is provided for dehydrogenation endothermic reaction, the reaction temperature is reduced, and the current environment-friendly requirement is met.
At present, Cr types of catalysts for preparing ethylene by oxidizing ethane with carbon dioxide are more, and although a silicon oxide supported Cr catalyst has better activity and selectivity, the stability of the catalyst is very poor; the zeolite-supported Cr type catalyst has high activity under the condition of high silica-alumina ratio, but the selectivity of ethylene is low, and the cost is greatly improved. Therefore, the cheap high-efficiency catalyst is an important research direction in the field of preparing ethylene by oxidizing ethane and dehydrogenating carbon dioxide at present.
Disclosure of Invention
The invention aims to provide a catalyst which is used for preparing ethylene by oxidizing ethane with carbon dioxide, and has the advantages of low price, high ethane conversion rate and high ethylene selectivity.
The invention provides a high-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide, which is characterized in that silicon dioxide microspheres are used as a carrier, vanadium is used as an active component, and the content of the active component is 0.5-3 wt%. The pore volume of the silicon dioxide microspheres is 0.5-0.8 mL/g, and the average pore diameter is 13-18 nm.
Generally, the silica microsphere carrier is prepared from water, ammonia water, ethanol and tetraethoxysilane under an alkaline condition, and is dried and roasted to prepare powder.
Further, the silicon dioxide microsphere carrier is prepared from water, ammonia water, ethanol and ethyl orthosilicate under an alkaline condition, and is dried and roasted to prepare powder.
Further, an impregnation method is adopted to introduce an ammonium metavanadate solution into the powder, and the powder is dried at 50-70 ℃ and then molded.
Further, drying and forming into small balls with the diameter of 1-3 mm.
Further, the formed pellets are roasted to prepare the catalyst.
Further, the roasting temperature is 600-700 ℃.
Furthermore, the pore volume of the silica microspheres is 0.52-0.74 mL/g.
Furthermore, the average pore diameter of the silicon dioxide microspheres is 13.15-17.75 nm.
The catalyst provided by the invention is used for the reaction of preparing ethylene by ethane dehydrogenation under the atmosphere of carbon dioxide, and comprises the following specific steps and conditions:
(1) activating the catalyst for 1-3 h in a carbon dioxide atmosphere at 600-700 ℃;
(2) the reaction pressure is 0.1-0.4 MPa; the reaction temperature is 600-700 ℃;
(3) the molar ratio of carbon dioxide to ethane in the reaction is 2: 1-4: 1.
The invention has the beneficial effects that: the invention greatly reduces the reaction temperature for preparing ethylene from ethane and reduces the reaction energy consumption; the catalyst has simple preparation method and low cost, and has higher ethane conversion rate and ethylene selectivity in the reaction of preparing ethylene by oxidizing ethane with carbon dioxide.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the invention is not limited thereto.
Example 1
Taking silica microspheres with pore volume of 0.52mL/g and average pore diameter of 15.45nm as a carrier, introducing 0.5wt% of vanadium component into the powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 50 ℃, forming into small balls with the diameter of 1mm, and roasting at 600 ℃ to obtain the catalyst 1 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 1 hour at 600 ℃ in the carbon dioxide atmosphere before reaction, then reaction gas is introduced at 600 ℃, the reaction pressure is 0.1MPa, and the reaction gas comprises the following components: 30mL/min ethane, 70mL/min carbon dioxide. Catalyst # 1 had an ethane conversion of 8.4% and an ethylene selectivity of 92.2%.
Example 2
Taking silica microspheres with pore volume of 0.74mL/g and average pore diameter of 16.25nm as a carrier, introducing 2.0wt% of vanadium component into powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 60 ℃, forming into small spheres with the diameter of 2mm, and roasting at 700 ℃ to obtain the catalyst 2 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 2 hours at 700 ℃ in the carbon dioxide atmosphere before reaction, then reaction gas is introduced at 700 ℃, the reaction pressure is 0.4MPa, and the reaction gas comprises the following components: 20mL/min ethane, 80mL/min carbon dioxide. Catalyst # 2 had an ethane conversion of 44.5% and an ethylene selectivity of 81.1%.
Example 3
Taking silica microspheres with pore volume of 0.63mL/g and average pore diameter of 17.75nm as a carrier, introducing 3.0wt% of vanadium component into the powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 70 ℃, forming into small balls with the diameter of 3mm, and roasting at 650 ℃ to obtain the catalyst 3 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 2 hours at 650 ℃ in the atmosphere of carbon dioxide before reaction, then reaction gas is introduced at 650 ℃, the reaction pressure is 0.3MPa, and the reaction gas comprises the following components: 25mL/min ethane, 75mL/min carbon dioxide. Catalyst # 3 had an ethane conversion of 35.8% and an ethylene selectivity of 82.6%.
Example 4
Taking silica microspheres with pore volume of 0.58mL/g and average pore diameter of 13.15nm as a carrier, introducing 1.5wt% of vanadium component into the powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 65 ℃, forming into small balls with diameter of 1mm, and roasting at 700 ℃ to obtain the catalyst 4 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 3 hours at 700 ℃ in the carbon dioxide atmosphere before reaction, then reaction gas is introduced at 700 ℃, the reaction pressure is 0.2MPa, and the reaction gas comprises the following components: 25mL/min ethane, 75mL/min carbon dioxide. Catalyst # 4 had an ethane conversion of 50.2% and an ethylene selectivity of 73.6%.
Example 5
Taking silica microspheres with pore volume of 0.55mL/g and average pore diameter of 15.45nm as a carrier, introducing 1.5wt% of vanadium component into the powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 65 ℃, forming into small spheres with the diameter of 1mm, and roasting at 700 ℃ to obtain the catalyst No. 5.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 3 hours at 700 ℃ in the carbon dioxide atmosphere before reaction, then reaction gas is introduced at 700 ℃, the reaction pressure is 0.2MPa, and the reaction gas comprises the following components: 25mL/min ethane, 75mL/min carbon dioxide. Catalyst # 4 had an ethane conversion of 48.3% and an ethylene selectivity of 70.2%.
Example 6
Taking silica microspheres with pore volume of 0.53mL/g and average pore diameter of 17.15nm as a carrier, introducing 2.5wt% of vanadium component into the powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 70 ℃, forming into small balls with the diameter of 2mm, and roasting at 650 ℃ to obtain the catalyst 6 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 3 hours at 650 ℃ in the atmosphere of carbon dioxide before reaction, then reaction gas is introduced at 650 ℃, the reaction pressure is 0.1MPa, and the reaction gas comprises the following components: 20mL/min ethane, 80mL/min carbon dioxide. Catalyst # 5 had an ethane conversion of 38.1% and an ethylene selectivity of 86.7%.
Example 7
Taking silica microspheres with pore volume of 0.70mL/g and average pore diameter of 15.35nm as a carrier, introducing 2.2wt% of vanadium component into powder by an ammonium metavanadate solution isovolumetric impregnation method, drying at 60 ℃, forming into small spheres with the diameter of 2mm, and roasting at 700 ℃ to obtain the catalyst 7 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 2 hours at 700 ℃ in the carbon dioxide atmosphere before reaction, then reaction gas is introduced at 700 ℃, the reaction pressure is 0.4MPa, and the reaction gas comprises the following components: 20mL/min ethane, 80mL/min carbon dioxide. Catalyst # 7 had an ethane conversion of 54.1% and an ethylene selectivity of 78.5%.
Comparative example 1
Drying the silica microspheres with pore volume of 0.53mL/g and average pore diameter of 17.15nm at 70 deg.C, molding into small spheres with diameter of 2mm, and calcining at 650 deg.C to obtain catalyst No. 6.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 3 hours at 650 ℃ in the atmosphere of carbon dioxide before reaction, then reaction gas is introduced at 650 ℃, the reaction pressure is 0.1MPa, and the reaction gas comprises the following components: 25mL/min ethane, 75mL/min carbon dioxide. Catalyst # 6 had an ethane conversion of 10.4% and an ethylene selectivity of 77.8%.
Comparative example 2
Taking silica microspheres with pore volume of 0.74mL/g and average pore diameter of 16.25nm as a carrier, drying at 60 ℃, forming into small spheres with the diameter of 2mm, and roasting at 700 ℃ to obtain the catalyst 7 #.
The ethane dehydrogenation activity of the above catalyst under a carbon dioxide atmosphere was measured on a fixed bed reactor. The specific reaction conditions are as follows: the catalyst dosage is 2mL, the catalyst is activated for 2 hours at 700 ℃ in the carbon dioxide atmosphere before reaction, then reaction gas is introduced at 700 ℃, the reaction pressure is 0.4MPa, and the reaction gas comprises the following components: 20mL/min ethane, 80mL/min carbon dioxide. Catalyst # 7 had an ethane conversion of 18.3% and an ethylene selectivity of 70.5%.
Claims (10)
1. A high-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide is characterized in that: the method is characterized in that silica microspheres are used as a carrier, vanadium is used as an active component, the content of the active component is 0.5-3 wt%, the pore volume of the silica microspheres is 0.5-0.8 mL/g, and the average pore diameter is 13-18 nm.
2. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 1, wherein: the silicon dioxide microsphere carrier is prepared by water, ammonia water, ethanol and tetraethoxysilane under an alkaline condition, and is dried and roasted to prepare powder.
3. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 2, wherein: the silicon dioxide microsphere carrier is prepared by water, ammonia water, ethanol and tetraethoxysilane under an alkaline condition, and is dried and roasted to prepare powder.
4. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 3, wherein: and introducing an ammonium metavanadate solution into the powder by adopting an impregnation method, drying at 50-70 ℃, and forming.
5. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 4, wherein: drying and forming into small balls with the diameter of 1-3 mm.
6. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 5, wherein: and roasting the formed pellets to obtain the catalyst.
7. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 6, wherein: the roasting temperature is 600-700 ℃.
8. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 1, wherein: the pore volume of the silica microspheres is 0.52-0.74 mL/g.
9. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 1, wherein: the average pore diameter of the silicon dioxide microspheres is 13.15-17.75 nm.
10. The high efficiency catalyst for producing ethylene by oxidizing ethane with carbon dioxide according to claim 1, wherein: the method is used for the reaction of preparing ethylene by oxidizing ethane with carbon dioxide, and comprises the following steps and conditions:
(1) activating the catalyst for 1-3 h in a carbon dioxide atmosphere at 600-700 ℃;
(2) the reaction pressure is 0.1-0.4 MPa; the reaction temperature is 600-700 ℃;
(3) the molar ratio of carbon dioxide to ethane in the reaction is 2: 1-4: 1.
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| CN202011085748.8A CN114349591A (en) | 2020-10-12 | 2020-10-12 | High-efficiency catalyst for preparing ethylene by oxidizing ethane with carbon dioxide |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224439A (en) * | 2003-01-27 | 2013-07-31 | 英国石油化学品有限公司 | Oxidation catalyst and its preparation |
| CN103979608A (en) * | 2014-05-22 | 2014-08-13 | 吉林大学 | Method for preparing hollow core-shell vanadium pentoxide microsphere |
| CN106563489A (en) * | 2016-10-28 | 2017-04-19 | 复旦大学 | Catalyst for preparing ethylene through ethane dehydrogenation under carbon dioxide atmosphere, and preparation method thereof |
| CN109382090A (en) * | 2017-08-08 | 2019-02-26 | 天津大学 | Molybdenum vanadium dual metal oxide catalyst and its application in low-carbon alkanes chemical chain dehydrogenation |
| CN109433257A (en) * | 2018-11-30 | 2019-03-08 | 大连理工大学 | A kind of catalyst of preparing ethene by oxidative dehydrogenation of ethane with carbon dioxide and preparation method thereof |
| CN110170333A (en) * | 2019-06-18 | 2019-08-27 | 西南化工研究设计院有限公司 | One kind is for ethane to ethylene catalyst under carbon dioxide atmosphere and preparation method thereof |
-
2020
- 2020-10-12 CN CN202011085748.8A patent/CN114349591A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224439A (en) * | 2003-01-27 | 2013-07-31 | 英国石油化学品有限公司 | Oxidation catalyst and its preparation |
| CN103979608A (en) * | 2014-05-22 | 2014-08-13 | 吉林大学 | Method for preparing hollow core-shell vanadium pentoxide microsphere |
| CN106563489A (en) * | 2016-10-28 | 2017-04-19 | 复旦大学 | Catalyst for preparing ethylene through ethane dehydrogenation under carbon dioxide atmosphere, and preparation method thereof |
| CN109382090A (en) * | 2017-08-08 | 2019-02-26 | 天津大学 | Molybdenum vanadium dual metal oxide catalyst and its application in low-carbon alkanes chemical chain dehydrogenation |
| CN109433257A (en) * | 2018-11-30 | 2019-03-08 | 大连理工大学 | A kind of catalyst of preparing ethene by oxidative dehydrogenation of ethane with carbon dioxide and preparation method thereof |
| CN110170333A (en) * | 2019-06-18 | 2019-08-27 | 西南化工研究设计院有限公司 | One kind is for ethane to ethylene catalyst under carbon dioxide atmosphere and preparation method thereof |
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