CN107970950B - Method for regenerating catalyst for preparing propylene by propane dehydrogenation - Google Patents
Method for regenerating catalyst for preparing propylene by propane dehydrogenation Download PDFInfo
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- CN107970950B CN107970950B CN201610922060.8A CN201610922060A CN107970950B CN 107970950 B CN107970950 B CN 107970950B CN 201610922060 A CN201610922060 A CN 201610922060A CN 107970950 B CN107970950 B CN 107970950B
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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
- B01J23/90—Regeneration or reactivation
- B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
- C07C5/327—Formation of non-aromatic carbon-to-carbon double bonds only
- C07C5/333—Catalytic processes
- C07C5/3335—Catalytic processes with metals
- C07C5/3337—Catalytic processes with metals of the platinum group
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- 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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- 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
- Y02P20/584—Recycling of catalysts
Abstract
The invention relates to a method for regenerating a catalyst for preparing propylene by propane dehydrogenation, which belongs to the technical field of industrial catalysis and comprises the following steps: a) removing carbon deposition on the surface of the catalyst by an online scorching method; b) treating the catalyst by on-line air calcination; c) reducing the catalyst by on-line hydrogen calcination; d) adding carbon auxiliary agent on the surface of the catalyst by a method of on-line carbon growth. The method adopts staged charcoal burning treatment to prevent the active components of the catalyst from sintering due to temperature runaway in the charcoal burning process. The catalyst is carbonized by mixing hydrogen with carbon-containing substances in the reduction activation process, so that the reaction performance of the catalyst can be effectively improved, and the dehydrogenation selectivity and stability are improved.
Description
Technical Field
The invention relates to the technical field of industrial catalysis, in particular to a method for regenerating a catalyst for preparing propylene by propane dehydrogenation.
Background
Propane is an important organic chemical raw material and is widely applied to chemical products such as polypropylene, polyacrylonitrile, propylene oxide, acetone and the like. Currently, propylene is mainly derived from the catalytic cracking process of naphtha steam cracking for ethylene production and petroleum refining. However, in recent years, with the large-scale application of shale gas in the united states, the raw material of an ethylene cracking plant is shifted from high-price naphtha to cheap ethane, resulting in a great reduction in the amount of propylene as a byproduct; a large amount of propane is byproduct in the American shale gas, and the propylene with higher added value is obtained in a high-selectivity way by a propane catalytic dehydrogenation method, so that the method has important research significance. Currently, the propane dehydrogenation technology in the world is already commercialized by the Oleflex process of UOP and the Catofin process of LUMMUS. The propane dehydrogenation devices built at home and abroad or under construction are from the two processes.
The platinum catalyst is a common active metal for catalyzing alkane dehydrogenation, and has high catalytic dehydrogenation reaction activity. However, the active metal tends to rapidly decrease the reactivity in the reaction atmosphere due to the surface carbon deposition of the catalytically active sites. Thus requiring frequent regeneration of the catalyst. The development of the catalyst is simple and easy to implement, the catalytic performance is high, and the catalyst with high stability has important significance.
CN104107704A discloses a regeneration method for improving the stability of a catalyst by staged carbon burning, redispersion, reducibility and sulfur supplement, which effectively improves the regeneration efficiency of the catalyst and reduces the occurrence of side reactions.
CN104923258A discloses a method for treating deactivated catalyst by CO, treating the deactivated catalyst in a mixed atmosphere of low-carbon oxygen-containing hydrocarbon and HCl, and finally burning carbon in low-concentration oxygen to regenerate the deactivated catalyst, so that loss and aggregation of active centers of the catalyst are avoided.
CN104084218A discloses a method for regenerating platinum alkane dehydrogenation catalyst by burning charcoal in stages, soaking in chloride aqueous solution, then roasting in air, and finally reducing by hydrogen.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a method for regenerating a catalyst for preparing propylene by propane dehydrogenation. The industrial platinum catalyst regeneration method is to re-disperse the platinum particles with high activity components through the oxidation process, thereby restoring the catalytic activity. The research finds that the carbonization treatment is carried out after the processes of carbon burning, oxidation and reduction, namely, the hydrogen and the carbon source are mixed in the reduction process of the catalyst, so that the reaction performance of the catalyst can be effectively improved, and the dehydrogenation selectivity and stability are improved.
The method for regenerating the catalyst for preparing propylene by propane dehydrogenation mainly comprises the following steps:
a) removing carbon deposition on the surface of the catalyst by an online scorching method; and (3) analyzing the burning tail gas by adopting a staged burning method and adopting online analysis equipment to regulate and control the burning process.
b) Treating the catalyst by on-line air calcination;
c) reducing the catalyst by on-line hydrogen calcination;
d) adding carbon auxiliary agent on the surface of the catalyst by a method of on-line carbon growth. In particular, the catalyst may be treated in-line by a carbonaceous gas.
The process of the present application is applicable to reactors commonly used in the art, such as a fixed bed reactor, a fluidized bed reactor. Wherein the content of the first and second substances,
the online coking method adopted in the step a) comprises the steps of analyzing the concentrations of carbon oxides and oxygen in the coking tail gas online; adjusting the content of air in the coking atmosphere in the reaction furnace according to the concentration of carbon oxides in the coking tail gas, and adjusting the temperature in the reaction furnace; wherein the carbon oxide is at least one selected from carbon dioxide and carbon monoxide.
Specifically, the concentration of oxygen in the coking tail gas in percentage by mass is controlled within the range of 0-20% during the coking period; the adjustment is based on the concentration of carbon monoxide and carbon dioxide in the tail gas, wherein the total mass percentage concentration of the carbon monoxide and the carbon dioxide is not more than 5%.
In the burning process, the burning parameters of the reaction furnace are adjusted under the following conditions:
1) the mass percentage concentration of the carbon oxide in the coke-burning tail gas (the sum of the mass percentage concentrations of carbon dioxide and carbon monoxide) is lower than 1%, and when the mass percentage concentration of the carbon oxide in the coke-burning tail gas is continuously reduced, the proportion of air is increased, and the proportion of nitrogen is reduced; in particular, the gas ratio can be changed at a speed of 2.5% first gear.
2) And when the mass percentage concentration of the carbon oxides in the coking tail gas (the sum of the molar percentage concentrations of carbon dioxide and carbon monoxide is lower than 1 percent and the concentrations of carbon monoxide and carbon dioxide in the coking tail gas are kept stable, the ratio of air to nitrogen is kept, and the temperature of the furnace tube is gradually increased. The temperature may be raised, for example, at a rate of, for example, 2.5 ℃ or 5 ℃.
In the burning process, the temperature of a catalyst bed layer in a furnace tube of the reaction furnace is controlled between 480 and 600 ℃.
When the mass percentage concentration of the carbon oxide is higher than 1%, the ratio of nitrogen to air is kept constant, and when the mass percentage concentration of the carbon oxide is reduced to 1%, the above adjustment is performed.
The regulation principle is that the proportion of nitrogen and air is firstly regulated, and then the temperature is regulated. The temperature in the furnace tube of the catalyst filling layer is monitored in the adjusting process, temperature runaway is prevented, the concentrations of carbon dioxide, carbon monoxide and oxygen in tail gas are monitored simultaneously, the combustion condition of coke is known, and the air quantity during the coke burning, the temperature of the furnace tube and the coke burning time of each step are adjusted according to the online analysis result.
The on-line analysis is infrared on-line analysis by using an infrared on-line analyzer. The detection probe of the infrared analyzer can be arranged at a gas outlet channel of the reaction furnace for detection. The time required by the scorching process can be controlled within 2 hours and can also be controlled within 1 hour.
The on-line coke-burning step of the invention can be used for quickly removing carbon on the surface of the propane and butane dehydrogenation catalyst. The process of the invention is primarily suitable for catalysts containing carbon promoters, such as Pt-Sn-C/Al2O3A catalyst. In the method of the present invention, the standard for the end of the coke-burning process is performed on the basis that the concentration of carbon-oxygen compounds in the dry gas of the coke-burning off-gas is less than 0.5%. The on-line coking step combines the on-line analysis of normal position, and the concentration of carbon dioxide, carbon monoxide and oxygen in the real-time supervision burning tail gas to use this as the operating condition of regulation and control burning process, it is more directly perceived reliable on the burning technology operating condition, and operating method is also very convenient.
And the step b) comprises roasting the catalyst under the condition of flowing air at the temperature of 500-700 ℃, wherein the roasting time is 1-4 hours.
And the step c) comprises roasting the catalyst under the condition of flowing hydrogen at the temperature of 400-600 ℃, wherein the roasting time is 1-4 hours.
Said step d) comprising in flowing H2And C2H4In a mixed atmosphere of (A), wherein H2And C2H4The volume ratio of (A) to (B) is 1: 1-1: 30, the roasting temperature is 300-500 ℃, and the roasting time is 3-30 minutes.
Compared with the prior art, the method adopts staged charcoal burning treatment, and simultaneously adopts an online analysis technology to optimally control the charcoal burning process, so as to prevent the active components of the catalyst from sintering caused by temperature runaway in the charcoal burning process. After the catalyst is oxidized and reduced, hydrogen and carbon-containing substances are mixed, and the catalyst is carbonized, so that the reaction performance of the catalyst can be effectively improved, and the dehydrogenation selectivity and stability are improved.
Detailed Description
The present invention will be further described with reference to the following examples. However, the present invention is not limited to the examples. The following% contents are all mass% contents unless otherwise specified. The infrared analyzer used was an MRU infrared analyzer. Example 1
The dehydrogenation reaction was carried out using a catalyst comprising alumina as a carrier and a platinum group metal as a main active component (the mass content of platinum in the catalyst was 0.2%, the mass content of Sn was 1.5%, the mass content of potassium was 1.5%, and the mass content of carbon was 0.05%. the preparation method was the preparation method in CN105396582A, see example 3 for details). Firstly, harsher experimental conditions are adopted to reduce the reaction activity. At 600 deg.C for 600h-1Reacting for 1h under pure propane (99.9%) atmosphere, heating to 610 ℃, and simultaneously increasing the volume space velocity to 2400h-1Reacting for 4h, and reducing to 600h-1And detecting the activity of the final reaction stage under the reaction condition of 600 ℃ for 1 h. At 600h-1Cooling to 480 ℃ under the condition of nitrogen, keeping the temperature stable, and adjusting the flow of nitrogen to volume space velocity of 6000h-1The temperature of the catalyst bed is kept to be 480 ℃ stably. The space velocity of nitrogen is reduced to 5400h-1Simultaneously controlling the air to be 600h-1(ii) a The on-line carbon dioxide concentration was monitored (in this example, CO was not detected, and therefore, the concentration of the carbon-oxygen compound was CO2When the concentration of the carbon dioxide is lower than 1 percent, the volume space velocity of the nitrogen is continuously reduced to 4500h-1Raising the air space velocity to 1500h-1The carbon dioxide concentration increases; continuously monitoring the concentration of the carbon dioxide in the online analysis, and reducing the space velocity of the nitrogen to 3000h when the concentration of the carbon dioxide is lower than 1 percent again-1To raise the air space velocity to3000h-1The carbon dioxide concentration increases; continuously monitoring the concentration of the carbon dioxide for on-line analysis, closing the nitrogen when the concentration of the carbon dioxide is lower than 1 percent again, and increasing the airspeed of the air to 6000h-1. The conditions are maintained until the carbon dioxide concentration is less than 0.5% and the coke burning is finished after the carbon dioxide concentration is stable.
Keeping the air atmosphere, and reducing the volume air speed to 800h-1The temperature of the reaction furnace was raised to 600 ℃ within 20min and maintained for 2 h. Switching to a hydrogen atmosphere with a volume space velocity of 800h-1Keeping for 1h, cooling to 500 deg.C within 30min, and keeping for 2 h. Maintaining the hydrogen flow rate, at a hydrogen to ethylene volume ratio of 1:1 for 15min in a mixed atmosphere. The ethylene atmosphere was turned off and the temperature was reduced in a hydrogen atmosphere.
At 600 ℃ for 600h-1The results of the evaluation of the reaction of the procatalyst and the regenerated catalyst after 1 hour of reaction with pure propane (99.9%) are shown in Table 1:
TABLE 1 regenerated catalyst evaluation results
| Conversion (%) | Selectivity (%) | |
| Original catalyst | 39.10 | 95.17 |
| First round of regeneration | 40.80 | 95.59 |
| Second round of regeneration | 40.58 | 95.56 |
| Third round of regeneration | 40.36 | 95.49 |
From the above results, it can be seen that the treatment by the method of the present application can effectively improve the reaction performance of the catalyst, and simultaneously improve the dehydrogenation selectivity and stability.
Claims (9)
1. A method for regenerating a catalyst for preparing propylene by propane dehydrogenation is characterized by comprising the following steps:
a) removing carbon deposition on the surface of the catalyst by an online scorching method;
b) treating the catalyst by on-line air calcination;
c) reducing the catalyst by on-line hydrogen calcination;
d) adding a carbon auxiliary agent on the surface of the catalyst by an on-line carbon growth method;
the online coking method in the step a) comprises the steps of analyzing the concentrations of carbon oxides and oxygen in the coking tail gas online; adjusting the content of air in the coking atmosphere in the reaction furnace according to the concentration of carbon oxides in the coking tail gas, and adjusting the temperature in the reaction furnace;
the mass percentage concentration range of oxygen in the tail gas in the coking period is 0-20%; the adjustment is based on the concentration of carbon monoxide and carbon dioxide in the tail gas, wherein the total mass percentage concentration of the carbon monoxide and the carbon dioxide is not more than 5%;
in the burning process, the burning parameters of the reaction furnace are adjusted under the following conditions:
1) the mass percentage concentration of carbon oxide in the coke-burning tail gas is lower than 1%, and when the mass percentage concentration is continuously reduced, the proportion of air is increased, and the proportion of nitrogen is reduced;
2) and when the mass percentage concentration of the carbon oxide in the coking tail gas is lower than 1%, and the concentration of the carbon monoxide and the concentration of the carbon dioxide in the coking tail gas are kept stable, the ratio of air to nitrogen is kept, and the temperature of the furnace tube is gradually increased.
2. The method for regenerating a catalyst for the dehydrogenation of propane to propylene according to claim 1, wherein: the in-line coking method in the step a), wherein the oxide of carbon is selected from at least one of carbon dioxide and carbon monoxide.
3. The method according to any one of claims 1 to 2, wherein: in the burning process, the temperature of a catalyst bed layer in a furnace tube of the reaction furnace is controlled between 480 and 600 ℃.
4. The method according to any one of claims 1 to 2, wherein: the time required for the scorch process is within 2 hours.
5. The method of claim 4, wherein: the time required for the scorch process is within 1 hour.
6. The method according to any one of claims 1 to 2, wherein: and the step b) comprises roasting the catalyst under the condition of flowing air at the temperature of 500-700 ℃, wherein the roasting time is 1-4 hours.
7. The method according to any one of claims 1 to 2, wherein: and the step c) comprises roasting the catalyst under the condition of flowing hydrogen at the temperature of 400-600 ℃, wherein the roasting time is 1-4 hours.
8. The method according to any one of claims 1 to 2, wherein: said step d) comprising in flowing H2And C2H4In a mixed atmosphere of (A), wherein H2And C2H4The volume ratio of (A) to (B) is 1: 1-1: 30, the roasting temperature is 300-500 ℃, and the roasting time is 3-30 minutes.
9. The method according to any one of claims 1 to 2, wherein: the online scorching is performed by utilizing an infrared online analyzer for online scorching analysis; and a detection probe of the infrared online analyzer is arranged at a gas outlet of the reaction furnace.
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| CN109499623A (en) * | 2018-10-30 | 2019-03-22 | 沈阳石蜡化工有限公司 | A kind of processing method of propylene acid oxidation catalysis coking |
| CN114425458A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Activation method of sulfur-poisoned light paraffin isomerization catalyst |
| CN114425394A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Regeneration method of inactivated light alkane isomerization catalyst |
| US20220126281A1 (en) * | 2021-06-30 | 2022-04-28 | Uop Llc | Process for regenerating a dehydrogenation catalyst |
| CN115612519B (en) * | 2022-10-28 | 2023-12-29 | 西南化工研究设计院有限公司 | Regeneration method and system of moving bed low-carbon alkane dehydrogenation catalyst |
| CN116444254A (en) * | 2023-04-23 | 2023-07-18 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing chrome corundum lightweight aggregate by using propane dehydrogenation dead catalyst |
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| JPS57132548A (en) * | 1981-02-09 | 1982-08-16 | Nippon Oil Co Ltd | Method for regeneration of catalyst containing palladium |
| CN1541140A (en) * | 2000-12-04 | 2004-10-27 | �����ɷ� | Regeneration of dehydrogenation catalyst |
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