CN114984998A - Catalyst with KIT-6 as carrier and preparation method and application thereof - Google Patents
Catalyst with KIT-6 as carrier and preparation method and application thereof Download PDFInfo
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- CN114984998A CN114984998A CN202210782824.3A CN202210782824A CN114984998A CN 114984998 A CN114984998 A CN 114984998A CN 202210782824 A CN202210782824 A CN 202210782824A CN 114984998 A CN114984998 A CN 114984998A
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0341—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0333—Iron group metals or copper
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/035—Microporous crystalline materials not having base exchange properties, such as silica polymorphs, e.g. silicalites
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/035—Microporous crystalline materials not having base exchange properties, such as silica polymorphs, e.g. silicalites
- B01J29/0352—Microporous crystalline materials not having base exchange properties, such as silica polymorphs, e.g. silicalites containing iron group metals, noble metals or copper
- B01J29/0356—Iron group metals or copper
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
- B01J29/045—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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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
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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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
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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
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- 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
A catalyst with KIT-6 as a carrier is prepared by taking a mesoporous molecular sieve KIT-6 as a carrier, taking Ga as an active component, taking at least one of Li, Na, K, Rb, Mg and Ca as an auxiliary agent 1, taking at least one of Mn, Ni, Zn, Co and La as an auxiliary agent 2, taking 0.1-5.0% of the weight of the carrier as an active component in terms of elements, taking 0.1-3% of the weight of the carrier as an auxiliary agent 1 in terms of elements and taking 0.1-3% of the weight of the carrier as an auxiliary agent 2 in terms of elements, synthesizing the catalyst by adopting a one-step hydrothermal method, and loading the active component, the auxiliary agent 1 and the auxiliary agent 2 on the carrier KIT-6 in the hydrothermal synthesis. The catalyst of the invention semi-surrounds the active component gallium and other elements in the carrier, the distribution of the active component on the carrier is more dispersed, which is beneficial to improving the activity of the catalyst, meanwhile, the active component is introduced when the carrier is crystallized, so the active component can enter the framework of the carrier or presents a semi-surrounding state, which is beneficial to inhibiting the generation of carbon deposition and prolonging the service cycle of the catalyst.
Description
Technical Field
The present invention relates to a catalyst preparation method.
Background
In recent 20 years, the research on mesoporous molecular sieves has been greatly developed, and the mesoporous molecular sieves have the advantages of large specific surface area, adjustable pore size, high thermal stability and high hydrothermal stability, so that the mesoporous molecular sieves have wide application in the field of catalysts.
The mesoporous silica molecular sieve KIT-6 is a three-dimensional cubic ordered mesoporous structure, has a large pore diameter, is adjustable between 4 and 12 nanometers, and is relatively easy to synthesize. The three-dimensional cubic pore canal special for KIT-6 is very suitable for loading active species like an open mesoporous template, and the active species can be uniformly dispersed in the whole pore canal without forming agglomerated large particles, so that the three-dimensional cubic pore canal is very suitable for serving as a carrier of a catalyst.
The dehydrogenation of propane to propylene is an important source of propylene, and the reaction is carried out under high-temperature and low-pressure conditions, and currently, the platinum-based catalyst and the chromium-based catalyst are most commonly used, but the defects of the two types of catalysts are obvious: the platinum catalyst has high cost and high requirement on propane raw materials; chromium catalysts have poor stability, are very easy to deposit carbon and deactivate, are toxic and easily pollute the environment. Therefore, the development of a catalyst with high activity, good stability and no toxicity is the key point of the existing propane dehydrogenation for preparing propylene.
Disclosure of Invention
Aiming at the problems of the prior industrial catalyst, the invention provides a catalyst taking a mesoporous silica molecular sieve KIT-6 with high activity, good stability and no toxicity as a carrier, a preparation method thereof and application thereof in the reaction of preparing propylene by propane dehydrogenation.
The technical scheme adopted by the invention for realizing the purpose is as follows: a catalyst with KIT-6 as a carrier, a mesoporous molecular sieve KIT-6 as a carrier, an active component Ga, an auxiliary agent 1 at least one of Li, Na, K, Rb, Mg and Ca, an auxiliary agent 2 at least one of Mn, Ni, Zn, Co and La, wherein the active component accounts for 0.1-5.0% of the weight of the carrier in terms of elements, the auxiliary agent 1 accounts for 0.1-3% of the weight of the carrier in terms of elements, and the auxiliary agent 2 accounts for 0.1-3% of the weight of the carrier in terms of elements.
The catalyst is synthesized by adopting a one-step hydrothermal method, and the active component, the auxiliary agent 1 and the auxiliary agent 2 are loaded on the carrier KIT-6 in the hydrothermal synthesis.
The method comprises the following steps:
1) dissolving a template agent P123 in dilute hydrochloric acid, adding n-butanol, and stirring to form a mixed solution;
2) slowly adding a silicon source into the mixed solution, and stirring for 2-6 hours;
3) adding a solution of an active component, an auxiliary agent 1 and an auxiliary agent 2 into a mixed solution containing a silicon source, and performing ultrasonic treatment on the mixed solution to obtain solid powder after hydrothermal treatment;
4) filtering, washing and drying the obtained solid powder;
5) and calcining the dried solid powder at 500-600 ℃ for 2-6 hours, removing the template agent P123, and granulating the obtained powder into particles of 20-40 meshes to obtain the catalyst.
The silicon source is at least one of ethyl orthosilicate and silica sol, the raw material of the active component is gallium nitrate, the raw material of the auxiliary 1 is at least one of lithium nitrate, sodium carbonate, potassium carbonate, rubidium carbonate, magnesium nitrate and calcium nitrate, and the raw material of the auxiliary 2 is at least one of manganese nitrate, nickel nitrate, zinc nitrate, cobalt nitrate and lanthanum nitrate.
The P123: n-butanol: hydrochloric acid: SiO 2 2 : active components: auxiliary agent 1: and (3) auxiliary agent 2: the water mass ratio is 1: 0.5-1.5: 1.5-2.5: 0.5-1: 0.0005 to 0.05: 0.0005 to 0.03: 0.0005 to 0.03: 30-40, and the stirring time is 2-6 hours.
The ultrasonic time is 20-40 minutes, the hydrothermal treatment temperature is 90-120 ℃, the hydrothermal treatment time is 12-36 hours, the drying temperature is 80-120, and the drying time is 2-10 hours.
A catalyst prepared by the method according to any one of claims 2 to 6.
Use of the catalyst of claim 7 in the dehydrogenation of propane to propylene.
The catalyst of the invention semi-surrounds the active component gallium and other elements in the carrier, the distribution of the active component on the carrier is more dispersed, which is beneficial to improving the activity of the catalyst, meanwhile, the active component is introduced when the carrier is crystallized, so the active component can enter the framework of the carrier or is in a semi-surrounding state, which is beneficial to inhibiting the generation of carbon deposition and prolonging the service cycle of the catalyst.
Drawings
Fig. 1 is an XRD spectrum of catalyst B5.
Fig. 2 is a plot of the propane dehydrogenation performance of catalyst a 1.
Fig. 3 is a graph of the propane dehydrogenation performance of catalyst B1.
Detailed Description
The present invention is further described with reference to the following specific examples, but the scope of the present invention is not limited by the examples, and those skilled in the art who have the above-mentioned disclosure will still be able to make some insubstantial modifications and adaptations to the present invention.
The catalytic reaction conditions are as follows: a fixed bed reactor; reaction temperature: 600 ℃; reaction pressure: normal pressure; the reaction gas composition is: propane: nitrogen gas 9: 1; the gas flow rate was 800 ml/min.
Catalyst loading: 12 ml.
Comparative example 1
Adding 20 g of KIT-6 molecular sieve into 40 ml of a mixed solution of nitric acid with the pH value of 2 (the gallium content is 2%), potassium carbonate (the potassium content is 0.5%) and manganese nitrate (the manganese content is 0.25%), carrying out ultrasonic treatment for 30 minutes, heating at 80 ℃ to evaporate to dry, roasting at 600 ℃ for 3 hours, and granulating the obtained powder into 20-40-mesh particles to obtain the catalyst A1. The results of the catalytic reaction are shown in Table 1. The reaction results are shown in FIG. 2 as a function of time.
Example 1
60 g of template agent P123 is added into dilute hydrochloric acid consisting of 1.8L of deionized water and 96 ml of concentrated hydrochloric acid, the mixture is stirred for 1 hour to be completely dissolved to form colorless transparent solution, and then 60 g of n-butyl alcohol is added to the mixture and stirred for 1 hour to form colorless transparent solution. 125 g of tetraethoxysilane is slowly dropped into the above solution, and stirred for 2 hours. Under the condition of stirring, adding 35 ml of nitric acid-gallium (the gallium content is 4%), 17.5 ml of potassium carbonate (the potassium content is 2%), 17.5 ml of manganese nitrate (the manganese content is 1%) in sequence, fully stirring and uniformly mixing the mixed solution, performing ultrasonic treatment for 30 minutes, performing hydrothermal treatment for 24 hours at 100 ℃, repeatedly washing the filtered powder with deionized water, drying for 5 hours at 100 ℃, roasting for 3 hours at 600 ℃, removing the template agent P123, and granulating the powder into 20-40-mesh particles to obtain the catalyst B1. The reaction results are shown in FIG. 3 as a function of time.
Example 2
60 g of template agent P123 is added into dilute hydrochloric acid consisting of 2.1L of deionized water and 120 ml of concentrated hydrochloric acid, the mixture is stirred for 1 hour to be completely dissolved to form colorless transparent solution, and then 30 g of n-butyl alcohol is added to the mixture and stirred for 1 hour to form colorless transparent solution. 166 g of ethyl orthosilicate were slowly dropped into the above solution, and stirred for 4 hours. Under the condition of stirring, adding 35 ml of nitric acid-gallium (the gallium content is 4%), 23 ml of lithium nitrate (the lithium content is 2%), 23 ml of nickel nitrate (the nickel content is 2%) in sequence, fully stirring and uniformly mixing the mixed solution, performing ultrasonic treatment for 20 minutes, performing hydrothermal treatment for 36 hours at 90 ℃, repeatedly washing the filtered powder with deionized water, drying for 10 hours at 80 ℃, roasting for 6 hours at 500 ℃, removing the template agent P123, and granulating the obtained powder into 20-40-mesh particles to obtain the catalyst B2.
Example 3
60 g of template agent P123 was added to dilute hydrochloric acid consisting of 2.4L of deionized water and 150 mL of concentrated hydrochloric acid, and stirred for 1 hour to be completely dissolved to form a colorless transparent solution, and then 90 g of n-butanol was added and stirred for 1 hour to form a colorless transparent solution. 208 g of tetraethoxysilane was slowly dropped into the above solution, and stirred for 6 hours. Under the condition of stirring, adding 29 ml of nitric acid-gallium (the gallium content is 4%), 29 ml of sodium carbonate (the sodium content is 2%), 29 ml of zinc nitrate (the zinc content is 2%) in sequence, fully stirring and uniformly mixing the mixed solution, performing ultrasonic treatment for 40 minutes, performing hydrothermal treatment for 12 hours at 120 ℃, repeatedly washing the filtered powder with deionized water, drying for 2 hours at 120 ℃, roasting for 4 hours at 550 ℃, removing the template agent P123, and granulating the powder into 20-40-mesh particles to obtain the catalyst B3.
Example 4
60 g of template agent P123 is added into dilute hydrochloric acid consisting of 1.8L of deionized water and 96 ml of concentrated hydrochloric acid, the mixture is stirred for 1 hour to be completely dissolved to form colorless transparent solution, and then 60 g of n-butyl alcohol is added to the mixture and stirred for 1 hour to form colorless transparent solution. 104 g of tetraethoxysilane was slowly dropped into the above solution, and stirred for 2 hours. Under the condition of stirring, adding 36 ml of gallium nitrate (the gallium content is 4%), 14.5 ml of rubidium carbonate (the rubidium content is 2%) and 14.5 ml of cobalt nitrate (the cobalt content is 1%) in sequence, fully stirring and uniformly mixing the mixed solution, performing ultrasonic treatment for 30 minutes, performing hydrothermal treatment for 12 hours at 120 ℃, repeatedly washing the filtered powder with deionized water, drying for 5 hours at 100 ℃, roasting for 2 hours at 600 ℃, removing a template agent P123, and granulating the powder into 20-40-mesh particles to obtain a catalyst B4.
Example 5
60 g of template agent P123 is added into dilute hydrochloric acid consisting of 2.1L of deionized water and 120 ml of concentrated hydrochloric acid, the mixture is stirred for 1 hour to be completely dissolved to form colorless transparent solution, and then 90 g of n-butyl alcohol is added to the mixture and stirred for 1 hour to form colorless transparent solution. 208 g of tetraethoxysilane was slowly dropped into the above solution, and stirred for 5 hours. Under the stirring condition, 5.8 milliliters of gallium nitrate (the gallium content is 1%), 5.8 milliliters of magnesium nitrate (the magnesium content is 1%) and 5.8 milliliters of lanthanum nitrate (the lanthanum content is 1%) are sequentially added, the mixed solution is fully stirred and uniformly mixed, then is subjected to ultrasonic treatment for 30 minutes, then is subjected to hydrothermal treatment for 18 hours at 110 ℃, the filtered powder is repeatedly washed by deionized water, is dried for 8 hours at 90 ℃, then is roasted for 2 hours at 600 ℃, the template agent P123 is removed, and the obtained powder is granulated into 20-40-mesh particles, so that the catalyst B5 is obtained. The XRD spectrum of the catalyst is shown in figure 1.
Example 6
60 g of template agent P123 is added into dilute hydrochloric acid consisting of 2.4L of deionized water and 150 ml of concentrated hydrochloric acid, the mixture is stirred for 1 hour to be completely dissolved to form colorless transparent solution, and then 60 g of n-butyl alcohol is added to the mixture and stirred for 1 hour to form colorless transparent solution. 187 g of tetraethyl orthosilicate were slowly added dropwise to the solution and stirred for 3 hours. Under the condition of stirring, 13 milliliters of gallium nitrate, 5.2 milliliters of calcium nitrate and 5.2 milliliters of manganese nitrate are sequentially added, wherein the content of gallium is 4 percent, the content of calcium is 2 percent, the content of manganese is 1 percent, the mixed solution is fully stirred, uniformly mixed, subjected to ultrasonic treatment for 30 minutes, subjected to hydrothermal treatment for 12 hours at 120 ℃, filtered, repeatedly washed by deionized water, dried for 5 hours at 100 ℃, roasted for 5 hours at 550 ℃, template agent P123 is removed, and the obtained powder is granulated into 20-40-mesh particles, so that the catalyst B6 is obtained.
TABLE 1
| Numbering | Catalyst and process for preparing same | Conversion (%) | Selectivity (%) | Yield (%) |
| Comparative example 1 | A1 | 40.5 | 93.2 | 37.7 |
| Example 1 | B1 | 45.6 | 94.0 | 42.9 |
| Example 2 | B2 | 39.8 | 93.2 | 37.1 |
| Example 3 | B3 | 35.6 | 94.5 | 33.6 |
| Example 4 | B4 | 51.2 | 94.9 | 48.6 |
| Example 5 | B5 | 29.6 | 80.8 | 23.9 |
| Example 6 | B6 | 32.5 | 87.2 | 28.3 |
While the invention has been described with reference to exemplary embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (8)
1. A catalyst taking KIT-6 as a carrier is characterized in that: the mesoporous molecular sieve KIT-6 is a carrier, the active component is Ga, the auxiliary agent 1 is at least one of Li, Na, K, Rb, Mg and Ca, the auxiliary agent 2 is at least one of Mn, Ni, Zn, Co and La, the active component accounts for 0.1-5.0% of the weight of the carrier by element, the auxiliary agent 1 accounts for 0.1-3% of the weight of the carrier by element, and the auxiliary agent 2 accounts for 0.1-3% of the weight of the carrier by element.
2. A method of preparing a KIT-6 supported catalyst of claim 1, characterized in that: the catalyst is synthesized by adopting a one-step hydrothermal method, and the active component, the auxiliary agent 1 and the auxiliary agent 2 are loaded on the carrier KIT-6 in the hydrothermal synthesis.
3. The method for preparing a KIT-6 supported catalyst according to claim 2, wherein the method comprises the following steps: the method comprises the following steps:
1) dissolving a template agent P123 in dilute hydrochloric acid, adding n-butanol, and stirring to form a mixed solution;
2) slowly adding a silicon source into the mixed solution, and stirring for 2-6 hours;
3) adding a solution of an active component, an auxiliary agent 1 and an auxiliary agent 2 into a mixed solution containing a silicon source, and performing ultrasonic treatment on the mixed solution to obtain solid powder after hydrothermal treatment;
4) filtering, washing and drying the obtained solid powder;
5) and calcining the dried solid powder at 500-600 ℃ for 2-6 hours, removing the template agent P123, and granulating the obtained powder into particles of 20-40 meshes to obtain the catalyst.
4. The method for preparing a KIT-6 supported catalyst according to claim 3, wherein the method comprises the following steps: the silicon source is at least one of ethyl orthosilicate and silica sol, the raw material of the active component is gallium nitrate, the raw material of the auxiliary 1 is at least one of lithium nitrate, sodium carbonate, potassium carbonate, rubidium carbonate, magnesium nitrate and calcium nitrate, and the raw material of the auxiliary 2 is at least one of manganese nitrate, nickel nitrate, zinc nitrate, cobalt nitrate and lanthanum nitrate.
5. A method of preparing the KIT-6 supported catalyst of claim 1, wherein the method comprises the steps of: the P123: n-butanol: hydrochloric acid: SiO 2 2 : active components: auxiliary agent 1: auxiliary agent 2: the water mass ratio is 1: 0.5-1.5: 1.5-2.5: 0.5-1: 0.0005 to 0.05: 0.0005 to 0.03: 0.0005 to 0.03: 30-40, and the stirring time is 2-6 hours.
6. The method for preparing a KIT-6 supported catalyst according to claim 1, wherein the method comprises the following steps: the ultrasonic time is 20-40 minutes, the hydrothermal treatment temperature is 90-120 ℃, the hydrothermal treatment time is 12-36 hours, the drying temperature is 80-120, and the drying time is 2-10 hours.
7. A catalyst prepared by the method according to any one of claims 2 to 6.
8. Use of the catalyst of claim 7 in the dehydrogenation of propane to propylene.
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Cited By (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115805097A (en) * | 2022-12-01 | 2023-03-17 | 中触媒新材料股份有限公司 | Large-grain Zn @ Silicalite-1 low-carbon alkane dehydrogenation catalyst and preparation method thereof |
| CN115805097B (en) * | 2022-12-01 | 2024-03-01 | 中触媒新材料股份有限公司 | Large-grain Zn@Silicalite-1 low-carbon alkane dehydrogenation catalyst and preparation method thereof |
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Application publication date: 20220902 |