CN112973749B - Catalyst, preparation method and application - Google Patents
Catalyst, preparation method and application Download PDFInfo
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- CN112973749B CN112973749B CN201911282392.4A CN201911282392A CN112973749B CN 112973749 B CN112973749 B CN 112973749B CN 201911282392 A CN201911282392 A CN 201911282392A CN 112973749 B CN112973749 B CN 112973749B
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
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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
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Abstract
A catalyst comprising a chromium-based composite; the chromium-based composite comprises a chromium-based body and an additive; the chromium-based main body comprises at least one of metal chromium, chromium nitride and amino chromium; the additive comprises a compound consisting of an element A and an element B; the element A is an alkali metal element or an alkaline earth metal element; the element B is at least one of N element and H element. The invention is used as a novel catalytic material, and shows good catalytic activity in the synthesis ammonia reaction.
Description
Technical Field
The application relates to a catalyst, a preparation method and application thereof, and belongs to the technical field of chemical materials.
Background
Ammonia is a basic raw material for producing important chemical products such as chemical fertilizers, nitric acid, plastics and the like, and is a hydrogen energy carrier with potential application prospects. The synthetic ammonia is related to grains, energy and environment, and has very important significance in industry. The catalytic conversion of nitrogen and hydrogen over transition metals is the primary means of industrial ammonia synthesis, and the current industrial process mainly used is the Haber-Bosch process. The reaction conditions of the process need high temperature and high pressure (the iron-based catalyst is 350-. For decades, the catalyst commonly used in industrial ammonia synthesis reaction is iron-based catalyst, and only a small part of devices adopt ruthenium-based catalyst with mild working conditions. The effective utilization of some renewable energy sources in the ammonia synthesis process and the development of new ammonia synthesis catalyst systems with low temperature, low pressure and high efficiency are still important research subjects at present.
Very little research has been done on non-iron (ruthenium) based catalysts, particularly chromium based catalysts, for ammonia synthesis. Early research results show that the ammonia synthesis activity of chromium-based catalysts is low, and at present, few researches on chromium-based ammonia synthesis catalysts and transition metal nitrogen hydrides are carried out. The mechanism of action of catalytic ammonia synthesis on transition metals is not well understood. How to modulate the composition and structure of the catalyst to realize low-temperature low-pressure high-efficiency ammonia synthesis still needs further research.
Disclosure of Invention
According to one aspect of the present application, a catalyst is provided, which is a new catalytic material with a good activity for synthesizing ammonia, in which a hydride/nitride of an alkali metal or an alkaline earth metal is added to chromium, a transition metal.
A catalyst is provided that includes a chromium-based composite; the chromium-based composite comprises a chromium-based body and an additive; the chromium-based body comprises at least one of metal chromium, chromium nitride and amino chromium; the additive comprises a compound consisting of an element A and an element B; the element A is an alkali metal element or an alkaline earth metal element; the element B is at least one of N element and H element.
Optionally, the compound consisting of the element A and the element B is selected from at least one compound having a chemical formula shown in formula I;
A(NH2)n3in the formula I, the valence of an element H is + 1;
n3 represents the valence of element A, and n3 has a value in the range of 1 or 2.
Optionally, the mass ratio of the chromium-based body to the additive is 1000:1 to 1: 500.
Optionally, the mass ratio of the chromium-based body to the additive is 200: 1-1: 100.
Optionally, the alkali metal element comprises at least one of Li, Na, K, Rb, Cs; the alkaline earth metal element comprises at least one of Mg, Ca, Sr and Ba.
Optionally, the chromium nitride comprises CrN, Cr2At least one of N; the amino chromium comprises Cr (NH)2)3、Cr2(NH2)3At least one of (1).
Optionally, the catalyst further comprises a support; the chromium-based composite is supported on the carrier; the carrier comprises any one of oxide, nitride and carbon material; the oxide includes Li2O、MgO、CaO、SrO、BaO、Al2O3、SiO2、TiO2、ZrO2、CeO2、Na2O、K2At least one of O; the above-mentionedThe nitride comprises BN, Si3N4、Mg3N2、Ca3N2And AlN.
Optionally, the carrier is present in the catalyst in an amount of 20 to 99 wt%.
The present application also provides a process for preparing the above catalyst, said process comprising at least: and reacting a mixture containing a chromium source and an element A source in liquid ammonia in an inert atmosphere to obtain the catalyst.
Optionally, the chromium source comprises at least one of an amino chromium, a chromium nitride, a chromium chloride; the element A source comprises at least one of a simple substance of the element A, a hydride of the element A, an amino compound of the element A and a nitrogen-hydrogen compound of the element A.
Optionally, the method comprises at least:
(1) in an inactive atmosphere, reacting a mixture containing a chromium source and an element A source in liquid ammonia to obtain a catalyst precursor;
(2) and mixing the catalyst precursor with a raw material containing a carrier source, and performing ball milling to obtain the catalyst.
Optionally, the support source comprises at least one of a hydroxide, a carbonate, a nitrate, an oxide, a nitride, a carbon material.
Preferably, the hydroxide comprises LiOH, Mg (OH)2、Ca(OH)2、Sr(OH)2、Ba(OH)2、Al(OH)3、Si(OH)4、Ti(OH)4、Zr(OH)4、Ce(OH)4At least one of NaOH and KOH;
the carbonate comprises Li2CO3、MgCO3、CaCO3、SrCO3、BaCO3、Al2(CO3)3、Si(CO3)2、Zr(CO3)2、Ce2(CO3)3、Na2CO3、K2CO3At least one of;
the nitrate comprises LiNO3、Mg(NO3)2、Ca(NO3)2、Sr(NO3)2、Ba(NO3)2、Al(NO3)3、Ti(NO3)4、Zr(NO3)4、Ce(NO3)3、NaNO3、KNO3At least one of (1).
Optionally, the molar ratio of the chromium source to the element A source is 1:100 to 100: 1; the reaction conditions are as follows: the reaction temperature is 20-300 ℃; the reaction time is 0.1-48 h.
Optionally, the rotation speed of the ball mill is 50-300 r/min.
In another aspect of the present application, there is also provided a method for synthesizing ammonia, the method at least comprising: reacting a mixed gas containing nitrogen and hydrogen in the presence of a catalyst to prepare ammonia; the catalyst is selected from any one of the catalysts described above and the catalysts prepared according to the above preparation method.
Optionally, the volume ratio of nitrogen to ammonia in the mixed gas is 100: 1-1: 100; the gas flow rate of the mixed gas is 1.2-2.4L/h.
Optionally, the reaction conditions are: the reaction temperature is 100-500 ℃; the reaction pressure is 1-30 atm.
Optionally, the upper limit of the reaction temperature is selected from the group consisting of 500 ℃, 450 ℃, 400 ℃, 350 ℃, 300 ℃, 250 ℃, 200 ℃, 150 ℃, and the lower limit is selected from the group consisting of 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, 450 ℃.
The beneficial effects that this application can produce include: the catalyst provided by the application is prepared by adding hydride/nitride of alkali metal or alkaline earth metal into transition metal chromium, is a novel catalytic material and has good synthetic ammonia activity.
Drawings
FIG. 1 shows CrN and Cr (NH)2)3Raman spectrum of the catalyst precursor and the catalyst in example 1 after actual catalytic reaction;
FIG. 2 is a powder XRD spectrum of the [ BaCrNH ] catalyst of example 1 after hydrogenation and after higher temperature reaction;
FIG. 3 shows [ BaCrNH ] in example 1]Catalyst in N2/H2(1/3) the reactivity of the synthetic ammonia and the reactivity of CrN/LiH (molar ratio 1: 5) are compared;
FIG. 4 shows CrN/Ba (NH) in example 22)2(molar ratio 1:2) catalyst in N2/H2(1/3) reaction activity of synthetic ammonia, and comparison with the activity of CrN/LiH (molar ratio 1: 5).
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
Example 1
In an argon glove box, accurately weighing chromium amino (Cr (NH)2)3)0.0456g, and 0.1249g of metal barium (Ba) were placed in a self-made stainless steel reactor. And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, pumping out liquid ammonia to obtain Cr (NH)2)3/Ba(NH2)2(molar ratio 1:2) catalyst.
Accurately weighing Cr (NH) in an argon glove box2)3/Ba(NH2)2(molar ratio 1:2) 0.0300g of catalyst was placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. The test results are shown in fig. 3. Cr (NH)2)3/Ba(NH2)2Can be hydrogenated in situ under the reaction condition to generate [ BaCrNH ]]Species, at 175 degrees, have shown some ammonia synthesis activity (ammonia formation rate of about 352mol g)cat -1h-1) And the ammonia production rate gradually increases with increasing temperature; at 300 ℃, the generation rate of ammonia can reach 6864umol gcat -1h-1. Is nearly twice that of the reported Cr/LiH (molar ratio 1: 2).
For raw material amino chromium (Cr (NH)2)3) Catalyst precursor Cr (b)NH2)3/Ba(NH2)2And Raman spectrum characterization is carried out on a sample after actual catalytic reaction of the catalyst, and the result is compared with that of CrN, as shown in figure 1, the obvious Cr-N vibration is found in the sample and is about 800cm < -1 >, and the Raman vibration cannot be observed due to the fact that pure CrN has no Raman activity.
The catalyst is hydrogenated at 200 ℃ and 300 ℃ and then a sample is subjected to XRD characterization and is compared with CrN and BaH2The ball-milled samples are compared, and the result is shown in figure 2, the sample after 200 ℃ hydrogenation basically has no obvious diffraction peak, and the sample after 300 ℃ hydrogenation has some samples which can be classified as BaH2Shows that the catalyst may be amorphous at lower temperatures and may react with hydrogen to form BaH at higher temperatures2。
Example 2
0.0336g of chromium nitride (CrN) and 0.1395g of metal barium (Ba) are accurately weighed in an argon glove box and placed in a self-made stainless steel reactor. And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, liquid ammonia is pumped out to obtain CrN/Ba (NH)2)2(molar ratio 1:2) catalyst.
Accurately weighing CrN/Ba (NH) in an argon glove box2)2(molar ratio 1:2) 0.0300g of catalyst was placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. The test results are shown in fig. 4. CrN and Ba (NH)2)2In-situ generation of BaCrNH under reaction conditions with a small probability]Species, testing found that the rate of ammonia production gradually increased with increasing temperature; at 300 ℃, CrN/Ba (NH)2)2The generation rate of ammonia can reach 1190umol gcat -1h-1。
Example 3
In an argon glove box, accurately weighing chromium amino (Cr (NH)2)3)0.0775g and 0.0217g of metallic lithium (Li) are placed in a self-made stainless steel reactorIn (1). And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, liquid ammonia is pumped out to obtain Cr (NH)2)3/LiNH2(molar ratio 1:4) catalyst.
Accurately weighing Cr (NH) in an argon glove box2)3/LiNH2(molar ratio 1:4) 0.0300g of catalyst was placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. Cr (NH)2)3/LiNH2Can generate [ LiCrNH ] through in-situ hydrogenation under reaction conditions]The generation rate of ammonia can reach 4583umol g at 300 DEG Ccat -1h-1。
Example 4
In an argon glove box, 0.0875g of chromium amide (CrN) and 0.0371g of metal lithium (Li) are accurately weighed and placed in a self-made stainless steel reactor. And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, liquid ammonia is pumped out to obtain CrN/LiNH2(molar ratio 1:4) catalyst.
Accurately weighing CrN/LiNH in an argon glove box2(molar ratio 1:4) 0.0300g of catalyst was placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. CrN and LiNH2In situ generation of [ LiCrNH ] with a small probability under the reaction conditions]Species of the species. At 300 ℃, the generation rate of ammonia can reach 2864umol gcat -1h-1。
Example 5
In an argon glove box, accurately weighing chromium amino (Cr (NH)2)3)0.1254g, and 0.1956g of metal potassium (K), were placed in a self-made stainless steel reactor. And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, liquid ammonia is pumped out to obtain Cr (NH)2)3/KNH2(molar ratio 1:4) catalyst.
Accurately weighing Cr (NH) in an argon glove box2)3/KNH2(molar ratio 1:4) 0.0300g of catalyst was placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. Cr (NH)2)3/KNH2Can generate [ KCrNH ] by in-situ hydrogenation under the reaction condition]The generation rate of ammonia can reach 5124umol g at 300 DEG Ccat -1h-1。
Example 6
In an argon glove box, 0.0876g of chromium nitride (CrN) and 0.2071g of metal potassium (K) are accurately weighed and placed in a self-made stainless steel reactor. And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, liquid ammonia is pumped out to obtain CrN/KNH2(molar ratio 1:4) catalyst.
Accurately weighing CrN/KNH in an argon glove box2(molar ratio 1:4) 0.0300g of catalyst was placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. CrN and KNH2Has small probability of generating [ KCrNH ] in situ under reaction conditions]Species of the species. At 300 deg.C, the generation rate of ammonia can reach 3081umol gcat -1h-1。
Example 7
In an argon glove box, accurately weighing chromium amino (Cr (NH)2)3)0.0523g, and barium hydride (BaH)2)0.1455g, placed in a self-made stainless steel reactor. And vacuumizing the reactor, cooling, introducing liquid ammonia, and immersing the reactant. After shaking for 2 hours, liquid ammonia was removed, and Cr (NH) similar to that in example 1 was obtained2)3/Ba(NH2)2(molar ratio 1:2) catalyst.
Accurately weighing Cr (NH) in an argon glove box2)3/Ba(NH2)2(molar ratio 1)2) 0.0300g of catalyst, placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. Cr (NH)2)3/Ba(NH2)2Can be hydrogenated in situ under the reaction condition to generate [ BaCrNH ]]The generation rate of ammonia can reach 4464umol g at 300 DEG Ccat -1h-1Slightly lower than the catalyst prepared by using the amino chromium and the metal barium as precursors.
Example 8
Cr (NH) was prepared as in example 12)3/Ba(NH2)2As a catalyst precursor, and then accurately weighing Cr (NH) in an argon glove box2)3/Ba(NH2)20.0312g of catalyst (molar ratio 1:2) and 0.1230g of magnesium oxide (MgO) carrier were placed in a ball mill pot and ball milled at 200rppm revolutions for 12 hours at normal temperature under an argon atmosphere. Obtaining the magnesium oxide loaded Cr (NH)2)3/Ba(NH2)2Catalyst (Cr (NH)2)3/Ba(NH2)2-MgO)。
Accurately weighing Cr (NH) in an argon glove box2)3/Ba(NH2)20.0300g of catalyst-MgO (Cr/Ba molar ratio 1:2), placed in a fixed bed stainless steel reactor. Sample is in N2/H2(1/3) heating the atmosphere to the required reaction temperature, controlling the pressure to be 10atm, controlling the flow rate of the reaction gas to be 1.8L/h, and sampling and analyzing after at least 2 hours. Cr (NH)2)3/Ba(NH2)2The MgO can be hydrogenated in situ under the reaction condition to generate [ BaCrNH ]]MgO species, ammonia production rate up to 2334umol g at 300 DEGcat -1h-1。
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (16)
1. A catalyst, wherein the catalyst comprises a chromium-based composite;
the chromium-based composite comprises a chromium-based body and an additive;
the chromium-based body comprises an amino chromium;
the additive comprises a compound consisting of an element A and an element B;
the element A is an alkali metal element or an alkaline earth metal element;
the element B is at least one of N element and H element;
the amino chromium comprises Cr (NH)2)3、Cr2(NH2)3At least one of;
the method at least comprises the following steps: and reacting a mixture containing a chromium source and an element A source in liquid ammonia in an inert atmosphere to obtain the catalyst.
2. The catalyst according to claim 1, wherein the compound consisting of the element a and the element B is at least one selected from the group consisting of compounds having the chemical formula shown in formula i;
A（NH2）n3 formula I
Wherein, in the formula I, the valence of the H element is + 1;
n3 represents the valence of element A, and n3 has a value in the range of 1 or 2.
3. The catalyst of claim 1, wherein the mass ratio of the chromium-based body to the additive is 1000:1 to 1: 500.
4. The catalyst of claim 1, wherein the mass ratio of the chromium-based body to the additive is 200:1 to 1: 100.
5. The catalyst of claim 1, wherein the alkali metal element comprises at least one of Li, Na, K, Rb, Cs; the alkaline earth metal element comprises at least one of Mg, Ca, Sr and Ba.
6. The catalyst of claim 1, further comprising a support; the chromium-based composite is supported on the carrier; the carrier comprises any one of oxide, nitride and carbon material; the oxide includes Li2O、MgO、CaO、SrO、BaO、Al2O3、SiO2、TiO2、ZrO2、CeO2、Na2O、K2At least one of O; the nitride comprises BN and Si3N4、Mg3N2、Ca3N2And AlN.
7. The catalyst according to claim 6, wherein the content of the carrier in the catalyst is 20 to 99 wt%.
8. The catalyst of claim 1, wherein the chromium source is an amino chromium;
the element A source comprises at least one of element A simple substance, element A hydride and element A nitrogen-hydrogen compound.
9. Catalyst according to claim 1, characterized in that said process comprises at least:
(1) in an inactive atmosphere, reacting a mixture containing a chromium source and an element A source in liquid ammonia to obtain a catalyst precursor;
(2) and mixing the catalyst precursor with a raw material containing a carrier source, and performing ball milling to obtain the catalyst.
10. The catalyst of claim 9, wherein the support source comprises at least one of a hydroxide, a carbonate, a nitrate, an oxide, a nitride, a carbon material.
11. The catalyst of claim 10, wherein the hydroxide comprises LiOH, Mg (OH)2、Ca(OH)2、Sr(OH)2、Ba(OH)2、Al(OH)3、Si(OH)4、Ti(OH)4、Zr(OH)4、Ce(OH)4At least one of NaOH and KOH;
the carbonate comprises Li2CO3、MgCO3、CaCO3、SrCO3、BaCO3、Al2(CO3)3、Si(CO3)2、Zr(CO3)2、Ce2(CO3)3、Na2CO3、K2CO3At least one of;
the nitrate comprises LiNO3、Mg(NO3)2、Ca(NO3)2、Sr(NO3)2、Ba(NO3)2、Al(NO3)3、Ti(NO3)4、Zr(NO3)4、Ce(NO3)3、NaNO3、KNO3At least one of (1).
12. The catalyst of claim 9, wherein the molar ratio of the chromium source to the source of element a is from 1:100 to 100: 1;
the reaction conditions are as follows: the reaction temperature is 20-300 ℃; the reaction time is 0.1-48 h.
13. The catalyst of claim 9, wherein the ball milling speed is 50-300 rpm.
14. A method for synthesizing ammonia, characterized in that it comprises at least: reacting a mixed gas containing nitrogen and hydrogen in the presence of a catalyst to prepare ammonia;
the catalyst is selected from the catalysts of any one of claims 1 to 13.
15. The method according to claim 14, wherein the volume ratio of the nitrogen to the hydrogen in the mixed gas is 100: 1-1: 100; the gas flow rate of the mixed gas is 1.2-2.4L/h.
16. The method according to claim 14, wherein the reaction conditions are: the reaction temperature is 100-500 ℃; the reaction pressure is 1-30 atm.
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| WO2008153826A2 (en) * | 2007-05-31 | 2008-12-18 | Corning Incorporated | Catalyst for hydrogen production by autothermal reforming, method of making same and use thereof |
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