CN115430437A - Molybdenum salt heterogeneous carrier and preparation method and application thereof - Google Patents
Molybdenum salt heterogeneous carrier and preparation method and application thereof Download PDFInfo
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- CN115430437A CN115430437A CN202211138046.0A CN202211138046A CN115430437A CN 115430437 A CN115430437 A CN 115430437A CN 202211138046 A CN202211138046 A CN 202211138046A CN 115430437 A CN115430437 A CN 115430437A
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Abstract
The invention discloses a molybdenum salt heterogeneous carrier and a preparation method and application thereof, belonging to the technical field of material preparation and catalysis. Firstly, complexing molybdenum salt with an organic ligand to obtain a molybdenum salt precursor, and then calcining the molybdenum salt precursor to obtain the molybdenum salt heterogeneous carrier. The method creatively prepares the heterogeneous carrier based on the theory of interaction between strong and weak carriers, has extremely strong inhibiting effect on resisting two sintering modes of Ostwald ripening and particle aggregation and migration involved in the using process of the catalyst, not only can greatly improve the stability of the catalyst, but also can prolong the service life of the catalyst, thereby reducing the use cost of the catalyst. Has very strong guiding significance for actual production and life.
Description
Technical Field
The invention belongs to the technical field of material preparation and catalysis, and particularly relates to a molybdenum salt heterogeneous carrier and a preparation method and application thereof.
Background
In the field of catalysis, especially in the field of thermocatalysis, the stability of the catalyst has always been a problem for researchers. The catalyst has two sintering modes in the thermocatalytic process: one is sintering by Ostwald ripening and the other is sintering by aggregation and migration of particles. Both sintering methods reduce or even lose the catalytic activity of the catalyst. The reduction or deactivation of the catalyst activity in the actual production has a great influence on the industrial catalytic process.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the molybdenum salt heterogeneous carrier, and the preparation method and the application thereof, wherein the molybdenum salt heterogeneous carrier is simple and convenient to operate, the raw materials are easy to obtain, the cost is low, the energy consumption is low, and the prepared molybdenum salt heterogeneous carrier has extremely strong sintering resistance.
The invention is realized by the following technical scheme:
the invention discloses a preparation method of a molybdenum salt heterogeneous carrier, which comprises the following steps: step 1: molybdenum salt and an organic ligand are regulated by acid to generate a molybdenum salt precursor;
and 2, step: and (3) calcining the molybdenum salt precursor obtained in the step (1) to obtain the molybdenum salt heterogeneous carrier with multiple coexisting components.
Preferably, in step 1, the molybdenum salt is one or more of sodium molybdate, ammonium molybdate, molybdenum trichloride and molybdenum pentachloride.
Preferably, in step 1, the organic ligand is an organic amine or an organic alcohol.
Further preferably, the organic amine is methylamine, ethylamine, propylamine, butylamine, pentylamine, hexylamine, heptylamine or octylamine; the organic alcohol is methanol, ethanol, propanol, butanol or pentanol.
Preferably, in step 1, the acid is one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, and acetic acid.
Preferably, in step 1, the concentration of the acid is 1.0 to 5.0mol/L.
Preferably, in the step 2, the calcining temperature is 200-2000 ℃ and the calcining time is 6-12 h.
Preferably, the multicomponent coexisting molybdenum salt heterogeneous carrier obtained in step 2 comprises two or more of molybdenum carbide, molybdenum oxide, molybdenum nitride, molybdenum phosphide and molybdenum disulfide.
The invention also discloses the molybdenum salt heterogeneous carrier prepared by the preparation method.
The invention also discloses an application of the molybdenum salt heterogeneous carrier as a heterogeneous catalyst carrier.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the preparation method of the molybdenum salt heterogeneous carrier, the heterogeneous carrier is prepared under the guidance of the strong and weak carrier interaction theory, and the catalyst with strong carrier interaction can be subjected to Ostwald ripening in the catalyst process, so that the active structure of the catalyst is damaged, and the activity of the catalyst is greatly reduced; the interaction of weak carriers can cause particle aggregation and migration in the catalytic process, destroy the active structure of the catalyst and greatly reduce the activity of the catalyst. The catalyst with strong carrier interaction has good inhibition effect on particle aggregation and migration, while the catalyst with weak carrier interaction has inhibition effect on Ostwald ripening. Therefore, the heterogeneous carrier prepared by the method has two interaction functions, and has extremely strong inhibition effect on two sintering modes of Ostwald ripening and particle aggregation and migration involved in the using process of the catalyst. Firstly, molybdenum salt precursors are prepared through molybdenum salt and organic ligand water bath, and then the molybdenum salt heterogeneous carrier obtained by directly calcining the molybdenum salt precursors in situ overcomes the defects of the traditional catalyst in the aspect of anti-sintering performance, improves the stability of the catalyst, prolongs the service life and reduces the use cost of the catalyst. Meanwhile, the method for preparing the heterogeneous carrier by in-situ calcination overcomes the defects of complicated preparation steps and high energy consumption of the traditional catalyst, and has the advantages of low cost, simple operation process, easily obtained raw materials, rich storage and the like.
Furthermore, the molybdenum salt is sodium molybdate, ammonium molybdate, molybdenum trichloride and molybdenum pentachloride, and has the advantages of easily obtained raw materials, low cost, high active site and high selectivity.
Furthermore, organic amine or organic alcohol is adopted as the organic ligand, so that lone-pair electrons are easily given.
Further, the acid is one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid and acetic acid, and can promote the molybdenum salt to coordinate with the organic ligand.
Further, the concentration of the acid is 1.0 to 5.0mol/L, and the molybdenum salt and the organic ligand can be promoted to coordinate at a proper reaction rate.
Furthermore, the calcining temperature is 200-2000 ℃, the calcining time is 6-12 h, and the prepared heterogeneous carrier crystal form is more stable.
According to the molybdenum salt heterogeneous carrier prepared by the preparation method disclosed by the invention, strong and weak carriers formed by a multi-component structure interact with each other, so that the sintering resistance of the heterogeneous carrier is greatly improved, and the service life and the catalytic performance of a catalyst are prolonged.
The application of the molybdenum salt heterogeneous carrier disclosed by the invention as a heterogeneous catalyst carrier is based on the molybdenum salt heterogeneous carrier with two or more than two components of molybdenum carbide, molybdenum oxide, molybdenum nitride, molybdenum phosphide and molybdenum disulfide coexisting, the unique structure of the molybdenum salt heterogeneous carrier enables the heterogeneous carrier to have a strong catalytic action, other metal particles are loaded for catalysis, the catalytic performance of the catalyst is improved, the service life of the catalyst is prolonged, the catalytic range of the catalyst can be expanded, and more possibilities are provided for multi-field catalysis.
Drawings
FIG. 1 is an X-ray powder diffractometer (XRD) pattern of the molybdenum salt heterogeneous catalyst prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope (SEM-EDS) elemental analysis chart of the product obtained in example 1;
FIG. 3 is an X-ray powder diffractometer (XRD) pattern of the product obtained in example 1 before and after the catalysis.
Detailed Description
The invention will now be described in further detail with reference to the following figures and examples, which are given by way of illustration and not of limitation.
Example 1
Adding 1.2g of sodium molybdate and 1.1mL of methylamine into 60mL of deionized water, adding 1.0mol/L of dilute hydrochloric acid into the reaction solution until a large amount of white floccules are generated, filtering and drying to obtain molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 200 ℃ for 12 hours to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 2
Adding 2.4g of ammonium molybdate and 2.2mL of ethylamine into 60mL of deionized water, adding 1.2mol/L of dilute hydrochloric acid and dilute sulfuric acid into the reaction solution until a large amount of white floccules are generated, filtering and drying to obtain molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 300 ℃ for 11h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide, molybdenum carbide and molybdenum nitride.
Example 3
Adding 4.8g of molybdenum pentachloride and 4.4mL of propylamine into 60mL of deionized water, adding 1.8mol/L of dilute acetic acid, dilute nitric acid and dilute hydrochloric acid into the reaction solution until a large amount of white floccules are generated, filtering and drying to obtain molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 400 ℃ for 10h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide, molybdenum carbide and molybdenum nitride.
Example 4
9.6g of molybdenum trichloride and 2.2mL of butylamine are added into 60mL of deionized water, and 2.0mol/L of dilute formic acid and dilute nitric acid are added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 500 ℃ for 9h to obtain the molybdenum salt heterogeneous carrier with two components of molybdenum carbide and molybdenum nitride coexisting.
Example 5
9.6g of ammonium molybdate and 2.2mL of pentylamine were added to 60mL of deionized water, and 2.5mol/L of dilute phosphoric acid was added to the above reaction solution until a large amount of white flocs were formed. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 600 ℃ for 8h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum carbide, molybdenum nitride and molybdenum phosphide.
Example 6
2.4g of molybdenum trichloride and 2.2mL of hexylamine were added to 60mL of deionized water, and 3.0mol/L of dilute nitric acid was added to the above reaction solution until a large amount of white flocs were formed. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 700 ℃ for 7h to obtain the molybdenum salt heterogeneous carrier with two components of molybdenum carbide and molybdenum nitride coexisting.
Example 7
4.8g of molybdenum pentachloride and 2.2mL of heptylamine were added to 60mL of deionized water, and 1.5mol/L of dilute hydrochloric acid and dilute formic acid were added to the above reaction solution until a large amount of white flocs were formed. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 800 ℃ for 12h to obtain the molybdenum salt heterogeneous carrier with two components of molybdenum carbide and molybdenum nitride coexisting.
Example 8
3.6g of sodium molybdate, 1.2g of molybdenum pentachloride and 2.2mL of octylamine were added to 60mL of deionized water, and 3.5mol/L of dilute hydrochloric acid was added to the reaction solution until a large amount of white flocs were formed. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 900 ℃ for 11h to obtain the molybdenum salt heterogeneous carrier with two components of molybdenum carbide and molybdenum nitride coexisting.
Example 9
9.6g of ammonium molybdate, 4.8g of molybdenum trichloride and 2.2mL of methanol are added into 60mL of deionized water, and 4.0mol/L of dilute hydrochloric acid and dilute formic acid are added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 1000 ℃ for 10 hours to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 10
9.6g of ammonium molybdate, 1.2g of molybdenum trichloride and 2.2mL of ethanol were added to 60mL of deionized water, and 4.5mol/L of dilute hydrochloric acid was added to the above reaction solution until a large amount of white flocs were formed. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 1100 ℃ for 9h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 11
9.6g of ammonium molybdate, 1.2g of sodium molybdate, 2.4g of molybdenum trichloride and 2.2mL of propanol are added into 60mL of deionized water, and 5.0mol/L of dilute hydrochloric acid and dilute acetic acid are added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 1200 ℃ for 8h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 12
9.6g of ammonium molybdate, 1.2g of molybdenum trichloride, 3.6g of molybdenum pentachloride and 2.2mL of butanol are added into 60mL of deionized water, and 1.5mol/L of dilute hydrochloric acid is added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 1300 ℃ for 7h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide, molybdenum carbide and molybdenum nitride.
Example 13
9.6g of sodium molybdate, 2.4g of ammonium molybdate, 3.6g of molybdenum trichloride and 2.2mL of pentanol are added to 60mL of deionized water, and 2.0mol/L of dilute hydrochloric acid is added to the reaction solution until a large amount of white floc is generated. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 1400 ℃ for 6h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide, molybdenum carbide and molybdenum nitride.
Example 14
9.6g of ammonium molybdate, 1.2g of molybdenum pentachloride, 3.6g of sodium molybdate and 2.2mL of pentanol were added to 60mL of deionized water, and 2.5mol/L of dilute hydrochloric acid was added to the above reaction solution until a large amount of white flocs were formed. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 1500 ℃ for 7h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide, molybdenum carbide and molybdenum nitride.
Example 15
3.6g of molybdenum trichloride, 2.4g of ammonium molybdate, 3.6g of molybdenum pentachloride and 2.2mL of butanol are added into 60mL of deionized water, and 2.5mol/L of dilute hydrochloric acid is added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. And calcining the obtained molybdenum salt precursor powder at 1600 ℃ for 8 hours to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 16
2.4g of molybdenum trichloride, 3.6g of molybdenum pentachloride, 4.8g of sodium molybdate and 2.2mL of propanol are added into 60mL of deionized water, and 3.0mol/L of dilute hydrochloric acid is added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 1700 ℃ for 9h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 17
4.8g of molybdenum pentachloride, 4.8g of sodium molybdate, 9.6g of ammonium molybdate and 2.2mL of ethanol are added into 60mL of deionized water, and 2.0mol/L of dilute hydrochloric acid is added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 1800 ℃ for 10h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
Example 18
9.6g of molybdenum pentachloride, 1.2g of molybdenum trichloride, 2.4g of sodium molybdate and 2.2mL of methylamine are added into 60mL of deionized water, and 2.6mol/L of dilute hydrochloric acid is added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 1900 ℃ for 11h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide, molybdenum carbide and molybdenum nitride.
Example 19
4.8g of molybdenum pentachloride, 3.6g of molybdenum trichloride, 2.4g of ammonium molybdate, 1.2g of ammonium molybdate and 2.2mL of propylamine are added into 60mL of deionized water, and 3.0mol/L of dilute hydrochloric acid is added into the reaction solution until a large amount of white floccules are generated. Filtering and drying to obtain the molybdenum salt precursor powder. Calcining the obtained molybdenum salt precursor powder at 2000 ℃ for 12h to obtain the molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
FIG. 1 is an X-ray powder diffractometer (XRD) pattern of the molybdenum salt heterogeneous catalyst prepared in example 1, from which it can be seen that XRD diffraction peaks of the prepared product correspond to those of MoC (PDF # 15-0457), mo standard card 2 N(PDF#25-1366)、Mo 2 O (PDF # 76-1807).
FIG. 2 is a scanning electron microscope (SEM-EDS) elemental analysis chart of the product of the present invention, from which it can be seen that the EDS elemental analysis of the prepared product is a composite of four elements of Mo-C-N-O.
The combination of FIG. 1 and FIG. 2 shows that the product obtained in example 1 is a molybdenum salt heterogeneous carrier with the coexistence of three components of molybdenum oxide-molybdenum carbide-molybdenum nitride.
FIG. 3 is X-ray powder diffractometer (XRD) pattern before and after catalysis of the product of the present invention, and it can be seen from the pattern that the heterogeneous carrier has no obvious crystal form change before and after catalysis, and has stable structure.
It should be noted that the above description is only a part of the embodiments of the present invention, and equivalent variations of the system described in the present invention are included in the protection scope of the present invention. Persons skilled in the art to which this invention pertains may substitute similar alternatives for the specific embodiments described, all without departing from the scope of the invention as defined by the claims.
Claims (10)
1. The preparation method of the molybdenum salt heterogeneous carrier is characterized by comprising the following steps:
step 1: molybdenum salt and an organic ligand are regulated by acid to generate a molybdenum salt precursor;
step 2: and (3) calcining the molybdenum salt precursor obtained in the step (1) to obtain a multi-component coexisting molybdenum salt heterogeneous carrier.
2. The method for preparing a molybdenum salt heterogeneous carrier according to claim 1, wherein in the step 1, the molybdenum salt is one or more of sodium molybdate, ammonium molybdate, molybdenum trichloride and molybdenum pentachloride.
3. The method for preparing a molybdenum salt heterocarrier according to claim 1, wherein in step 1, the organic ligand is organic amine or organic alcohol.
4. The method for preparing a molybdenum salt heterocarrier according to claim 3, wherein the organic amine is methylamine, ethylamine, propylamine, butylamine, pentylamine, hexylamine, heptylamine or octylamine; the organic alcohol is methanol, ethanol, propanol, butanol or pentanol.
5. The method for preparing a molybdenum salt heterogeneous carrier according to claim 1, wherein in the step 1, the acid is one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid and acetic acid.
6. The method for preparing a molybdenum salt heterosupporter according to claim 1, wherein the concentration of the acid in step 1 is 1.0-5.0 mol/L.
7. The method for preparing a molybdenum salt heterogeneous carrier according to claim 1, wherein the calcination temperature in the step 2 is 200 to 2000 ℃ and the calcination time is 6 to 12 hours.
8. The method for preparing a molybdenum salt heterosupporter according to claim 1, wherein the multicomponent coexisting molybdenum salt heterosupporter obtained in step 2 comprises two or more of molybdenum carbide, molybdenum oxide, molybdenum nitride, molybdenum phosphide and molybdenum disulfide.
9. The molybdenum salt heterogeneous carrier prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the molybdenum salt heterogeneous support according to claim 9 as a heterogeneous catalyst support.
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Citations (3)
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| GB655557A (en) * | 1946-09-04 | 1951-07-25 | Goodrich Co B F | Improvements in or relating to the production of aldehydes and to catalysts for use in oxidative processes |
| CN107597097A (en) * | 2017-09-04 | 2018-01-19 | 北京林业大学 | A kind of preparation method and applications of Supported molybdenum oxide catalyst |
| CN110201693A (en) * | 2019-06-14 | 2019-09-06 | 陕西科技大学 | A kind of molybdenum carbide catalyst and its preparation method and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB655557A (en) * | 1946-09-04 | 1951-07-25 | Goodrich Co B F | Improvements in or relating to the production of aldehydes and to catalysts for use in oxidative processes |
| CN107597097A (en) * | 2017-09-04 | 2018-01-19 | 北京林业大学 | A kind of preparation method and applications of Supported molybdenum oxide catalyst |
| CN110201693A (en) * | 2019-06-14 | 2019-09-06 | 陕西科技大学 | A kind of molybdenum carbide catalyst and its preparation method and application |
Non-Patent Citations (2)
| Title |
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| LIANG MA ET AL .，: ""Efficient hydrogen evolution reaction catalyzed by molybdenum carbide and molybdenum nitride nanocatalysts synthesized via the urea glass route"", 《J. MATER. CHEM. A》, vol. 3, pages 8361 - 8368 * |
| WEIWEN WANG ET AL.: ""In-situ synthesis of coupled molybdenum carbide and molybdenum nitride as electrocatalyst for hydrogen evolution reaction"", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 792, pages 230 - 239 * |
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