CN114477247A - Method for synthesizing nano magnesium oxide by microwave induced combustion - Google Patents
Method for synthesizing nano magnesium oxide by microwave induced combustion Download PDFInfo
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- CN114477247A CN114477247A CN202210343176.1A CN202210343176A CN114477247A CN 114477247 A CN114477247 A CN 114477247A CN 202210343176 A CN202210343176 A CN 202210343176A CN 114477247 A CN114477247 A CN 114477247A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention provides a method for preparing nano-magnesia by utilizing microwave-induced combustion synthesis reaction, which comprises the steps of firstly using light-burned magnesia prepared from microcrystalline magnesite as a raw material, dissolving the light-burned magnesia with a dilute nitric acid solution, filtering, taking out filtrate, adjusting the pH value of the solution to 8-10 with concentrated ammonia water, standing, and carrying out secondary filtration to obtain a magnesium nitrate solution. The nano magnesium oxide powder material is prepared by mixing a magnesium nitrate solution and one or more of urea, citric acid or glycine as raw materials according to a certain proportion and adopting a microwave induced combustion method. And then, calcining the magnesium oxide powder material at 300-600 ℃ for 1-4 h in a heat preservation manner, performing ball milling on the calcined material, and drying to obtain the nano magnesium oxide powder. The preparation method has the characteristics of simple preparation process, high heating speed, high thermal efficiency, energy conservation, time conservation and uniform heating, and the prepared nano-magnesia has the characteristics of small granularity, uniform dispersion, high purity and high activity, and can expand the application range of the technology to the preparation of other nano-oxide materials.
Description
Technical Field
The invention relates to a preparation method for synthesizing nano-magnesia by taking microcrystalline magnesite as a raw material through microwave-induced combustion, belonging to the field of material preparation.
Background
The magnesite in China is abundant in resources and huge in reserves, and is at the top of the world at present. The type mainly uses crystalline magnesite, and a small amount of microcrystalline magnesite. The Tibet Kammy magnesite is high-grade large-scale microcrystalline magnesite which is only stored in the known terrestrial magnesite in the world, and high-quality magnesite accounts for 90 percent of the total storage amount. The light-burned magnesia obtained by calcining the microcrystal magnesite has extremely high purity, and the content of the magnesia is more than or equal to 98 percent. Compared with magnesite in northeast China, the magnesite-magnesite avoids containing more elements such as iron, aluminum, silicon, calcium and the like. Compared with the magnesium source obtained by concentrating and refining seawater, the magnesium source does not contain chlorine element. Therefore, the Tibet microcrystalline magnesite is very suitable to be used as a raw material for producing environment-friendly high-end magnesian chemical products. According to the characteristic, the microcrystalline magnesite can be used for producing nano magnesia materials with better quality.
The nano magnesium oxide is a white powdery particle, belongs to one of nano materials, and is non-toxic, tasteless and large in specific surface area. Compared with the common magnesium oxide material, the nano magnesium oxide has higher specific surface area and surface reactivity, so the performance of the nano magnesium oxide is different from that of the bulk material in the aspects of thermal, optical, electrical, magnetic and the like. The nano-magnesia is widely applied to the fields of adsorbents, antibacterial agents, catalyst carriers, special ceramics and the like, and has huge application prospect and economic potential. The traditional preparation technology of nano magnesium oxide mainly comprises the following steps: vapor phase oxidation, vapor phase pyrolysis, solid phase synthesis, homogeneous precipitation, sol-gel, and hydrothermal methods, and the like. The microwave-induced combustion synthesis method is characterized in that the precursor molecules absorb microwaves under the action of microwaves, the dielectric polarization and the dipole moment of the precursor molecules are changed rapidly, and the microwaves interact with molecules on the surface and in the interior of a material to generate heat. The microwave-assisted heating mode has the characteristics of uniform heating, high heating speed and high heat efficiency, and can quickly induce combustion synthesis reaction to form uniform nano magnesium oxide powder.
At present, there are many researches on the synthesis of nano-oxides by using different methods, but there are relatively few researches on the synthesis of nano-magnesium oxide by microwave-induced combustion. A process for preparing nano-class magnesium oxide (CN104386716A) includes such steps as pulverizing dolomite to 5.5mm, calcining at 1260 deg.C, adding water, digesting at 93 deg.C, introducing CO at room temp2Carbonizing until the pH value of the system is 9.3, forming solid calcium carbonate and liquid magnesium bicarbonate, performing solid-liquid separation to obtain a magnesium bicarbonate solution, adding sodium hexametaphosphate and polyacrylic acid into the magnesium bicarbonate solution, stirring uniformly and fully, pyrolyzing at 78 ℃ for 95 minutes until basic magnesium carbonate solid precipitates, and calcining at 780 ℃ for 70 minutes to obtain the nano magnesium oxide.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for synthesizing nano magnesium oxide by microwave-assisted combustion. The method has the advantages of simple production process, low production cost and relatively short product preparation period, and can obtain nano magnesium oxide particles with small particle size, uniform dispersion and high activity.
The technical scheme of the invention is as follows:
a method for preparing nano magnesia powder by utilizing microwave-induced combustion synthesis reaction is characterized in that nitrate is used as an oxidant, fuel is used as a reducing agent, wherein the nitrate is selected from a magnesium nitrate solution prepared by taking light-burned magnesia prepared from microcrystalline magnesite as a raw material, the fuel is selected from one or more of urea, citric acid or glycine, and the nano magnesia powder material is prepared by adopting microwave-induced combustion synthesis reaction. The method comprises the following specific steps:
(1) preparing a magnesium nitrate solution: calcining microcrystalline magnesite at high temperature to obtain light-burned magnesium oxide, mixing the light-burned magnesium oxide with a dilute nitric acid solution, and filtering to remove filter residues.
(2) Adjusting the pH value of the solution, standing, and then filtering to obtain a magnesium nitrate solution.
(3) Mixing of oxidant and fuel: and uniformly mixing the oxidant and the fuel to obtain a precursor solution.
(4) Microwave-induced combustion synthesis: and carrying out microwave-induced combustion synthesis reaction on the precursor solution to obtain the nano magnesium oxide powder.
(5) Powder calcination: the nano magnesia powder body which is synthesized by microwave-induced combustion is calcined for a period of time under the condition of heat preservation.
(6) Ball milling: ball-milling the calcined powder, and vacuum-drying to obtain high-purity uniformly-dispersed nano magnesium oxide.
According to the invention, the molar ratio of the light-burned magnesium oxide to the dilute nitric acid in the step (1) is 1: (2-3). The concentration of the nitric acid solution is 20-40 wt%.
According to the invention, ammonia water is used in the step (2) to adjust the pH value of the solution to 8-10, and the solution is kept stand for 1-3 hours.
According to the invention, the citric acid used in step (3) is citric acid monohydrate (C)6H8O7·H2O)。
According to the invention, the magnesium nitrate solution and the urea solution in step (3) are Mg2+: the urea molar ratio is 3: (3-8) uniformly mixing to prepare a precursor solution; or mixing magnesium nitrate solution and citric acid solution according to Mg2+: the molar ratio of urea is 9: (3-8) uniformly mixing to prepare a precursor solution; or mixing magnesium nitrate solution and glycine solution according to Mg2+: the molar ratio of urea is 9: (8-12) uniformly mixing to prepare a precursor solution; or mixing magnesium nitrate solution with mixed solution of citric acid and glycine according to Mg2+: citric acid: the molar ratio of glycine is 9: (1-4): (4-6) uniformly mixing to prepare a precursor solution.
According to the invention, the solution in the step (3) is stirred and mixed uniformly at constant temperature and constant speed by using a magnetic stirrer. The precursor solution is filled in a magnesium oxide crucible.
According to the invention, the microwave combustion device in the step (4) is an industrial microwave oven.
According to the invention, the nano magnesium oxide powder calcining device in the step (5) is a muffle furnace. The heat preservation calcining temperature of the nano magnesium oxide powder is 350-600 ℃, and the heat preservation time is 1-3 h.
According to the invention, the ball milling mode in the step (6) is wet ball milling, and the medium is absolute ethyl alcohol.
The working principle of the invention is as follows:
the invention uses light-burned magnesium oxide, dilute nitric acid and one or more of urea, citric acid monohydrate and glycine as raw materials, uses an industrial microwave oven as a combustion reaction furnace, synthesizes nano magnesium oxide through microwave-induced combustion, puts precursor solution into a magnesium oxide crucible, puts the crucible into the industrial microwave oven, and quickly heats the precursor solution under the action of microwaves, and generates fine agglomerates through boiling, expansion and combustion. Then, ball milling is carried out on the nano magnesium oxide synthesized by microwave induced combustion, thereby forming nano magnesium oxide powder.
The invention has the beneficial effects that: the microwave-assisted heating mode has the characteristics of uniform heating, high heating speed and high heat efficiency, and greatly saves energy. Meanwhile, the nano magnesium oxide prepared by microwave-induced combustion synthesis has uniform granularity and high purity.
Detailed Description
The technical solution of the present invention is further described with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1:
a method for synthesizing nano magnesium oxide by microwave combustion comprises the following steps:
preparing a magnesium nitrate solution: 40g of light-burned magnesia powder was weighed, diluted nitric acid solution was used, and the molar ratio of MgO: HNO3Configuring as 1:2 to obtain Mg (NO)3)2Solution, then Mg (NO)3)2The solution was dissolved by stirring with a magnetic stirrer in a beaker and filtered.
Adjusting the pH value: to dissolve the completed Mg (NO)3)2Dropwise adding ammonia water into the solution, adjusting the pH value of the solution to 9, standing for 2h, and filtering.
Mixing the magnesium nitrate solution with the fuel: mixing magnesium nitrate solution and glycine solution according to Mg2+: the molar ratio of glycine is 9: 11, mixing to prepare a precursor solution.
Microwave-induced combustion synthesis: and placing the prepared precursor solution into a magnesium oxide crucible, and then placing the magnesium oxide crucible into an industrial microwave oven for microwave combustion synthesis.
Powder calcination: the powder synthesized by microwave combustion is put into a muffle furnace, the temperature in the furnace is raised to 500 ℃, and the temperature is kept for 3 hours.
Ball milling: and carrying out wet ball milling on the calcined nano magnesium oxide powder for 2 hours, and then carrying out vacuum drying on the material to obtain the nano magnesium oxide powder.
The magnesium oxide nano powder obtained by the embodiment has the particle size of 40-100 nm, is uniformly distributed, has the citric acid activity value of 80-120 s, and has high activity.
Example 2:
a method for synthesizing nano magnesium oxide by microwave combustion comprises the following steps:
preparing a magnesium nitrate solution: 40g of light-burned magnesia powder was weighed, diluted nitric acid solution was used, and the molar ratio of MgO: HNO3Configuring as 1:2 to obtain Mg (NO)3)2Solution, then Mg (NO)3)2The solution was dissolved by stirring with a magnetic stirrer in a beaker and filtered.
Adjusting the pH value: to dissolve the completed Mg (NO)3)2And dropwise adding ammonia water into the solution, adjusting the pH value of the solution to 10, standing for 2h, and filtering.
Mixing the magnesium nitrate solution with the fuel: mixing the magnesium nitrate solution with the fuel: mixing magnesium nitrate solution with urea solution according to Mg2+: and mixing the urea at a molar ratio of 3:6 to prepare a precursor solution.
Microwave-induced combustion synthesis: and placing the prepared precursor solution into a magnesium oxide crucible, and then placing the magnesium oxide crucible into an industrial microwave oven for microwave combustion synthesis.
Powder calcination: the powder synthesized by microwave combustion is put into a muffle furnace, the temperature in the furnace is raised to 450 ℃, and the temperature is kept for 3 hours.
Ball milling: and carrying out wet ball milling on the calcined nano magnesium oxide powder for 2 hours, and then carrying out vacuum drying on the material to obtain the nano magnesium oxide powder.
The magnesium oxide nano powder obtained by the embodiment has the particle size of 40-100 nm, is uniformly distributed, has the citric acid activity value of 70-110 s, and has high activity.
Example 3:
a method for synthesizing nano magnesium oxide by microwave combustion comprises the following steps:
preparing a magnesium nitrate solution: 40g of light-burned magnesia powder was weighed, diluted nitric acid solution was used, and the molar ratio of MgO: HNO3Configuring as 1:2 to obtain Mg (NO)3)2Solution, then Mg (NO)3)2The solution was dissolved by stirring with a magnetic stirrer in a beaker and filtered.
Adjusting the pH value: to dissolve the completed Mg (NO)3)2And dropwise adding ammonia water into the solution, adjusting the pH value of the solution to 10, standing for 2h, and filtering.
Mixing the magnesium nitrate solution with the fuel: mixing the magnesium nitrate solution with the fuel: mixing magnesium nitrate solution and citric acid solution according to Mg2+: and mixing the citric acid with the molar ratio of 3:6 to prepare a precursor solution.
Microwave-induced combustion synthesis: and placing the prepared precursor solution into a magnesium oxide crucible, and then placing the magnesium oxide crucible into an industrial microwave oven for microwave combustion synthesis.
Powder calcination: the powder synthesized by microwave combustion is put into a muffle furnace, the temperature in the furnace is raised to 400 ℃, and the temperature is kept for 3 hours.
Ball milling: and carrying out wet ball milling on the calcined nano magnesium oxide powder for 2 hours, and then carrying out vacuum drying on the material to obtain the nano magnesium oxide powder.
The magnesium oxide nano powder obtained by the embodiment has the particle size of 40-100 nm, is uniformly distributed, has the citric acid activity value of 70-110 s, and has high activity.
Example 4:
a method for synthesizing nano magnesium oxide by microwave combustion comprises the following steps:
preparing a magnesium nitrate solution: 40g of light-burned magnesia powder was weighed, diluted nitric acid solution was used, and the molar ratio of MgO: HNO3Configuring as 1:2 to obtain Mg (NO)3)2Solution, then Mg (NO)3)2The solution was dissolved by stirring with a magnetic stirrer in a beaker and filtered.
Adjusting the pH value: to dissolve the completed Mg (NO)3)2And dropwise adding ammonia water into the solution, adjusting the pH value of the solution to 10, standing for 2h, and filtering.
Mixing the magnesium nitrate solution with the fuel: mixing the magnesium nitrate solution with the fuel: mixing magnesium nitrate solution with citric acid and glycine solution according to Mg2+: citric acid: mixing glycine in a molar ratio of 9:2:6 to prepare a precursor solution.
Microwave-induced combustion synthesis: and placing the prepared precursor solution into a magnesium oxide crucible, and then placing the magnesium oxide crucible into an industrial microwave oven for microwave combustion synthesis.
Powder calcination: the powder synthesized by microwave combustion is put into a muffle furnace, the temperature in the furnace is raised to 600 ℃, and the temperature is kept for 3 hours.
Ball milling: and carrying out wet ball milling on the calcined nano magnesium oxide powder for 2 hours, and then carrying out vacuum drying on the material to obtain the nano magnesium oxide powder.
The magnesium oxide nano powder obtained by the embodiment has the particle size of 40-100 nm, uniform distribution, citric acid activity value of 100-140 s and high activity.
The above embodiments are merely some specific embodiments of the present invention, and therefore, the present invention is not limited to the above embodiments, and other embodiments are possible. All modifications directly or indirectly derivable by a person skilled in the art from the present disclosure are to be considered within the scope of the present invention.
Claims (10)
1. A method for preparing nano magnesium oxide powder by utilizing microwave-induced combustion synthesis reaction comprises the following specific steps:
(1) preparing a magnesium nitrate solution: calcining microcrystalline magnesite at high temperature to obtain light-burned magnesium oxide, mixing the light-burned magnesium oxide with a dilute nitric acid solution, and filtering to remove filter residues.
(2) Adjusting the pH value: adjusting the pH value of the solution, standing, and then filtering to obtain a magnesium nitrate solution.
(3) Mixing of oxidant and fuel: and uniformly mixing the oxidant and the fuel to obtain a precursor solution.
(4) Microwave-induced combustion synthesis: and carrying out microwave-induced combustion synthesis reaction on the precursor solution to obtain the nano magnesium oxide powder.
(5) Powder calcination: the nano magnesia powder body which is synthesized by microwave-induced combustion is calcined for a period of time under the condition of heat preservation.
(6) Ball milling: ball milling and drying the calcined powder to finally prepare the high-purity nano magnesium oxide powder.
2. The method for preparing nano magnesium oxide powder by microwave-induced combustion synthesis reaction according to claim 1, wherein the molar ratio of the light-burned magnesium oxide to the dilute nitric acid is 1: (2-3).
3. The method for preparing nano magnesium oxide powder through microwave-induced combustion synthesis reaction according to claim 1, wherein the concentration of the dilute nitric acid solution in the step (1) is 20-40 wt%.
4. The method for preparing nano magnesium oxide powder by microwave-induced combustion synthesis reaction according to claim 1, wherein in the step (2), ammonia water is used for adjusting the pH value of the solution to 8-10, and then the solution is allowed to stand for 1-3 hours.
5. The method for preparing nano magnesia powder by microwave-induced combustion synthesis reaction as claimed in claim 1, wherein nitrate is used as oxidant and fuel is used as reductant in step (3), wherein nitrate is selected from magnesium nitrate solution prepared by using light-burned magnesia prepared from microcrystalline magnesite as raw materialThe fuel is selected from one or more of urea, citric acid or glycine, and the nano magnesium oxide powder material is prepared by adopting microwave-induced combustion synthesis reaction. Mixing magnesium nitrate solution with urea solution according to Mg2+: the urea molar ratio is 3: (3-8) uniformly mixing to prepare a precursor solution; or mixing magnesium nitrate solution and citric acid solution according to Mg2+: the citric acid molar ratio is 9: (3-8) uniformly mixing to prepare a precursor solution; or mixing magnesium nitrate solution and glycine solution according to Mg2+: the molar ratio of glycine is 9: (8-12) uniformly mixing to prepare a precursor solution; or mixing magnesium nitrate solution with mixed solution of citric acid and glycine according to Mg2+: citric acid: the molar ratio of glycine is 9: (1-4): (4-6) uniformly mixing to prepare a precursor solution.
6. The method for preparing nano magnesium oxide powder by microwave-induced combustion synthesis reaction according to claim 1, wherein the citric acid solution in the step (3) is citric acid monohydrate (C)6H8O7·H2O)。
7. The method for preparing nano magnesium oxide powder by microwave-induced combustion synthesis reaction as claimed in claim 1, wherein the solution in step (3) is stirred and mixed uniformly at constant temperature and constant speed by using a magnetic stirrer.
8. The method for preparing nano magnesium oxide powder by microwave-induced combustion synthesis reaction as claimed in claim 1, wherein the precursor solution in step (3) is loaded in a magnesium oxide crucible.
9. The method for preparing nano magnesium oxide powder by microwave-induced combustion synthesis reaction according to claim 1, wherein the device for synthesizing nano magnesium oxide powder by microwave-induced combustion in step (4) is an industrial microwave oven.
10. The method for preparing nano magnesium oxide powder through microwave-induced combustion synthesis reaction according to claim 1, wherein the nano magnesium oxide powder in the step (5) is subjected to heat preservation and calcination at 350-600 ℃ for 1-3 h.
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