CN116947058B - Hafnium silicate powder and preparation method thereof - Google Patents
Hafnium silicate powder and preparation method thereofInfo
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- CN116947058B CN116947058B CN202310989118.0A CN202310989118A CN116947058B CN 116947058 B CN116947058 B CN 116947058B CN 202310989118 A CN202310989118 A CN 202310989118A CN 116947058 B CN116947058 B CN 116947058B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- Chemical & Material Sciences (AREA)
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- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses hafnium silicate powder and a preparation method thereof, belonging to the technical field of compound synthesis; the preparation method of the hafnium silicate powder comprises the steps of adding a soluble silicic acid compound aqueous solution into the soluble hafnium compound aqueous solution, regulating the pH value of a system to be 2-4, continuously stirring until transparent gel substances appear, obtaining a gel mixture, regulating the pH value of the gel mixture to be 7, performing hydrothermal reaction, cooling, washing, filtering and collecting reaction products to obtain hafnium silicate particles, crushing the hafnium silicate particles, uniformly mixing the hafnium silicate particles with an adhesive and a suspending agent, performing ball milling granulation, and performing flash evaporation to obtain the hafnium silicate powder, wherein the hafnium silicate powder obtained by adopting the technical scheme of the invention has uniform particle size distribution, high purity and yield, and simultaneously, the preparation method can reduce the difficulty of ball milling granulation, thereby reducing the production cost and improving the production efficiency.
Description
Technical Field
The invention belongs to the technical field of compound synthesis, and particularly relates to hafnium silicate powder and a preparation method thereof.
Background
Hafnium is a shiny silver gray transition metal that does not react with dilute hydrochloric acid, dilute sulfuric acid, and strong alkaline solutions, but is soluble in hydrofluoric acid and aqua regia. Hafnium in the crust is 0.00045%, and is usually associated with zirconium in nature, and the chemical property of hafnium is very similar to that of zirconium, so that the hafnium has good corrosion resistance, is not easy to be corroded by common acid-base aqueous solution, is easy to dissolve in hydrofluoric acid to form fluorine complex, and can be directly combined with oxygen, nitrogen and other gases at high temperature to form oxides and nitrides.
The element hafnium is commonly associated with zircon sand, has characteristics similar to zirconium silicate and extremely high melting point, is taken as high-temperature structural ceramic, has extremely high chemical inertness, basically does not react with other acids except hydrofluoric acid, has corrosion resistance for any alkali, can be used in various ultrahigh-temperature environments, has high effective atomic coefficient, has strong absorption capacity of compounds on high-energy rays, and is a potential scintillating material, so that the hafnium compound has important use value and wide application prospect.
Hafnium silicate powder is produced differently from zirconium silicate because natural hafnium silicate does not exist in nature. At present, zirconium silicate can be obtained directly after simple processing such as zircon sand grinding, ball milling and the like. The preparation process of hafnium silicate is complicated, the reaction process is more, the obtained product contains a great amount of impurities, the granularity of hafnium silicate powder is difficult to ensure, and in addition, the grain hardness of the hafnium silicate prepared by the prior art is higher, so that a great amount of time and energy are consumed in the final grinding process, and the operation cost is high. Therefore, the existing preparation process of hafnium silicate powder is more and more difficult to meet the current material requirements, and breakthrough improvement is needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide hafnium silicate powder with high yield, high purity and uniform granularity and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is that the preparation method of the hafnium silicate powder comprises the following steps:
(1) Adding the water solution of soluble silicic acid compound into the water solution of soluble hafnium compound, regulating the pH value of the system to 2-4, and continuously stirring until transparent gel-like substance appears to obtain gel mixture;
(2) Adjusting the pH value of the gel mixture in the step (1) to 7, performing hydrothermal reaction, and cooling, washing, filtering and collecting reaction products after the reaction is finished to obtain hafnium silicate particles;
(3) And (3) after the hafnium silicate particles in the step (2) are crushed, uniformly mixing the hafnium silicate particles with an adhesive and a suspending agent, performing ball milling granulation, and then performing flash evaporation to obtain hafnium silicate powder.
In the preparation method of the hafnium silicate powder, the hafnium silicate powder is obtained through water phase reaction and subsequent dehydration treatment by combining with the subsequent hydrothermal reaction under the pressurized state. The preparation method is simple and convenient to operate, so that the introduction of impurities can be reduced fundamentally, meanwhile, the size of particles can be controlled according to actual requirements in the subsequent ball milling granulation process, hafnium silicate powder with high uniformity is obtained, and the hardness of the obtained hafnium silicate particles is low due to the fact that the steps of hydrothermal reaction, washing and the like are carried out in the early stage, the crushing difficulty in the step (3) can be obviously reduced, the energy consumption and the time in the crushing process are further reduced, the production cost is reduced, and the production efficiency is improved.
As a preferred embodiment of the preparation method of the present invention, the soluble silicic acid compound comprises any one of sodium metasilicate, metasilicic acid, potassium silicate, sodium silicate and sodium metasilicate pentahydrate, and the soluble hafnium compound comprises any one of hafnium oxychloride, hafnium oxychloride hydrate and hafnium tetrachloride.
As a preferred embodiment of the production method of the present invention, the mass concentration of the soluble hafnium compound in the aqueous solution of the soluble hafnium compound is 110 to 130g/L.
As a preferred embodiment of the production method of the present invention, the mass concentration of the soluble silicic acid compound in the aqueous solution of the soluble silicic acid compound is 40 to 60g/L.
The mass concentration of the soluble hafnium compound in the soluble hafnium compound aqueous solution and the mass concentration of the soluble silicic acid compound in the soluble silicic acid compound aqueous solution are controlled within the above ranges, so that the soluble hafnium compound aqueous solution and the soluble silicic acid compound aqueous solution have proper reaction mass concentrations during the mixing reaction, the purity of the product obtained subsequently is ensured, and the yield of the product is further improved.
As a preferred embodiment of the production method of the present invention, the molar ratio of silicon element in the soluble silicic acid compound to hafnium element in the soluble hafnium compound is 1 (0.95-1.05).
As a preferred embodiment of the preparation method of the present invention, the molar ratio of silicon element in the soluble silicic acid compound to hafnium element in the soluble hafnium compound is 1:1.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the stirring speed of the continuous stirring is 120-150r/min.
The stirring speed of 120-150r/min can help the combination of silicon element and hafnium element to form gel-like substances quickly, so that the reaction efficiency is improved, if the stirring speed is too low, the reaction time is too long, the incomplete and uneven reaction occurs, the reaction yield and purity are reduced, and if the stirring speed is too high, whether gel-like substances are formed or not is difficult to judge, so that the judgment of the reaction end point is influenced.
As a preferred embodiment of the preparation method of the present invention, in the step (2), the pH of the gel mixture in the step (1) is adjusted to 7 by using ammonia water. Ammonia water with a mass concentration of 5mol/L was used.
As a preferred embodiment of the preparation method of the present invention, in the step (2), the time of the hydrothermal reaction is controlled within 3.5-4.5 hours, and the pressure of the hydrothermal reaction is controlled within 1.2-1.3 MPa. Particularly, when the reaction time is 4 hours and the pressure is 1.25MPa, the reaction rate can be controlled, and the granularity and granularity uniformity of the generated product can be further controlled.
In the step (2), deionized water is used for washing, and the mass ratio of the washed substance to the deionized water for washing is 1 (1-1.5), so that water-soluble ions such as chlorine, sodium and the like can be washed off in the process.
In the step (3), the adhesive comprises aluminum hydroxide, the suspending agent comprises polyethylene glycol, and aluminum hydroxide is used as the adhesive, wherein a small amount of aluminum can increase the plasticity of the product, preferably, the polymerization degree of the polyethylene glycol is 2000, when the polymerization degree of the polyethylene glycol is 2000, the product with moderate grain size and good uniformity can be obtained in an assisted manner, and the problems of easy agglomeration of powder caused by excessively small polymerization degree of the polyethylene glycol and increased cost caused by excessively high polymerization degree of the polyethylene glycol are avoided.
As a preferred embodiment of the preparation method of the invention, in the step (3), the mass percentage of the adhesive agent is 0.025-0.035% and the mass percentage of the suspending agent is 0.045-0.055% based on the total mass of the ball-milling and granulating materials.
When the added adhesive and suspending agent are in the mass percent range, the mixed powder can be well ball-milled with crushed hafnium silicate particles and can help the hafnium silicate particles to be dispersed, so that hafnium silicate powder with uniform particle size is formed.
In addition, the invention also provides hafnium silicate powder, which is prepared by the preparation method, wherein D 50 =3.07-3.98 μm of the hafnium silicate powder is achieved, and the particle size distribution coefficient P is less than or equal to 3.81.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the hafnium silicate powder, the hafnium silicate powder with high purity and high yield is obtained through water phase reaction and subsequent hydro-thermal reaction under the pressurized state, meanwhile, the grain size can be controlled according to actual requirements during ball milling granulation, the hafnium silicate powder with high uniformity is obtained, and the hardness of the obtained hafnium silicate grains is low through the steps of hydro-thermal reaction, washing and the like in the early stage, so that the crushing difficulty can be obviously reduced, the energy consumption and time in the crushing process can be further reduced, the production cost can be reduced, and the production efficiency can be improved.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The embodiment of the invention provides hafnium silicate, and the preparation method of the hafnium silicate comprises the following steps:
(1) Adding a sodium metasilicate pentahydrate aqueous solution (alkaline) with the mass concentration of 50g/L into a hafnium oxychloride aqueous solution (acidic) with the mass concentration of 120g/L, continuously stirring in the adding process, ensuring the molar ratio of silicon element to hafnium element to be 1:1 after the adding is finished, regulating the pH value of the system to be 4, and continuously stirring at the stirring speed of 120r/min until a transparent gel-like substance appears, thereby obtaining a gel mixture;
(2) Regulating the pH value of the gel mixture in the step (1) to 7 by ammonia water, transferring the gel mixture into an autoclave, placing the autoclave on a boiling water bath, slowly pressurizing to 1.25MPa, reacting for 3.5 hours, cooling to room temperature after the reaction is finished, washing the gel mixture with deionized water for 2 times, wherein the mass of the deionized water is 1.5 times that of a material to be washed, washing, vacuum filtering, and collecting filter residues;
(3) And (3) after crushing the filter residues in the step (2), uniformly mixing the filter residues with aluminum hydroxide and polyethylene glycol, and performing ball milling and granulating, wherein the weight percentage of the aluminum hydroxide is 0.03% and the weight percentage of the polyethylene glycol with the polymerization degree of 2000 is 0.05% based on the total mass of the ball-milled materials, and performing flash evaporation after ball milling and granulating to obtain hafnium silicate powder.
Example 2
The embodiment of the invention provides hafnium silicate, and the preparation method of the hafnium silicate comprises the following steps:
(1) Adding a sodium metasilicate pentahydrate aqueous solution (alkaline) with the mass concentration of 60g/L into a hafnium oxychloride aqueous solution (acidic) with the mass concentration of 130g/L, continuously stirring in the adding process, ensuring the molar ratio of silicon element to hafnium element to be 1:1 after the adding is finished, regulating the pH value of the system to be 3, and continuously stirring at the stirring speed of 150r/min until a transparent gel-like substance appears, thereby obtaining a gel mixture;
(2) Regulating the pH value of the gel mixture in the step (1) to 7 by ammonia water, transferring the gel mixture into an autoclave, placing the autoclave on a boiling water bath, slowly pressurizing to 1.2MPa, reacting for 4 hours, cooling to room temperature after the reaction is finished, washing the gel mixture with deionized water for 2 times, wherein the mass of the deionized water is 1.0 times that of a material to be washed, and filtering the gel mixture in a vacuum way after washing, and collecting filter residues;
(3) And (3) after crushing the filter residues in the step (2), uniformly mixing the filter residues with aluminum hydroxide and polyethylene glycol, and performing ball milling and granulating, wherein the weight percentage of the aluminum hydroxide is 0.03% and the weight percentage of the polyethylene glycol with the polymerization degree of 2000 is 0.05% based on the total mass of the ball-milled materials, and performing flash evaporation after ball milling and granulating to obtain hafnium silicate powder.
Example 3
The embodiment of the invention provides hafnium silicate, and the preparation method of the hafnium silicate comprises the following steps:
(1) Adding a sodium metasilicate pentahydrate aqueous solution (alkaline) with the mass concentration of 40g/L into a hafnium oxychloride aqueous solution (acidic) with the mass concentration of 110g/L, continuously stirring in the adding process, ensuring the molar ratio of silicon element to hafnium element to be 1:1 after the adding is finished, regulating the pH value of the system to be 2, and continuously stirring at the stirring speed of 135r/min until a transparent gel-like substance appears, thereby obtaining a gel mixture;
(2) Regulating the pH value of the gel mixture in the step (1) to 7 by ammonia water, transferring the gel mixture into an autoclave, placing the autoclave on a boiling water bath, slowly pressurizing to 1.3MPa, reacting for 3 hours, cooling to room temperature after the reaction is finished, washing the gel mixture with deionized water for 2 times, wherein the mass of the deionized water is 1.2 times that of a material to be washed, and filtering the gel mixture in a vacuum way after washing, and collecting filter residues;
(3) And (2) after crushing the filter residues in the step (2), uniformly mixing the filter residues with aluminum hydroxide, ammonia water and polyethylene glycol, and performing ball milling and granulation, wherein the weight percentage of the aluminum hydroxide is 0.03% and the weight percentage of the polyethylene glycol with the polymerization degree of 2000 is 0.05% based on the total mass of the ball-milled materials, and performing flash evaporation after ball milling and granulation to obtain hafnium silicate powder.
Comparative example 1
The comparative example of the present invention provides a hafnium silicate which differs from example 2 only in that the pH of the adjustment system in step (1) is 6.
Comparative example 2
The comparative example of the present invention provides a hafnium silicate which differs from example 2 only in that the pH of the adjustment system in step (1) is 1.
Comparative example 3
The comparative example of the present invention provides a hafnium silicate which differs from example 2 only in that the stirring speed in step (1) is 80r/min.
Comparative example 4
The comparative example of the present invention provides a hafnium silicate which differs from example 2 only in that in step (1) an aqueous sodium metasilicate pentahydrate solution having a mass concentration of 100g/L is added to an aqueous hafnium oxychloride solution having a mass concentration of 240 g/L.
Comparative example 5
The comparative example of the present invention provides a hafnium silicate which differs from example 2 only in that in step (2) the pressure is slowly increased to 2MPa.
Comparative example 6
The comparative example of the present invention provides a hafnium silicate which differs from example 2 only in that in step (2) it is placed on a boiling water bath and reacted for 3.5 hours without pressurization.
Comparative example 7
The comparative example of the present invention provides hafnium silicate, which is different from example 2 only in that polyethylene glycol having a polymerization degree of 600 is added in step (3).
Comparative example 8
The comparative example of the present invention provides hafnium silicate, which is different from example 2 only in that polyethylene glycol having a polymerization degree of 3000 is added in step (3).
Effect example
The information on purity, yield and particle diameter of hafnium silicate prepared in examples 1 to 3 and comparative examples 1 to 8 is recorded in this effect example, and the specific statistics are shown in Table 1;
TABLE 1
As can be seen from Table 1, when the technical scheme of the invention is adopted, the purity of the obtained product is over 99.92%, the yield is over 78.95%, the obtained D 50 = 3.07-3.98 μm, the particle size distribution coefficient P is less than or equal to 3.81, and the obtained hafnium silicate powder has excellent particle size uniformity;
it can be seen from example 2 and comparative examples 1 to 2 that when the pH adjusted in advance was changed so that the pH was not within the range given in the present invention, the desired product of the present invention could not be obtained;
As can be seen from example 2 and comparative example 3, when the stirring rate is reduced, the purity and yield of the obtained hafnium silicate powder are significantly reduced;
As can be seen from example 2 and comparative example 4, when the mass concentration of the soluble silicate and the soluble hafnium compound is increased, the yield of the obtained hafnium silicate powder inversely shows a tendency to decrease;
As can be seen from example 2 and comparative examples 5 to 6, when the pressure of the hydrothermal reaction is changed, the yield of the product is lowered and the uniformity of particle size of the product is also lowered;
As can be seen from example 2 and comparative example 7, when the polymerization degree of polyethylene glycol is reduced, the yield of the product is lowered, and the uniformity of particle size of the product is also lowered;
As can be seen from example 2 and comparative example 8, when the polymerization degree of polyethylene glycol is increased, the yield of the product is lowered.
Finally, it should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, and that those skilled in the art will understand that changes can be made to the technical solutions of the invention or equivalents thereof without departing from the spirit and scope of the technical solutions of the invention.
Claims (5)
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| CN202310989118.0A CN116947058B (en) | 2023-08-08 | 2023-08-08 | Hafnium silicate powder and preparation method thereof |
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| CN202310989118.0A CN116947058B (en) | 2023-08-08 | 2023-08-08 | Hafnium silicate powder and preparation method thereof |
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| CN116947058B true CN116947058B (en) | 2025-09-19 |
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- 2023-08-08 CN CN202310989118.0A patent/CN116947058B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| "Soft hydrothermal synthesis of hafnon, HfSiO4";Paul Estevenon等;《CRYSTAL GROWTH DESIGN》;20200129;1820-1828 * |
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