CN111377458A - Preparation method of superfine iron boride - Google Patents

Preparation method of superfine iron boride Download PDF

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CN111377458A
CN111377458A CN202010308577.4A CN202010308577A CN111377458A CN 111377458 A CN111377458 A CN 111377458A CN 202010308577 A CN202010308577 A CN 202010308577A CN 111377458 A CN111377458 A CN 111377458A
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iron boride
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CN111377458B (en
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蒋央芳
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    • C—CHEMISTRY; METALLURGY
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    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/04—Metal borides
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    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

The invention discloses a preparation method of superfine iron boride. Mixing the ferrous gluconate solution with the boric acid solution, and performing spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.01-1.02; sintering the spray-dried material in a methane atmosphere for 5-10h at 800-1200 ℃ to obtain a reducing material; continuously introducing carbon dioxide into the reducing material, and reacting at the temperature of 700-850 ℃ for 2-4h to obtain a sintering material; and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride. The invention can prepare the superfine ferric boride with small grain size, large BET and high purity.

Description

Preparation method of superfine iron boride
Technical Field
The invention relates to a preparation method of superfine iron boride, belonging to the technical field of powder preparation.
Background
Iron boride (Iron boride) is a boride of Iron, has the formula FeB, and has a molecular weight of 66.66. The iron boride is gray orthorhombic crystal, the melting point is 1652 ℃, and the density is 7.15 g/mL. The arrangement mode of the iron boride is a sawtooth chain shape, iron atoms are positioned on the corners of a triangular prism, and boron atoms are positioned at the center of the triangular prism and are connected in the sawtooth chain in a covalent bond mode. The melting point of the iron boride is 1652 ℃, the density is 7.15g/mL, the iron boride is dissolved in dilute and concentrated nitric acid, concentrated and 1:1 hydrochloric acid solution, and H is 1:12SO4And HClO4Mu ineffAt low temperature, it exists in α -form, at high temperature, it exists in β -form with the same Tc (602K), it changes from α to β with the change of magnetic moment, both can form ferromagnet, it reacts with boiling water, and it is hard, refractory and corrosion resistant.
The conventional preparation method comprises the following steps: 1. mixing the boron and the iron uniformly according to the molar ratio of 1:1, and carrying out co-heating at 1200-1300 ℃ in argon gas to obtain the iron-based alloy. 2. FeS and BCl in Hydrogen3At a temperature higher than 500 ℃, or by reacting ferrous chloride solution with sodium borohydride (NaBH)4) And (3) reacting to obtain the product.
However, the iron boride prepared by the conventional preparation method has large particle size, small BET and low activity.
Disclosure of Invention
In view of the above, the invention provides a preparation method of superfine iron boride, which can prepare the superfine iron boride with small particle size, large BET and high purity.
The invention solves the technical problems by the following technical means:
a preparation method of superfine iron boride comprises the following steps:
(1) mixing the ferrous gluconate solution with the boric acid solution, and performing spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.01-1.02;
(2) sintering the spray-dried material in a methane atmosphere for 5-10h at 800-1200 ℃ to obtain a reducing material;
(3) continuously introducing carbon dioxide into the reducing material, and reacting at the temperature of 700-850 ℃ for 2-4h to obtain a sintering material;
(4) and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride.
The concentration of the ferrous gluconate solution in the step (1) is 1.5-3mol/L, the concentration of the boric acid solution is 1-2mol/L, a centrifugal spray dryer is adopted for spray drying, the rotating speed of a centrifugal atomizing wheel is 15000-20000r/min, the air inlet temperature in the atomizing process is 200-300 ℃, the discharging temperature is less than or equal to 90 ℃, the particle size of atomized liquid drops is less than or equal to 50 mu m, and the particle size of a spray drying material is less than or equal to 20 mu m.
And (3) sintering the spray drying material in the step (2) in a methane atmosphere, wherein the calcining process comprises a heating process and a heat preservation process, the heating rate of the heating process is 100-.
The volume of the methane gas introduced per hour in the step (2) is 800 times of 300 times of the volume of the filled spray-dried material.
And (4) in the step (3), the volume of carbon dioxide introduced per hour is 500 times of the volume of the filled spray drying material, and the material is discharged after the sintering is finished and the material temperature of the material is cooled to be less than or equal to 60 ℃.
And (4) performing jet milling by using high-pressure nitrogen as a gas source under the pressure of 4-7 atmospheric pressures, grading by using a grading wheel, controlling the grain size of discharged materials to be less than or equal to 3 microns, sieving by using a 200-mesh sieve, and performing vacuum packaging to obtain the superfine iron boride.
The invention relates to a preparation method of iron boride, which comprises the steps of mixing a ferrous gluconate solution with a boric acid solution, uniformly mixing borate, ferrous ions and gluconate through spray drying, calcining in a methane atmosphere to obtain carbon-coated and doped iron boride particles, introducing carbon dioxide at a lower temperature, reacting the carbon dioxide with hot carbon to obtain carbon monoxide, and consuming the coated and doped carbon to obtain the iron boride.
Calcining process under the methane atmosphere, owing to there is gluconic acid root to exist, thermal decomposition under high temperature obtains carbon to effectual adhesion and the growing up of having avoided between the adjacent iron boride is and is melted, thereby obtains superfine iron boride, then the carbon dioxide gas of rethread, can react doping and coated carbon consumption, thereby obtains pure iron boride, also can improve the porosity of iron boride simultaneously, increase BET, reinforcing activity.
The invention can prepare the superfine ferric boride with small grain size and large BET, and simultaneously, the anion gluconate ions can be decomposed into carbon at high temperature, and consumed by carbon dioxide without remaining, and other impurities are not introduced, so the purity of the obtained product is high.
The invention has no waste water and small environmental protection pressure.
The invention has the beneficial effects that: can prepare the superfine ferric boride with small grain size, large BET and high purity.
Drawings
FIG. 1 shows SEM of a product obtained in example 1 of the present invention.
FIG. 2 shows SEM of a product obtained in example 2 of the present invention.
FIG. 3 is a SEM of a product obtained in example 3 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following specific examples and accompanying drawings, wherein the preparation method of the ultrafine iron boride comprises the following steps:
(1) mixing the ferrous gluconate solution with the boric acid solution, and performing spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.01-1.02;
(2) sintering the spray-dried material in a methane atmosphere for 5-10h at 800-1200 ℃ to obtain a reducing material;
(3) continuously introducing carbon dioxide into the reducing material, and reacting at the temperature of 700-850 ℃ for 2-4h to obtain a sintering material;
(4) and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride.
The concentration of the ferrous gluconate solution in the step (1) is 1.5-3mol/L, the concentration of the boric acid solution is 1-2mol/L, a centrifugal spray dryer is adopted for spray drying, the rotating speed of a centrifugal atomizing wheel is 15000-20000r/min, the air inlet temperature in the atomizing process is 200-300 ℃, the discharging temperature is less than or equal to 90 ℃, the particle size of atomized liquid drops is less than or equal to 50 mu m, and the particle size of a spray drying material is less than or equal to 20 mu m.
And (3) sintering the spray drying material in the step (2) in a methane atmosphere, wherein the calcining process comprises a heating process and a heat preservation process, the heating rate of the heating process is 100-.
The volume of the methane gas introduced per hour in the step (2) is 800 times of 300 times of the volume of the filled spray-dried material.
And (4) in the step (3), the volume of carbon dioxide introduced per hour is 500 times of the volume of the filled spray drying material, and the material is discharged after the sintering is finished and the material temperature of the material is cooled to be less than or equal to 60 ℃.
And (4) performing jet milling by using high-pressure nitrogen as a gas source under the pressure of 4-7 atmospheric pressures, grading by using a grading wheel, controlling the grain size of discharged materials to be less than or equal to 3 microns, sieving by using a 200-mesh sieve, and performing vacuum packaging to obtain the superfine iron boride.
Example 1
A preparation method of superfine iron boride comprises the following steps:
(1) mixing a ferrous gluconate solution and a boric acid solution, and then carrying out spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.01;
(2) sintering the spray-dried material in a methane atmosphere for 10h at 1200 ℃ to obtain a reduced material;
(3) continuously introducing carbon dioxide into the reducing material, and reacting for 4 hours at the temperature of 700 ℃ to obtain a sintering material;
(4) and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride.
The concentration of the ferrous gluconate solution in the step (1) is 1.5mol/L, the concentration of the boric acid solution is 1mol/L, a centrifugal spray dryer is adopted for spray drying, the rotating speed of a centrifugal atomizing wheel is 20000r/min, the air inlet temperature in the atomizing process is 300 ℃, the discharging temperature is 82 ℃, the particle size of atomized liquid drops is less than or equal to 50 mu m, and the particle size of a spray drying material is 12.4 mu m.
And (3) sintering the spray drying material in the step (2) in a methane atmosphere, wherein the calcining process comprises a heating process and a heat preservation process, the heating rate of the heating process is 100 ℃/h, an induced draft fan is started in the heating process, waste gas generated in the heating process is discharged through the induced draft fan, the humidity in the sintering furnace in the heating process is maintained to be less than or equal to 20%, then the induced draft fan is closed in the heat preservation process, and natural air exhaust is adopted.
The volume of methane gas introduced per hour in the step (2) is 300 times of the volume of the charged spray-dried material.
And (3) introducing carbon dioxide in a volume which is 500 times of the volume of the charged spray drying material per hour in the step (3), cooling the sintered material until the material temperature of the material is less than or equal to 60 ℃, and discharging the material.
And (4) performing jet milling by using high-pressure nitrogen as a gas source under the pressure of 4 atmospheric pressures, grading by using a grading wheel, controlling the grain size of discharged materials to be 1.4 mu m, sieving by using a 200-mesh sieve, and performing vacuum packaging to obtain the superfine iron boride.
The final obtained detection data of the iron boride are as follows:
index (I) D10 D50 D90 BET Fe
Numerical value 0.4μm 1.4μm 3.2μm 18.4m2/g 83.65％
B O Tap density Ni Mn Co
16.29％ 0.05％ 3.72g/mL 6.1ppm 10.3ppm 8.7ppm
Cd Cu Zn Ca C P
0.1ppm 0.1ppm 0.4ppm 4.5ppm 0.18％ 0.0045％
Example 2
A preparation method of superfine iron boride comprises the following steps:
(1) mixing a ferrous gluconate solution and a boric acid solution, and then carrying out spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.02;
(2) sintering the spray-dried material in a methane atmosphere for 10h at 1200 ℃ to obtain a reduced material;
(3) continuously introducing carbon dioxide into the reducing material, and reacting for 2 hours at the temperature of 850 ℃ to obtain a sintering material;
(4) and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride.
The concentration of the ferrous gluconate solution in the step (1) is 3mol/L, the concentration of the boric acid solution is 2mol/L, a centrifugal spray dryer is adopted for spray drying, the rotating speed of a centrifugal atomizing wheel is 20000r/min, the air inlet temperature in the atomizing process is 200 ℃, the discharging temperature is 85 ℃, the particle size of atomized liquid drops is less than or equal to 50 mu m, and the particle size of a spray drying material is 7.9 mu m.
And (3) sintering the spray drying material in the step (2) in a methane atmosphere, wherein the calcining process comprises a heating process and a heat preservation process, the heating rate of the heating process is 100 ℃/h, an induced draft fan is started in the heating process, waste gas generated in the heating process is discharged through the induced draft fan, the humidity in the sintering furnace in the heating process is maintained to be less than or equal to 20%, then the induced draft fan is closed in the heat preservation process, and natural air exhaust is adopted.
The volume of methane gas introduced per hour in the step (2) is 300 times of the volume of the charged spray-dried material.
And (3) introducing carbon dioxide in an amount which is 200 times the volume of the charged spray-dried material per hour in the step (3), cooling the sintered material until the material temperature of the material is less than or equal to 60 ℃, and discharging the material.
And (4) performing jet milling by using high-pressure nitrogen as a gas source under the pressure of 4 atmospheric pressures, grading by using a grading wheel, controlling the grain size of discharged materials to be 2.1 mu m, sieving by using a 200-mesh sieve, and performing vacuum packaging to obtain the superfine iron boride.
The detection data of the finally obtained basic ammonium ferric phosphate are as follows:
index (I) D10 D50 D90 BET Fe
Numerical value 0.5μm 2.1μm 4.9μm 17.2m2/g 83.51％
B O Tap density Ni Mn Co
16.39％ 0.06％ 3.67g/mL 6.6ppm 10.8ppm 8.1ppm
Cd Cu Zn Ca C P
0.1ppm 0.1ppm 0.3ppm 4.2ppm 0.17％ 0.0043％
Example 3
A preparation method of superfine iron boride comprises the following steps:
(1) mixing the ferrous gluconate solution with the boric acid solution, and performing spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.015;
(2) sintering the spray-dried material in a methane atmosphere, wherein the sintering time is 8h, and the sintering temperature is 1000 ℃ for reaction to obtain a reduced material;
(3) continuously introducing carbon dioxide into the reducing material, and reacting for 3 hours at the temperature of 780 ℃ to obtain a sintering material;
(4) and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride.
The concentration of the ferrous gluconate solution in the step (1) is 2mol/L, the concentration of the boric acid solution is 1.2mol/L, a centrifugal spray dryer is adopted for spray drying, the rotating speed of a centrifugal atomizing wheel is 18000r/min, the air inlet temperature in the atomizing process is 250 ℃, the discharging temperature is 87 ℃, the particle size of atomized liquid drops is less than or equal to 50 mu m, and the particle size of a spray-dried material is 10.5 mu m.
And (3) sintering the spray drying material in the step (2) in a methane atmosphere, wherein the calcining process comprises a heating process and a heat preservation process, the heating rate of the heating process is 150 ℃/h, an induced draft fan is started in the heating process, waste gas generated in the heating process is discharged through the induced draft fan, the humidity in the sintering furnace in the heating process is maintained to be less than or equal to 20%, then the induced draft fan is closed in the heat preservation process, and natural air exhaust is adopted.
The volume of methane gas introduced per hour in the step (2) is 500 times of the volume of the charged spray-dried material.
And (3) introducing the carbon dioxide with the volume 350 times of the volume of the charged spray drying material per hour in the step (3), cooling the sintered material until the material temperature of the material is less than or equal to 60 ℃, and discharging the material.
And (4) performing jet milling by using high-pressure nitrogen as a gas source under the pressure of 6 atmospheric pressures, grading by using a grading wheel, controlling the grain size of discharged materials to be 1.7 mu m, sieving by using a 200-mesh sieve, and performing vacuum packaging to obtain the superfine iron boride.
The detection data of the finally obtained basic ammonium ferric phosphate are as follows:
index (I) D10 D50 D90 BET Fe
Numerical value 0.5μm 1.7μm 4.4μm 18.3m2/g 83.55％
B O Tap density Ni Mn Co
16.31％ 0.05％ 3.69g/mL 6.2ppm 10.1ppm 7.4ppm
Cd Cu Zn Ca C P
0.1ppm 0.1ppm 0.2ppm 4.1ppm 0.18％ 0.0046％
As shown in fig. 1, 2 and 3, SEM of the products obtained in examples 1, 2 and 3 according to the present invention shows that a large number of pores are generated due to the decomposition of carbon, i.e., the reaction of carbon dioxide with carbon to obtain carbon monoxide, and the escape of carbon monoxide, and that the products are burst-shaped, have a very non-smooth surface, a large specific surface area and a small particle size.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.

Claims (6)

1. The preparation method of the superfine iron boride is characterized by comprising the following steps:
(1) mixing the ferrous gluconate solution with the boric acid solution, and performing spray drying to obtain a spray-dried material, wherein the molar ratio of the ferrous gluconate solution to the boric acid is 1: 1.01-1.02;
(2) sintering the spray-dried material in a methane atmosphere for 5-10h at 800-1200 ℃ to obtain a reducing material;
(3) continuously introducing carbon dioxide into the reducing material, and reacting at the temperature of 700-850 ℃ for 2-4h to obtain a sintering material;
(4) and (3) performing jet milling, screening and vacuum packaging on the sintered material to obtain the superfine iron boride.
2. The method for preparing ultra-fine iron boride according to claim 1, wherein: the concentration of the ferrous gluconate solution in the step (1) is 1.5-3mol/L, the concentration of the boric acid solution is 1-2mol/L, a centrifugal spray dryer is adopted for spray drying, the rotating speed of a centrifugal atomizing wheel is 15000-20000r/min, the air inlet temperature in the atomizing process is 200-300 ℃, the discharging temperature is less than or equal to 90 ℃, the particle size of atomized liquid drops is less than or equal to 50 mu m, and the particle size of a spray drying material is less than or equal to 20 mu m.
3. The method for preparing ultra-fine iron boride according to claim 1, wherein: and (3) sintering the spray drying material in the step (2) in a methane atmosphere, wherein the calcining process comprises a heating process and a heat preservation process, the heating rate of the heating process is 100-.
4. The method for preparing ultra-fine iron boride according to claim 1, wherein: the volume of the methane gas introduced per hour in the step (2) is 800 times of 300 times of the volume of the filled spray-dried material.
5. The method for preparing ultra-fine iron boride according to claim 1, wherein: and (4) in the step (3), the volume of carbon dioxide introduced per hour is 500 times of the volume of the filled spray drying material, and the material is discharged after the sintering is finished and the material temperature of the material is cooled to be less than or equal to 60 ℃.
6. The method for preparing ultra-fine iron boride according to claim 1, wherein: and (4) performing jet milling by using high-pressure nitrogen as a gas source under the pressure of 4-7 atmospheric pressures, grading by using a grading wheel, controlling the grain size of discharged materials to be less than or equal to 3 microns, sieving by using a 200-mesh sieve, and performing vacuum packaging to obtain the superfine iron boride.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5225000A (en) * 1975-08-21 1977-02-24 Komatsu Ltd Method for production of feb powder
CN101921114A (en) * 2010-09-15 2010-12-22 胡建东 High-purity titanium boride (TiB) ceramic powder with face-centered cubic structure and preparation method thereof
CN102328935A (en) * 2011-04-12 2012-01-25 西安交通大学 Method for preparing blocky Fe2B compound with zinc liquid corrosion resistance
CN105304944A (en) * 2014-07-28 2016-02-03 北京理工大学 Alkaline secondary battery taking boride prepared through reversed-phase microemulsion method as anode material
CN105322160A (en) * 2014-07-28 2016-02-10 北京理工大学 Alkaline secondary battery taking boride prepared by micro-emulsion method as negative electrode material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5225000A (en) * 1975-08-21 1977-02-24 Komatsu Ltd Method for production of feb powder
CN101921114A (en) * 2010-09-15 2010-12-22 胡建东 High-purity titanium boride (TiB) ceramic powder with face-centered cubic structure and preparation method thereof
CN102328935A (en) * 2011-04-12 2012-01-25 西安交通大学 Method for preparing blocky Fe2B compound with zinc liquid corrosion resistance
CN105304944A (en) * 2014-07-28 2016-02-03 北京理工大学 Alkaline secondary battery taking boride prepared through reversed-phase microemulsion method as anode material
CN105322160A (en) * 2014-07-28 2016-02-10 北京理工大学 Alkaline secondary battery taking boride prepared by micro-emulsion method as negative electrode material

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