CN106830719B - Preparation method of magnesium oxide for high-temperature HiB steel - Google Patents
Preparation method of magnesium oxide for high-temperature HiB steel Download PDFInfo
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- CN106830719B CN106830719B CN201710211894.2A CN201710211894A CN106830719B CN 106830719 B CN106830719 B CN 106830719B CN 201710211894 A CN201710211894 A CN 201710211894A CN 106830719 B CN106830719 B CN 106830719B
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- C—CHEMISTRY; METALLURGY
- 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
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Abstract
The invention relates to a preparation method of magnesium oxide for high-temperature HiB steel, in particular to a preparation method of magnesium oxide for high-temperature HiB steel, which improves the quality of the existing high-temperature HiB steel. Calcining dolomite, combining with water, carbonizing in a carbonizing tower, and filtering to separate solid calcium carbonate and magnesium bicarbonate water solution. Adding boric acid into the obtained magnesium bicarbonate water solution, carrying out pyrolysis filtration to obtain magnesium carbonate, calcining step by step, and carrying out jet milling and packaging to obtain the magnesium oxide for the high-temperature HiB steel. The method has the advantages of unique production process, low cost, no generation of three wastes, capability of obviously improving the magnetic induction strength of the high-temperature HiB steel and reducing the iron loss, and can be purposefully popularized and used in high-temperature HiB steel manufacturers.
Description
Technical Field
The invention relates to the field of oriented silicon steel sheet manufacturing, in particular to a preparation method of magnesium oxide for high-temperature HiB steel.
Background
In addition to the use of beneficial additives during the manufacture of high temperature HiB steel, it is most important to use magnesium oxide for high temperature HiB steel. Which is a high-temperature annealing separant and an insulating coating generating agent in the current high-temperature HiB steel production. The main mechanism is that magnesium oxide is coated on the surface of silicon steel and then generates a forsterite film (reaction formula 2MgO + SiO) with silicon in the silicon steel at high temperature (1200 ℃, 7 multiplied by 24 h)2→Mg2SiO4). The forsterite film has high electrical insulation, and the difference of expansion rates between the forsterite film and the silicon steel sheet substrate endows tension to the surface of the silicon steel sheet, so that the forsterite film has a Gaussian structure, refines magnetic domains and further optimizes the orientation effect.
At present, domestic enterprises for preparing high-temperature HiB steel only have Wu steel. On the basis of the practical use of the magnesium oxide for the high-performance silicon steel, the iron loss (P) can be met17) Less than or equal to 1.05W/Kg, magnetic induction intensity (B)8) Not less than 1.92T. As the requirements of customers are continuously improved, the iron loss (P) of the HiB steel product at high temperature is urgently required by the Wu Steel17) Less than or equal to 1.00W/Kg, magnetic induction intensity (B)8) Not less than 1.93T, in order to meet the use quality requirement, the magnesium oxide process for high-performance silicon steel is optimized, and the magnesium oxide for preparing the high-temperature HiB steel is not slow enough.
Disclosure of Invention
The invention provides a preparation method of magnesium oxide for high-temperature HiB steel, aiming at improving the quality of the existing magnesium oxide for high-temperature HiB steel.
The invention is realized by adopting the following technical scheme: a preparation method of magnesium oxide for high-temperature HiB steel comprises the following process steps:
(1) calcining dolomite: mixture of dolomite magnesium carbonate and calcium carbonate. Calcining at the high temperature of 900 ℃ and the temperature of 1000 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide.
(2) Hydration: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: 10 to 15 ℃, reacting in an ash dissolving tank at the temperature of 60 to 80 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction.
(3) Carbonizing: introducing purified 28-38% carbon dioxide into a carbonization tower, and carbonizing in the turbid liquid of magnesium hydroxide and calcium hydroxide at carbonization pressure of 0.25-0.35MPa and carbonization temperature of 25-40 deg.C to obtain solid calcium carbonate and liquid magnesium bicarbonate, respectively.
(4) And (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate water solution.
(5) Adding boron: boric acid with the content of 99.9 percent is added into the magnesium bicarbonate water solution, and the final boron content in the solution is controlled to be 500-1000 ppm.
(6) Pyrolysis: heating the magnesium bicarbonate water solution added with boron in a pyrolysis tank at 90-100 ℃ to obtain a basic magnesium carbonate product.
(7) And (3) filtering: and filtering the pyrolyzed magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 75-85%.
(8) Primary calcination: calcining the filtered basic magnesium carbonate at the temperature of 700 ℃ and 800 ℃ to obtain magnesium carbonate with the MgO content of 40-45%.
(9) Secondary calcination: calcining the magnesium carbonate subjected to primary calcination at the temperature of 1000-1100 ℃ to obtain the magnesium oxide with the purity of more than 98.5 percent.
(10) Airflow crushing: after high-temperature calcination, cooling the magnesium oxide, and then carrying out gas flow crushing to obtain powder with fine particle size and certain distribution.
According to the preparation method of the magnesium oxide for the high-temperature HiB steel, the water used in the step (2) is pyrolysis wastewater and softened water treated by resin, and the conductivity of the softened water is less than or equal to 100 mus/cm, so that the solubility of soluble salts is increased.
The preparation raw material of the magnesium oxide for the high-temperature HiB steel and the mechanism for improving the quality of the oriented silicon steel are as follows:
1. raw materials
Dolomite: the process selects and uses the dolomite which is smooth and rich in local reserves. The main technical indexes are MgO: 20-23%, CaO: 26-30%, Fe: 0.07-0.15 percent.
2. Mechanism for improving quality of oriented silicon steel sheet
The main mechanism is that the crystal form grain size of the magnesium oxide tends to grow up after the pyrolysis temperature is increased and boric acid is added, the original 200nm is changed into 300nm, the air permeability of the moisture removal process after the magnesium oxide is coated is increased, and the hydration rate is reduced. At high temperature (1200 ℃, 7 multiplied by 24 h), the forsterite film is generated with silicon in the silicon steel (reaction formula 2MgO + SiO)2→Mg2SiO4). The forsterite film has high electrical insulation, and the difference of expansion rates between the forsterite film and the silicon steel sheet substrate endows tension to the surface of the silicon steel sheet, so that the forsterite film has a Gaussian structure, refines magnetic domains and further optimizes the orientation effect.
The magnesium oxide for high-temperature HiB steel prepared by the preparation method provided by the invention meets the quality requirement of the magnesium oxide for high-temperature HiB steel of the military steel through the detection of a military steel quality inspection center. The results of the tests obtained are shown in the following table:
| item | Check value |
| Content of magnesium oxide (MgO), percent | 98.6 |
| Content of calcium oxide (CaO), percent | 0.30 |
| Sulfate (SO)4) Content (a) of | 0.20 |
| Chloride (Cl) content,% ] | 0.010 |
| Iron (Fe) content% | 0.013 |
| Content of residue on sieve (320 mesh)% | 0.02 |
| Hydration rate% | 2.10 |
| Boron (B) content, ppm | 680 |
| Particle size (D50), um | 5.1 |
| Particle size (D90), um | 15.7 |
In order to verify the effect of the magnesium oxide for high-temperature HiB steel in practical use, the present inventors made an on-line test of magnesium oxide to the department of the silicon-steel industry for wulfproducts. The analytical reports show that the iron loss (P) after the use of magnesium oxide for high-temperature HiB steel in the manufacture of high-temperature HiB steel is compared with that after the use of magnesium oxide for high-performance silicon steel17) The magnetic induction intensity is reduced by 0.05W/Kg (B)8) The improvement is more than or equal to 0.01T.
In a word, compared with the prior art, the magnesium oxide for the high-temperature HiB steel is produced by using dolomite as a raw material, has no three-waste pollution, simple production process and lower cost, and can be pertinently supplied to the high-temperature HiB steel for use.
Detailed Description
Example 1:
a preparation method of magnesium oxide for high-temperature HiB steel comprises the following process steps: (1) calcining dolomite: calcining dolomite at high temperature of 900 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide. (2) Hydration: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: 10, reacting in an ash dissolving tank at the temperature of 60 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction. (3) Carbonizing: introducing purified carbon dioxide (with concentration of 28%) into a carbonization tower, and carbonizing in the magnesium hydroxide calcium hydroxide turbid liquid (carbonization pressure of 0.25MPa and carbonization temperature of 25 ℃) filled in advance to obtain solid calcium carbonate and liquid magnesium bicarbonate respectively. (4) And (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate water solution. (5) Adding boron: reacting boric acid (H)3BO3Content 99.9%) was added to an aqueous solution of magnesium bicarbonate (final boron content controlled at 500-. (6) Pyrolysis: heating the magnesium bicarbonate water solution in a pyrolysis tank at 90 ℃ to obtain a basic magnesium carbonate product. (7) And (3) filtering: and filtering the pyrolyzed magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 75%. (8) Primary calcination: the basic magnesium carbonate was calcined at 700 ℃ to obtain magnesium carbonate (MgO: 40%). (9) Secondary calcination: calcining magnesium carbonate at 1000 deg.C to obtain magnesium oxide (MgO is greater than or equal to 98.5%). (10) Airflow crushing: after high-temperature calcination, the magnesium oxide needs to be cooled and then is pulverized by gas flow. The powder with fine granularity and certain distribution is obtained. (11) Packaging: 20Kg per bag and packaging by kraft paper.
Example 2:
a preparation method of magnesium oxide for high-temperature HiB steel comprises the following process steps: (1) calcining dolomite: calcining dolomite at a high temperature of 920 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide. (2) Hydration of: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: 11, reacting in an ash dissolving tank at the temperature of 65 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction. (3) Carbonizing: introducing purified carbon dioxide (with concentration of 30%) into a carbonization tower, and carbonizing in the magnesium hydroxide calcium hydroxide turbid liquid (carbonization pressure of 0.28MPa and carbonization temperature of 28 ℃) filled in advance to obtain solid calcium carbonate and liquid magnesium bicarbonate respectively. (4) And (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate water solution. (5) Adding boron: reacting boric acid (H)3BO3Content 99.9%) was added to an aqueous solution of magnesium bicarbonate (final boron content controlled at 500-. (6) Pyrolysis: heating the magnesium bicarbonate water solution in a pyrolysis tank at 93 ℃ to obtain a basic magnesium carbonate product. (7) And (3) filtering: and filtering the pyrolyzed magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 78%. (8) Primary calcination: the basic magnesium carbonate was calcined at 720 ℃ to obtain magnesium carbonate (MgO: 41%). (9) Secondary calcination: calcining magnesium carbonate at 1020 ℃ to obtain magnesium oxide (MgO is more than or equal to 98.5%). (10) Airflow crushing: after high-temperature calcination, the magnesium oxide needs to be cooled and then is pulverized by gas flow. The powder with fine granularity and certain distribution is obtained. (11) Packaging: 20Kg per bag and packaging by kraft paper.
Example 3:
a preparation method of magnesium oxide for high-temperature HiB steel comprises the following process steps: (1) calcining dolomite: calcining dolomite at high temperature of 950 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide. (2) Hydration: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: 12, reacting in an ash dissolving tank at the temperature of 70 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction. (3) Carbonizing: introducing purified carbon dioxide (with concentration of 32%) into a carbonization tower, and carbonizing in the magnesium hydroxide calcium hydroxide turbid liquid (carbonization pressure of 0.30MPa and carbonization temperature of 30 ℃) filled in advance to obtain solid calcium carbonate and liquid magnesium bicarbonate respectively. (4) And (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate water solution. (5) Adding boron:reacting boric acid (H)3BO3Content 99.9%) was added to an aqueous solution of magnesium bicarbonate (final boron content controlled at 500-. (6) Pyrolysis: heating the magnesium bicarbonate water solution in a pyrolysis tank at 95 ℃ to obtain a basic magnesium carbonate product. (7) And (3) filtering: and filtering the pyrolyzed magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 80%. (8) Primary calcination: the basic magnesium carbonate was calcined at 750 ℃ to obtain magnesium carbonate (MgO: 43%). (9) Secondary calcination: calcining magnesium carbonate at 1050 ℃ to obtain magnesium oxide (MgO is more than or equal to 98.5%). (10) Airflow crushing: after high-temperature calcination, the magnesium oxide needs to be cooled and then is pulverized by gas flow. The powder with fine granularity and certain distribution is obtained. (11) Packaging: 20Kg per bag and packaging by kraft paper.
Example 4:
a preparation method of magnesium oxide for high-temperature HiB steel comprises the following process steps: (1) calcining dolomite: calcining dolomite at high temperature of 980 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide. (2) Hydration: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: 13, reacting in an ash dissolving tank at the temperature of 75 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction. (3) Carbonizing: introducing purified carbon dioxide (with concentration of 35%) into a carbonization tower, and carbonizing in the magnesium hydroxide calcium hydroxide turbid liquid (carbonization pressure of 0.32MPa and carbonization temperature of 35 ℃) filled in advance to obtain solid calcium carbonate and liquid magnesium bicarbonate respectively. (4) And (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate water solution. (5) Adding boron: reacting boric acid (H)3BO3Content 99.9%) was added to an aqueous solution of magnesium bicarbonate (final boron content controlled at 500-. (6) Pyrolysis: heating the magnesium bicarbonate water solution in a pyrolysis tank at 98 ℃ to obtain a basic magnesium carbonate product. (7) And (3) filtering: and filtering the pyrolyzed magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 82%. (8) Primary calcination: the basic magnesium carbonate was calcined at 780 ℃ to obtain magnesium carbonate (MgO: 44%). (9) Secondary calcination: calcining magnesium carbonate at 1080 deg.C to obtainMagnesium oxide (MgO is more than or equal to 98.5%). (10) Airflow crushing: after high-temperature calcination, the magnesium oxide needs to be cooled and then is pulverized by gas flow. The powder with fine granularity and certain distribution is obtained. (11) Packaging: 20Kg per bag and packaging by kraft paper.
Example 5:
a preparation method of magnesium oxide for high-temperature HiB steel comprises the following process steps: (1) calcining dolomite: calcining dolomite at high temperature of 1000 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide. (2) Hydration: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: 15, reacting in an ash dissolving tank at the temperature of 80 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction. (3) Carbonizing: introducing purified carbon dioxide (concentration 38%) into a carbonization tower, and carbonizing in the magnesium hydroxide calcium hydroxide turbid liquid (carbonization pressure 0.35MPa, carbonization temperature 40 ℃) filled in advance to obtain solid calcium carbonate and liquid magnesium bicarbonate respectively. (4) And (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate water solution. (5) Adding boron: reacting boric acid (H)3BO3Content 99.9%) was added to an aqueous solution of magnesium bicarbonate (final boron content controlled at 500-. (6) Pyrolysis: heating the magnesium bicarbonate water solution in a pyrolysis tank at 100 ℃ to obtain a basic magnesium carbonate product. (7) And (3) filtering: and filtering the pyrolyzed magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 85%. (8) Primary calcination: the basic magnesium carbonate was calcined at 800 ℃ to obtain magnesium carbonate (MgO: 45%). (9) Secondary calcination: calcining magnesium carbonate at 1100 deg.C to obtain magnesium oxide (MgO is greater than or equal to 98.5%). (10) Airflow crushing: after high-temperature calcination, the magnesium oxide needs to be cooled and then is pulverized by gas flow. The powder with fine granularity and certain distribution is obtained. (11) Packaging: 20Kg per bag and packaging by kraft paper.
Claims (2)
1. The preparation method of the magnesium oxide for the high-temperature HiB steel is characterized by comprising the following process steps:
(1) calcining dolomite: calcining dolomite at high temperature of 900 ℃ and 1000 ℃ in a shaft kiln to obtain a mixture of carbon dioxide gas, magnesium oxide and calcium oxide;
(2) hydration: mixing a mixture of magnesium oxide and calcium oxide with water in a mass ratio of 1: reacting in an ash dissolving tank at the temperature of between 10 and 15 ℃ and between 60 and 80 ℃, and obtaining magnesium hydroxide and calcium hydroxide through hydration reaction;
(3) carbonizing: introducing purified 28-38% carbon dioxide into a carbonization tower, and carbonizing in a turbid solution of magnesium hydroxide and calcium hydroxide which is filled in the carbonization tower in advance, wherein the carbonization pressure is 0.25-0.35MPa, the carbonization temperature is 25-40 ℃, and the products are solid calcium carbonate and liquid magnesium bicarbonate respectively;
(4) and (3) filtering: filtering with a plate-and-frame filter press to obtain calcium carbonate solid and magnesium bicarbonate aqueous solution;
(5) adding boron: adding 99.9 percent boric acid into a magnesium bicarbonate aqueous solution, and controlling the final boron content to be 500-1000 ppm;
(6) pyrolysis: heating the magnesium bicarbonate water solution added with boron in a pyrolysis tank at 90-100 ℃ to obtain a basic magnesium carbonate product;
(7) and (3) filtering: filtering the pyrolyzed basic magnesium carbonate in a plate-and-frame filter press to obtain basic magnesium carbonate solid with the water content of 75-85%;
(8) primary calcination: calcining the filtered basic magnesium carbonate at the temperature of 700 ℃ and 800 ℃ to obtain magnesium carbonate with the MgO content of 40-45%;
(9) secondary calcination: calcining the magnesium carbonate subjected to primary calcination at the temperature of 1000-1100 ℃ to obtain magnesium oxide with the purity of more than or equal to 98.5%;
(10) airflow crushing: after high-temperature calcination, cooling the magnesium oxide, and then carrying out gas flow crushing to obtain powder with fine particle size and certain distribution.
2. The method for preparing the magnesium oxide for the high-temperature HiB steel according to claim 1, wherein the water used in the step (2) is pyrolysis wastewater and softened water treated by resin, and the electrical conductivity of the softened water is less than or equal to 100 μ s/cm.
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| CN101891219A (en) * | 2010-08-20 | 2010-11-24 | 山西宏亚科技有限责任公司 | Method for preparing special magnesium borate for oriented silicon steel |
| CN105271845A (en) * | 2015-11-18 | 2016-01-27 | 和顺银圣化工有限公司 | Method for preparing magnesium oxide for high-performance silicon steel through dolomite |
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| CN101891219A (en) * | 2010-08-20 | 2010-11-24 | 山西宏亚科技有限责任公司 | Method for preparing special magnesium borate for oriented silicon steel |
| CN105271845A (en) * | 2015-11-18 | 2016-01-27 | 和顺银圣化工有限公司 | Method for preparing magnesium oxide for high-performance silicon steel through dolomite |
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