CN115676858B - Preparation method of flaky porous silicon steel grade magnesium oxide - Google Patents
Preparation method of flaky porous silicon steel grade magnesium oxide Download PDFInfo
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- CN115676858B CN115676858B CN202211384844.1A CN202211384844A CN115676858B CN 115676858 B CN115676858 B CN 115676858B CN 202211384844 A CN202211384844 A CN 202211384844A CN 115676858 B CN115676858 B CN 115676858B
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 78
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 33
- 239000010959 steel Substances 0.000 title claims abstract description 33
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims description 17
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 25
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 25
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 25
- 238000003763 carbonization Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 14
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 13
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 14
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 3
- 239000011736 potassium bicarbonate Substances 0.000 claims description 3
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 3
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 27
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000010000 carbonizing Methods 0.000 abstract description 3
- 150000002681 magnesium compounds Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract description 2
- 238000007710 freezing Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 4
- 239000001099 ammonium carbonate Substances 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 210000004243 sweat Anatomy 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- JTXJZBMXQMTSQN-UHFFFAOYSA-N amino hydrogen carbonate Chemical compound NOC(O)=O JTXJZBMXQMTSQN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910017625 MgSiO Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002370 magnesium bicarbonate Substances 0.000 description 1
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 description 1
- 235000014824 magnesium bicarbonate Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a process for preparing flaky porous silicon steel grade magnesium oxide, which comprises the following steps: and adopting a wide temperature range-wide temperature difference strategy, and rapidly calcining the magnesium hydroxide after freezing liquid nitrogen to prepare the light-burned magnesium oxide. Adding high-temperature light-burned magnesium oxide into the carbonized liquid, carbonizing and aging. And aging and filtering to obtain basic magnesium carbonate. Calcining basic magnesium carbonate to obtain the flaky porous silicon steel grade magnesium oxide. According to the scheme, magnesium hydroxide is used as a raw material to prepare flaky porous silicon steel grade magnesium oxide, a light-burned magnesium oxide template is formed by using a wide temperature range-wide temperature difference strategy, and the flaky porous silicon steel grade magnesium oxide is obtained after carbonization and aging calcination. The scheme II related by the invention is as follows: the method comprises the steps of taking magnesium compound powder which is calcined to generate light magnesium oxide raw material powder as a treatment object; the treatment object is placed in ultralow temperature for heat preservation, and then sintered. The silicon steel grade magnesium oxide prepared by the invention has controllable apparent specific volume and morphology, stable product quality and high production efficiency, and meets the industrial production requirement.
Description
Technical Field
The invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, and belongs to the technical field of magnesium oxide preparation.
Background
The Qinghai Bohr sweat salt lake contains rich resources such as potassium and lithium, and a large amount of bischofite can be generated in the process of developing Bohr sweat salt lake resources, and the Qinghai Bohr sweat salt lake is locally called as 'magnesium hazard'. Magnesium is deposited by ammonia method by Qinghai western magnesium industry Co., ltd, and magnesium hydroxide products are prepared on a large scale by using bischofite as a raw material. In order to further improve the added value of magnesium products, a process for preparing the flaky porous silicon steel grade magnesium oxide from magnesium hydroxide is researched. The process can greatly improve the product value, has great economic benefit, and lays a foundation for realizing diversification, serialization and scale production of high-end magnesium-based compound products in China.
The silicon steel grade magnesium oxide is one of light magnesium oxide, the purity requirement is more than 98%, the suspension performance in water is good, the hydration rate is low, the silicon steel grade magnesium oxide is coated between silicon steel sheets in the form of suspension in the process of producing oriented silicon steel sheets, and an MgSiO 3 insulating layer is formed with silicate in the high-temperature annealing process, and the effects of dephosphorization and desulfurization are achieved. The magnesium resources in China are rich, however, the market share of high-end magnesium products is lower. With the progress of economy and science in China, large enterprises such as armed steel, bao steel and the like have started to produce oriented silicon steel sheets, and only enterprises such as Shanghai Zhengtai and the like in China can produce silicon steel grade magnesium oxide products meeting the quality standards of the enterprises. The silicon steel grade magnesia market is currently under further development.
However, the current silicon steel grade magnesium oxide has long process flow, low purity and unstable product quality, and cannot meet the demands of the production development of oriented silicon steel sheets which are rapidly growing in China. The ammonium bicarbonate is mainly used as a carbonizing agent in the production of silicon steel grade magnesium oxide from salt lake magnesium resources, and the prepared silicon steel grade magnesium oxide product has higher apparent specific volume. The mass ratio of water in the silicon steel magnesium oxide suspension is severely limited in production, and if the mass ratio of water is too high, the silicon steel plate can rust. Under the condition that the mass percentage of water and magnesium oxide is limited, the magnesium oxide prepared from ammonium bicarbonate has high apparent specific volume, small density and overlarge volume, so that the magnesium oxide cannot be effectively dispersed in suspension; silicon steel grade magnesium oxide prepared from ammonium bicarbonate is limited in the use process of enterprises.
The existing magnesium oxide preparation method does not use a wide temperature range-wide temperature difference process, and no report of preparing flaky porous silicon steel grade magnesium oxide exists.
Disclosure of Invention
Aiming at the defects of the silicon steel grade magnesium oxide preparation process in the prior art, the invention provides a process for preparing the flaky porous silicon steel grade magnesium oxide by adopting ultralow temperature to treat magnesium hydroxide raw material powder or calcining to generate magnesium compound powder of light magnesium oxide raw material powder such as magnesium carbonate, bicarbonate, basic magnesium carbonate and the like and matching with corresponding processes.
The invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, which comprises at least one of the following schemes;
Taking magnesium hydroxide as a treatment object, and obtaining light-burned magnesium oxide by utilizing a wide temperature range-wide temperature difference strategy; (2) Adding the high-temperature light-burned magnesia into the carbonized liquid for carbonization and aging, and filtering to obtain basic magnesium carbonate; (3) Washing, drying and calcining basic magnesium carbonate to obtain flaky porous silicon steel grade magnesium oxide; wherein the wide temperature range is to enlarge the temperature range by using the environment with the temperature less than-50 ℃, and the temperature of the magnesium hydroxide is reduced to-50 ℃ in the environment, and the heat is preserved;
In the second scheme, at least one of magnesium compound powder such as magnesium carbonate, bicarbonate and basic magnesium carbonate which are calcined to generate light magnesium oxide raw material powder is used as a treatment object; firstly, placing a treatment object at ultralow temperature for heat preservation, and then sintering; obtaining flaky porous silicon steel grade magnesium oxide; the ultra-low temperature refers to an environment with a temperature less than or equal to-50 ℃.
Preferably, the invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, in the scheme I, the wide temperature range is to enlarge the temperature range by utilizing liquid nitrogen, magnesium hydroxide is placed in the liquid nitrogen, the temperature is reduced to minus 180 ℃ to minus 196 ℃, and the temperature is kept for 1 to 4 hours.
Preferably, the invention is a preparation method of flaky porous silicon steel grade magnesium oxide, and the purity of magnesium hydroxide raw material is more than 98.5%.
Preferably, the invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, in the scheme one, the wide temperature difference is a temperature rising process of quickly rising temperature to reach wide temperature difference gradient, magnesium hydroxide is placed in a furnace, the temperature is raised to 610-800 ℃ at a temperature rising speed of 8-10 ℃/min, uniformly stirred, kept for 0.5-5h, and cooled to 100-200 ℃.
Preferably, the invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, in the scheme I, light burned magnesium oxide with the temperature of 100-200 ℃ is directly added into carbonized liquid.
Preferably, the invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, wherein in the scheme I, the carbonized liquid consists of one or more of sodium bicarbonate and potassium bicarbonate.
Preferably, the invention is a preparation method of flaky porous silicon steel grade magnesium oxide, in the scheme I, the carbonization time is 1-4 h, preferably 2-4 h, and the carbonization temperature is 70-100 ℃.
Preferably, the invention is a preparation method of flaky porous silicon steel grade magnesium oxide, the adding rate of the carbonization liquid is 0.1-0.3L/h, wherein the concentration of the solution of bicarbonate is 0.1-0.8 mol/L, preferably 0.2-0.8 mol/L, and the adding amount of the bicarbonate is 0.1-0.9 times, preferably 0.2-0.8 times of the theoretical molar amount of carbonization reaction.
Preferably, the invention relates to a preparation method of flaky porous silicon steel grade magnesium oxide, in the scheme I, the aging reaction time is 1-5h, preferably 2-5 h, and the stirring speed is 100-400r/min, preferably 100-350r/min.
Preferably, the invention is a preparation method of flaky porous silicon steel grade magnesium oxide, in the first scheme, the calcination process is as follows: placing the filter residue after washing and drying in a furnace, and heating to 850-1150 ℃ at a heating rate of 5-8 ℃/min for calcination.
According to the scheme I, the wide temperature range-wide temperature difference strategy is adopted to match the optimized carbonizing agent, so that the magnesia with the porous flaky morphology can be obtained, and the apparent specific volume of the magnesia can be further reduced; solving the pain point of the current silicon steel grade magnesium oxide process; the prepared silicon steel grade magnesia has stable quality and high production efficiency and meets the industrial production requirement.
The purity of the product obtained by the invention is more than 99.5 percent. The apparent specific volume is 3.3-5.2ml/g.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
1. the wide temperature range-wide temperature difference strategy of the invention utilizes liquid nitrogen to cool down and expand the temperature range, and rapidly heats up to realize wide temperature difference in the calcining process, thereby achieving the purpose of controlling the appearance of magnesium oxide.
2. The flaky porous magnesium oxide prepared by the invention is easy to disperse in water and easy to prepare silicon steel grade magnesium oxide suspension.
3. The flaky porous magnesia prepared by the invention has lower apparent specific volume, improves the solid content in the silicon steel grade magnesia suspension, and meets the industrial use requirement.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is an XRD analysis pattern of sheet-like porous silicon steel grade magnesium oxide obtained in example 3 of the scheme.
FIG. 3 is an SEM image of sheet-like porous silicon steel grade magnesium oxide obtained in example 3.
FIG. 4 is a graph showing the particle size distribution of the flaky porous silicon steel grade magnesium oxide obtained in example 3.
FIG. 5 is a photograph of a sheet-like porous silica steel grade magnesium oxide suspension of embodiment 3 after annealing on the surface of a silicon steel sheet.
FIG. 6 is an SEM image of the flaky porous silicon steel grade magnesium oxide obtained in example 4 of scheme II.
FIG. 7 is an SEM image of the silicon steel grade magnesium oxide obtained in comparative example 3.
FIG. 8 is a photograph of a silicon steel grade magnesium oxide suspension of comparative example 3 after annealing on the surface of a silicon steel sheet.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following further description of the present invention is provided in connection with the embodiments, and it should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1 scheme one
And (1) placing magnesium hydroxide (purity is 98.7%) in liquid nitrogen, cooling to-190 ℃ and preserving heat for 2h, taking out the magnesium hydroxide, placing the magnesium hydroxide in a furnace, heating to 650 ℃ at a heating rate of 8 ℃/min, uniformly stirring, preserving heat for 3h, and naturally cooling to 100 ℃.
Step (2): the magnesium oxide at 100 ℃ is added into the carbonization liquid, the adding rate of the sodium bicarbonate solution is 0.2L/h, the concentration of the bicarbonate solution is 0.5mol/L, and the adding amount of the bicarbonate is 0.8 times of the theoretical molar amount of the carbonization reaction. The carbonization reaction temperature is 70 ℃, and the carbonization time is 2 hours. The aging reaction time is 2 hours, and the stirring speed is 100r/min. And filtering by a plate filter press.
Step (3): and drying by adopting a flash dryer, wherein the air inlet temperature of the dryer is 240 ℃, the mixing temperature is 110 ℃, and the air outlet temperature is 110 ℃. Placing the filter residue after washing and drying in a furnace, heating to 1000 ℃ at a heating rate of 8 ℃/min, and calcining for 1h.
The purity of the magnesium oxide product is 99.6%, and the apparent specific volume is 5.1ml/g.
Example 2 scheme one
And (1) placing magnesium hydroxide (purity is more than 99%) in liquid nitrogen, cooling to-195 ℃ and preserving heat for 3H, taking out the magnesium hydroxide, placing the magnesium hydroxide in a furnace, heating to 680 ℃ at a heating rate of 8 ℃/min, uniformly stirring, preserving heat for 2H, and naturally cooling to 150 ℃.
Step (2): magnesium oxide at 150 ℃ is directly added into the carbonization liquid, the adding rate of potassium bicarbonate solution is 0.3L/h, the concentration of bicarbonate solution is 0.6mol/L, and the adding amount of bicarbonate is 0.7 times of the theoretical molar amount of carbonization reaction. The carbonization reaction temperature is 80 ℃ and the carbonization time is 2.5h. The aging reaction time is 3 hours, and the stirring speed is 150r/min. And filtering by a plate filter press.
Step (3): and drying by adopting a flash dryer, wherein the air inlet temperature of the dryer is 240 ℃, the mixing temperature is 115 ℃, and the air outlet temperature is 105 ℃. Placing the washed and dried filter residues into a furnace, heating to 1100 ℃ at a heating rate of 8 ℃/min, and calcining for 1.5h.
The purity of the magnesium oxide product is 99.7%, and the apparent specific volume is 4.7ml/g.
Example 3 scheme one
And (1) placing magnesium hydroxide (purity is 99.2%) in liquid nitrogen, cooling to-195 ℃ and preserving heat for 3H, taking out the magnesium hydroxide, placing the magnesium hydroxide in a furnace, heating to 680 ℃ at a heating rate of 10 ℃/min, uniformly stirring, preserving heat for 3H, and naturally cooling to 200 ℃.
Step (2): adding magnesium oxide into carbonization liquid at 200 ℃, wherein the adding rate of sodium bicarbonate solution is 0.25L/h, the concentration of bicarbonate solution is 0.8mol/L, and the adding amount of bicarbonate is 0.6 times of the theoretical molar amount of carbonization reaction. The carbonization reaction temperature is 90 ℃, and the carbonization time is 3 hours. The aging reaction time is 3.5h, and the stirring speed is 200r/min. And filtering by a plate filter press. Basic magnesium carbonate is shown in fig. 2.
Step (3): and drying by adopting a flash dryer, wherein the air inlet temperature of the dryer is 240 ℃, the mixing temperature is 115 ℃, and the air outlet temperature is 105 ℃. Placing the washed and dried filter residues into a furnace, heating to 1100 ℃ at a heating rate of 8 ℃/min, and calcining for 2 hours.
The purity of the magnesium oxide product is 99.7%, the apparent specific volume is 3.4ml/g, and the median particle diameter is 4.4um. XRD and SEM patterns are shown in fig. 2 and 3. The particle size distribution is shown in FIG. 4. The magnesium oxide is flaky and porous in appearance. Fig. 5 is a photograph of magnesium oxide after annealing of a silicon steel sheet, without punctate crystal dew.
Example 4 (scheme two)
Placing basic magnesium carbonate (purity 99.5%) into liquid nitrogen, cooling to-195 ℃ and preserving heat for 3H, taking out the basic magnesium carbonate, placing into a furnace, heating to 750 ℃ at a heating rate of 10 ℃/min, uniformly stirring, preserving heat for 2H, and naturally cooling to room temperature. The purity of the magnesium oxide product is 99.6%, and the apparent specific volume is 4.1ml/g. SEM fig. 6. The magnesium oxide is flaky and porous in appearance.
Comparative example 1
15G (purity 99.2%) of magnesium hydroxide is put into a reaction kettle, 200mL of deionized water is added, the temperature of water is raised to 85 ℃, the mixture is fully stirred, a metering pump is regulated at the moment, an ammonia bicarbonate solution with the concentration of 50g/L is dropwise added into the reaction kettle at the rate of 0.2L/h, the mixture is fully stirred and reacted, and the obtained suspension is subjected to suction filtration and washing. Drying at 100 ℃ to obtain the precursor. And (3) putting the obtained precursor into a muffle furnace, heating to 900 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h to obtain the high-purity light magnesium oxide with the purity of 99.8%. The apparent specific volume is 10ml/g.
Comparative example 2
15G (purity 99.2%) of magnesium hydroxide is put into a reaction kettle, 250mL of deionized water is added, the temperature of water is raised to 75 ℃, the mixture is fully stirred, at the moment, a metering pump is used for dripping 55g/L of ammonium bicarbonate solution into the reaction kettle at the rate of 0.25L/h, the mixture is fully stirred and reacted, and the obtained suspension is filtered and washed. Drying at 100 ℃ to obtain the precursor. And (3) putting the obtained precursor into a muffle furnace, setting the heating rate to be 7 ℃/min, heating to 950 ℃, and preserving heat for 1h to obtain the high-purity light magnesium oxide with the purity of 99.6%. The apparent specific volume is 9ml/g.
Comparative example 3
15G (purity 99.2%) of magnesium hydroxide is put into a reaction kettle, 300mL of deionized water is added, the temperature of water is raised to 80 ℃, the mixture is fully stirred, a metering pump is regulated at the moment, an ammonia bicarbonate solution with the concentration of 60g/L is dropwise added into the reaction kettle at the rate of 0.3L/h, the mixture is fully stirred and reacted, and the obtained suspension is subjected to suction filtration and washing. Drying at 100 ℃ to obtain the precursor. And (3) putting the obtained precursor into a muffle furnace, heating to 1100 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1h to obtain the high-purity light magnesium oxide with the purity of 99.7%. The apparent specific volume was 10.6g/ml. The SEM image is shown in fig. 7. The magnesium oxide is in a random loose sheet shape. Fig. 8 is a photograph of the calcined magnesia on the surface of silicon steel, more punctiform dew crystals exist, and the performance of the silicon steel sheet is affected.
The background section of the present invention may contain background information about the problems or environments of the present invention and is not necessarily descriptive of the prior art. Accordingly, inclusion in the background section is not an admission of prior art by the applicant.
The foregoing is a further detailed description of the invention in connection with specific embodiments, and it is not intended that the invention be limited to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention. In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Those skilled in the art may combine and combine the features of the different embodiments or examples described in this specification and of the different embodiments or examples without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the invention as defined by the appended claims.
Claims (3)
1. A preparation method of flaky porous silicon steel grade magnesium oxide is characterized by comprising the following steps: comprising the following steps:
(1) Taking magnesium hydroxide as a treatment object, and obtaining light-burned magnesium oxide by utilizing a wide temperature range-wide temperature difference strategy;
(2) Adding the high-temperature light-burned magnesia into the carbonized liquid for carbonization and aging, and filtering to obtain basic magnesium carbonate;
(3) Washing, drying and calcining basic magnesium carbonate to obtain flaky porous silicon steel grade magnesium oxide;
the wide temperature range is to enlarge the temperature range by utilizing liquid nitrogen, the magnesium hydroxide is placed in the liquid nitrogen, the temperature is reduced to-180 ℃ to-196 ℃, and the temperature is kept for 1-4 hours;
The wide temperature difference is a temperature rising process of quickly rising temperature to reach a wide temperature difference gradient, magnesium hydroxide is placed in a furnace, the temperature is raised to 610-800 ℃ at a temperature rising speed of 8-10 ℃/min, the stirring is uniform, the temperature is kept for 0.5-5h, and the temperature is lowered to 100-200 ℃; directly adding light burned magnesia with the temperature of 100-200 ℃ into the carbonized liquid;
The carbonization liquid is composed of one or more of sodium bicarbonate and potassium bicarbonate;
the carbonization time is 1-4 h, and the carbonization temperature is 70-100 ℃;
the adding rate of the carbonization liquid is 0.1-0.3L/h, wherein the solution concentration of the bicarbonate is 0.1-0.8 mol/L, and the adding amount of the bicarbonate is 0.1-0.9 times of the theoretical molar amount of carbonization reaction;
the purity of the obtained product is more than 99.5%; the apparent specific volume is 3.3-5.2 ml/g.
2. The method for preparing the flaky porous silicon steel grade magnesium oxide according to claim 1, which is characterized in that: the aging reaction time is 1-5h, and the stirring speed is 100-400r/min.
3. The method for preparing the flaky porous silicon steel grade magnesium oxide according to claim 1, which is characterized in that: the calcination process is as follows: placing the filter residue after washing and drying in a furnace, and heating to 850-1150 ℃ at a heating rate of 5-8 ℃/min for calcination.
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| CN202211384844.1A CN115676858B (en) | 2022-11-07 | 2022-11-07 | Preparation method of flaky porous silicon steel grade magnesium oxide |
| ZA2023/10229A ZA202310229B (en) | 2022-11-07 | 2023-11-02 | Preparation method for flake porous silicon steel grade magnesium oxide |
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| CN115676858A CN115676858A (en) | 2023-02-03 |
| CN115676858B true CN115676858B (en) | 2024-04-26 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495881A (en) * | 2014-12-19 | 2015-04-08 | 中南大学 | Process for preparing high-purity silicon steel magnesium oxide from magnesium hydroxide |
| CN207973685U (en) * | 2018-02-12 | 2018-10-16 | 沈阳鑫博工业技术股份有限公司 | A kind of device preparing silicon-steel grade magnesium oxide using dolomite |
| CN112850759A (en) * | 2021-02-26 | 2021-05-28 | 绵阳远达电子材料有限公司 | Production process of magnesium oxide |
| WO2022071797A1 (en) * | 2020-09-29 | 2022-04-07 | Technische Universiteit Eindhoven | Magnesia powder |
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- 2022-11-07 CN CN202211384844.1A patent/CN115676858B/en active Active
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495881A (en) * | 2014-12-19 | 2015-04-08 | 中南大学 | Process for preparing high-purity silicon steel magnesium oxide from magnesium hydroxide |
| CN207973685U (en) * | 2018-02-12 | 2018-10-16 | 沈阳鑫博工业技术股份有限公司 | A kind of device preparing silicon-steel grade magnesium oxide using dolomite |
| WO2022071797A1 (en) * | 2020-09-29 | 2022-04-07 | Technische Universiteit Eindhoven | Magnesia powder |
| CN112850759A (en) * | 2021-02-26 | 2021-05-28 | 绵阳远达电子材料有限公司 | Production process of magnesium oxide |
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| CN115676858A (en) | 2023-02-03 |
| ZA202310229B (en) | 2024-05-30 |
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