CN111850238B - Deoxidizer for smelting metal waste residues and preparation method thereof - Google Patents
Deoxidizer for smelting metal waste residues and preparation method thereof Download PDFInfo
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- CN111850238B CN111850238B CN202010716948.2A CN202010716948A CN111850238B CN 111850238 B CN111850238 B CN 111850238B CN 202010716948 A CN202010716948 A CN 202010716948A CN 111850238 B CN111850238 B CN 111850238B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/06—Deoxidising, e.g. killing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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Abstract
The invention discloses a deoxidizer for smelting metal waste residues, which is prepared from the following raw materials in parts by weight: 35-50 parts of expanded graphite powder, 20-30 parts of calcium carbonate, 20-30 parts of calcium oxide, 5-8 parts of passivated magnesium particles and 10-20 parts of pore-expanding agent, wherein the calcium oxide, the expanded graphite powder, the passivated magnesium particles, the pore-expanding agent and the calcium carbonate are sequentially added into a ball mill for ball milling, the rotating speed of the ball mill is controlled to be 800-minus 850r/min, the forward and reverse ball milling time is 1h, a mixture B is prepared, and then the mixture B is pressed to prepare a blank; the invention also discloses a preparation method of the deoxidizer for smelting the metal waste residue; the pore-expanding agent is added in the invention, so that the deoxidizer has a larger specific surface area and high porosity when in use, is beneficial to internal diffusion of gas, and can improve the utilization rate of internal components of the deoxidizer and improve the deoxidation effect.
Description
Technical Field
The invention belongs to the technical field of metal smelting, and particularly relates to a deoxidizer for smelting metal waste residues and a preparation method thereof.
Background
The non-metallic inclusions in the steel are mainly compounds formed by metal elements such as iron, manganese, chromium, aluminum, titanium and the like and oxygen, sulfur, nitrogen and the like. Wherein the oxide is mainly a deoxidation product, including a primary deoxidation product which cannot float upwards and a deoxidation product formed by a deoxidation reaction (secondary oxidation) in the molten steel solidification process; or due to slag, refractories, etc. mixed into the steel. The existence of the non-metallic inclusion destroys the continuity of a steel matrix, causes the nonuniformity of a steel structure, and has certain influence on various properties of the steel, such as the reduction of the strength, the toughness and the like of the steel. The non-metallic inclusions are mainly sulfides (MnS, FeS, etc.), oxides (FeO, MnO, CaO, Al2O3, etc.), silicates, nitrides (TiN, AlN), etc.
The Chinese patent CN101906509A discloses an Al-Ca-Fe deoxidizer for steel making, which is a spherical composition formed by combining powders such as metal aluminum powder, metal calcium powder, metal iron powder and the like, and the combined components, the shape and the size of the composition and the shape after balling ensure that the deoxidizer has the following characteristics: the metal aluminum powder, the metal calcium powder and the metal iron powder are pressed into balls, and the preparation method is simple and convenient; the finished product has high strength and can be directly fed into a high-level stock bin of a steel mill for use; the finished product has high specific gravity, strong reduction capability and strong molten steel deoxidation capability, and compared with similar deoxidizers, the total oxygen content of the molten steel is low; the deoxidation products are mutually accumulated and grow up, and the upward floating is fast; the inclusion content in the steel is reduced, and the inclusions can be denatured; the fluidity of the molten steel is good during casting.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a deoxidizer for smelting metal waste residues and a preparation method thereof.
The pore-expanding agent is added, when the deoxidizer is used, the deoxidizer has a large specific surface area and high porosity, internal diffusion of gas is facilitated, the utilization rate of internal components of the deoxidizer can be improved, and the deoxidation effect is improved.
The purpose of the invention can be realized by the following technical scheme:
a deoxidizer for smelting metal waste residues is prepared from the following raw materials in parts by weight: 35-50 parts of expanded graphite powder, 20-30 parts of calcium carbonate, 20-30 parts of calcium oxide, 5-8 parts of passivated magnesium particles, 10-20 parts of pore-expanding agent,
the deoxidizer for smelting the metal waste residue is prepared by the following method:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, a pore-expanding agent and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800-;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the temperature of the high-temperature furnace to rise to 350-550 ℃ at the speed of 5 ℃/min, and roasting at the temperature for 3-5h to prepare the deoxidizer for smelting the metal waste residue.
Further, the pore-expanding agent is one or two of polyethylene glycol and trimethylbenzene which are mixed according to any proportion.
Further, the expanded graphite powder is produced by the following method:
(1) adding graphite into a beaker, adding sodium nitrate and concentrated sulfuric acid with the mass fraction of 98%, stirring in an ice bath for 15min, adding potassium chlorate, continuing to stir for 30min, then heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, heating to 75 ℃, reacting for 30min, adding aqueous hydrogen peroxide with the mass fraction of 10%, and continuing to react for 10min to prepare a primarily treated graphite mixed solution A;
(2) adding ethylene oxide into the prepared graphite mixed solution A, heating to 30-35 ℃, carrying out ultrasonic treatment for 30min at the temperature, then cooling to-8 ℃, adding silicon tetrachloride, stirring at the rotating speed of 120-180r/min for 30-45min, adding triethylamine, heating to 45 ℃, stirring at the rotating speed of 200-240r/min for 10min, then continuously heating and refluxing for 5h, transferring to deionized water, filtering, washing, drying at 80 ℃ for 8-10h, grinding to obtain expanded graphite powder, and controlling the weight ratio of the graphite mixed solution A, the ethylene oxide, the silicon tetrachloride and the triethylamine to be 50: 5: 1: 2.
In the step (1), the graphite is subjected to primary treatment under the action of potassium chlorate, 10% hydrogen peroxide water solution and the like, and rich oxygen-containing functional groups are added on the surface of the treated graphite, so that agglomeration is not easy to occur; and (2) modifying graphite, namely mixing and stirring silicon tetrachloride and graphite at-8 ℃, modifying graphite oxide by using silicon tetrachloride, introducing silicon element into the graphite in the modification process, so that the graphite is easier to form a single-layer structure, forming wrinkles on the surface of the graphite, further increasing the specific surface area of the graphite, enabling the structure of the expanded graphite to be looser due to the wrinkles on the surface of the expanded graphite when the expanded graphite is gathered, forming large-aperture through holes, and further enhancing the adsorption performance of the expanded graphite through the large-aperture through holes.
Further, the weight ratio of the graphite, the sodium nitrate, the 98 percent concentrated sulfuric acid, the potassium chlorate and the aqueous hydrogen peroxide solution is controlled to be 2: 1: 10: 0.5-0.8: 2-3.
A preparation method of a deoxidizer for smelting metal waste residue comprises the following steps:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, a pore-expanding agent and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800-;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the temperature of the high-temperature furnace to rise to 350-550 ℃ at the speed of 5 ℃/min, and roasting at the temperature for 3-5h to prepare the deoxidizer for smelting the metal waste residue.
The invention has the beneficial effects that:
according to the deoxidizer for smelting the metal waste residue, the pore-expanding agent is added, when the deoxidizer is used, the deoxidizer has a large specific surface area and high porosity, internal diffusion of gas is facilitated, the utilization rate of internal components of the deoxidizer can be improved, and the deoxidizing effect is improved; and (2) modifying graphite, namely mixing and stirring silicon tetrachloride and graphite at-8 ℃, modifying graphite oxide by using silicon tetrachloride, introducing silicon element into the graphite in the modification process, so that the graphite is easier to form a single-layer structure, forming wrinkles on the surface of the graphite, further increasing the specific surface area of the graphite, enabling the structure of the expanded graphite to be looser due to the wrinkles on the surface of the expanded graphite when the expanded graphite is gathered, forming large-aperture through holes, further enhancing the adsorption performance of the expanded graphite through the large-aperture through holes, and further improving the gas removal effect of the deoxidizer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A deoxidizer for smelting metal waste residues is prepared from the following raw materials in parts by weight: 35 parts of expanded graphite powder, 20 parts of calcium carbonate, 20 parts of calcium oxide, 5 parts of passivated magnesium particles, 10 parts of polyethylene glycol,
the deoxidizer for smelting the metal waste residue is prepared by the following method:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, polyethylene glycol and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800r/min, and controlling the forward and reverse ball milling time to be 1h to prepare a mixture B, and then pressing the mixture B to prepare a blank;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the high-temperature furnace to heat up to 350 ℃ at the speed of 5 ℃/min, and roasting for 3h at the temperature to obtain the deoxidizer for smelting the metal waste residues.
The expanded graphite powder is prepared by the following method:
(1) adding graphite into a beaker, adding sodium nitrate and 98% concentrated sulfuric acid by mass, stirring in an ice bath for 15min, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, heating to 75 ℃, reacting for 30min, adding 10% aqueous hydrogen peroxide by mass, and continuously reacting for 10min to prepare a graphite mixed solution A after primary treatment, wherein the weight ratio of the graphite to the sodium nitrate to the 98% concentrated sulfuric acid to the potassium chlorate to the aqueous hydrogen peroxide is controlled to be 2: 1: 10: 0.5: 2;
(2) adding ethylene oxide into the prepared graphite mixed solution A, heating to 30 ℃, carrying out ultrasonic treatment for 30min at the temperature, then cooling to-8 ℃, adding silicon tetrachloride, stirring for 30min at the rotating speed of 120r/min, adding triethylamine, heating to 45 ℃, stirring for 10min at the rotating speed of 200r/min, then continuing heating and refluxing for 5h, transferring to deionized water, filtering, washing, drying for 8h at the temperature of 80 ℃, grinding to obtain expanded graphite powder, and controlling the weight ratio of the graphite mixed solution A, the ethylene oxide, the silicon tetrachloride and the triethylamine to be 50: 5: 1: 2.
Example 2
A deoxidizer for smelting metal waste residues is prepared from the following raw materials in parts by weight: 40 parts of expanded graphite powder, 22 parts of calcium carbonate, 22 parts of calcium oxide, 6 parts of passivated magnesium particles, 12 parts of polyethylene glycol,
the deoxidizer for smelting the metal waste residue is prepared by the following method:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, polyethylene glycol and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800r/min, and controlling the forward and reverse ball milling time to be 1h to prepare a mixture B, and then pressing the mixture B to prepare a blank;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the high-temperature furnace to heat up to 350 ℃ at the speed of 5 ℃/min, and roasting for 3h at the temperature to obtain the deoxidizer for smelting the metal waste residues.
The expanded graphite powder is prepared by the following method:
(1) adding graphite into a beaker, adding sodium nitrate and 98% concentrated sulfuric acid by mass, stirring in an ice bath for 15min, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, heating to 75 ℃, reacting for 30min, adding 10% aqueous hydrogen peroxide by mass, and continuously reacting for 10min to prepare a graphite mixed solution A after primary treatment, wherein the weight ratio of the graphite to the sodium nitrate to the 98% concentrated sulfuric acid to the potassium chlorate to the aqueous hydrogen peroxide is controlled to be 2: 1: 10: 0.5: 2;
(2) adding ethylene oxide into the prepared graphite mixed solution A, heating to 30 ℃, carrying out ultrasonic treatment for 30min at the temperature, then cooling to-8 ℃, adding silicon tetrachloride, stirring for 30min at the rotating speed of 120r/min, adding triethylamine, heating to 45 ℃, stirring for 10min at the rotating speed of 200r/min, then continuing heating and refluxing for 5h, transferring to deionized water, filtering, washing, drying for 8h at the temperature of 80 ℃, grinding to obtain expanded graphite powder, and controlling the weight ratio of the graphite mixed solution A, the ethylene oxide, the silicon tetrachloride and the triethylamine to be 50: 5: 1: 2.
Example 3
A deoxidizer for smelting metal waste residues is prepared from the following raw materials in parts by weight: 45 parts of expanded graphite powder, 28 parts of calcium carbonate, 28 parts of calcium oxide, 7 parts of passivated magnesium particles, 16 parts of polyethylene glycol,
the deoxidizer for smelting the metal waste residue is prepared by the following method:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, polyethylene glycol and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800r/min, and controlling the forward and reverse ball milling time to be 1h to prepare a mixture B, and then pressing the mixture B to prepare a blank;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the high-temperature furnace to heat up to 350 ℃ at the speed of 5 ℃/min, and roasting for 3h at the temperature to obtain the deoxidizer for smelting the metal waste residues.
The expanded graphite powder is prepared by the following method:
(1) adding graphite into a beaker, adding sodium nitrate and 98% concentrated sulfuric acid by mass, stirring in an ice bath for 15min, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, heating to 75 ℃, reacting for 30min, adding 10% aqueous hydrogen peroxide by mass, and continuously reacting for 10min to prepare a graphite mixed solution A after primary treatment, wherein the weight ratio of the graphite to the sodium nitrate to the 98% concentrated sulfuric acid to the potassium chlorate to the aqueous hydrogen peroxide is controlled to be 2: 1: 10: 0.5: 2;
(2) adding ethylene oxide into the prepared graphite mixed solution A, heating to 30 ℃, carrying out ultrasonic treatment for 30min at the temperature, then cooling to-8 ℃, adding silicon tetrachloride, stirring for 30min at the rotating speed of 120r/min, adding triethylamine, heating to 45 ℃, stirring for 10min at the rotating speed of 200r/min, then continuing heating and refluxing for 5h, transferring to deionized water, filtering, washing, drying for 8h at the temperature of 80 ℃, grinding to obtain expanded graphite powder, and controlling the weight ratio of the graphite mixed solution A, the ethylene oxide, the silicon tetrachloride and the triethylamine to be 50: 5: 1: 2.
Example 4
A deoxidizer for smelting metal waste residues is prepared from the following raw materials in parts by weight: 50 parts of expanded graphite powder, 30 parts of calcium carbonate, 30 parts of calcium oxide, 8 parts of passivated magnesium particles, 20 parts of polyethylene glycol,
the deoxidizer for smelting the metal waste residue is prepared by the following method:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, polyethylene glycol and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800r/min, and controlling the forward and reverse ball milling time to be 1h to prepare a mixture B, and then pressing the mixture B to prepare a blank;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the high-temperature furnace to heat up to 350 ℃ at the speed of 5 ℃/min, and roasting for 3h at the temperature to obtain the deoxidizer for smelting the metal waste residues.
The expanded graphite powder is prepared by the following method:
(1) adding graphite into a beaker, adding sodium nitrate and 98% concentrated sulfuric acid by mass, stirring in an ice bath for 15min, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, heating to 75 ℃, reacting for 30min, adding 10% aqueous hydrogen peroxide by mass, and continuously reacting for 10min to prepare a graphite mixed solution A after primary treatment, wherein the weight ratio of the graphite to the sodium nitrate to the 98% concentrated sulfuric acid to the potassium chlorate to the aqueous hydrogen peroxide is controlled to be 2: 1: 10: 0.5: 2;
(2) adding ethylene oxide into the prepared graphite mixed solution A, heating to 30 ℃, carrying out ultrasonic treatment for 30min at the temperature, then cooling to-8 ℃, adding silicon tetrachloride, stirring for 30min at the rotating speed of 120r/min, adding triethylamine, heating to 45 ℃, stirring for 10min at the rotating speed of 200r/min, then continuing heating and refluxing for 5h, transferring to deionized water, filtering, washing, drying for 8h at the temperature of 80 ℃, grinding to obtain expanded graphite powder, and controlling the weight ratio of the graphite mixed solution A, the ethylene oxide, the silicon tetrachloride and the triethylamine to be 50: 5: 1: 2.
Comparative example 1
Compared with example 1, the preparation method of the comparative example is as follows:
step S1, sequentially adding calcium oxide, graphite powder, passivated magnesium particles, polyethylene glycol and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800r/min, and controlling the forward and reverse ball milling time to be 1h to prepare a mixture B, and then pressing the mixture B to prepare a blank;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the high-temperature furnace to heat up to 350 ℃ at the speed of 5 ℃/min, and roasting for 3h at the temperature to obtain the deoxidizer for smelting the metal waste residues.
Comparative example 2
The comparative example is a deoxidizer for smelting in the market.
As can be seen from the above table, the deoxidation capacities of examples 1 to 4 were 25.2 to 26.3mL/g, the deoxidation depths were 0.08 to 0.09ppm, the deoxidation capacities of comparative examples 1 to 2 were 18.6 to 20.8mL/g, and the deoxidation depths were 0.035 to 0.040 ppm; therefore, the deoxidizer has larger specific surface area and high porosity, is beneficial to the internal diffusion of gas, and can improve the utilization rate of internal components of the deoxidizer and improve the deoxidation effect.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean 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 invention. In this specification, the schematic representations of the terms used above do not necessarily refer 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.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (2)
1. The deoxidizer for smelting the metal waste residue is characterized by being prepared from the following raw materials in parts by weight: 35-50 parts of expanded graphite powder, 20-30 parts of calcium carbonate, 20-30 parts of calcium oxide, 5-8 parts of passivated magnesium particles and 10-20 parts of pore-expanding agent;
the deoxidizer for smelting the metal waste residue is prepared by the following method:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, a pore-expanding agent and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800-;
step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the temperature of the high-temperature furnace to rise to 350-550 ℃ at the speed of 5 ℃/min, and roasting for 3-5h at the temperature to prepare the deoxidizer for smelting the metal waste residue;
the expanded graphite powder is prepared by the following method:
(1) adding graphite into a beaker, adding sodium nitrate and 98 mass percent concentrated sulfuric acid, stirring in an ice bath for 15min, adding potassium chlorate, continuing to stir for 30min, then heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, heating to 75 ℃, reacting for 30min, adding 10 mass percent aqueous hydrogen peroxide, continuing to react for 10min to prepare a graphite mixed solution A after primary treatment, and controlling the weight ratio of the graphite to the sodium nitrate to the 98 mass percent concentrated sulfuric acid to the potassium chlorate to the aqueous hydrogen peroxide to be 2: 1: 10: 0.5-0.8: 2-3;
(2) adding ethylene oxide into the prepared graphite mixed solution A, heating to 30-35 ℃, carrying out ultrasonic treatment for 30min at the temperature, then cooling to-8 ℃, adding silicon tetrachloride, stirring at the rotating speed of 120-180r/min for 30-45min, adding triethylamine, heating to 45 ℃, stirring at the rotating speed of 200-240r/min for 10min, then continuously heating and refluxing for 5h, transferring to deionized water, filtering, washing, drying at 80 ℃ for 8-10h, grinding to obtain expanded graphite powder, and controlling the weight ratio of the graphite mixed solution A, the ethylene oxide, the silicon tetrachloride and the triethylamine to be 50: 5: 1: 2;
the pore-expanding agent is one or two of polyethylene glycol and trimethylbenzene which are mixed according to any proportion.
2. The method for preparing the deoxidizer for smelting the metal waste residue, which is disclosed by claim 1, is characterized by comprising the following steps of:
step S1, sequentially adding calcium oxide, expanded graphite powder, passivated magnesium particles, a pore-expanding agent and calcium carbonate into a ball mill for ball milling, controlling the rotating speed of the ball mill to be 800-;
and step S2, transferring the prepared blank into a high-temperature furnace for calcination, controlling the temperature of the high-temperature furnace to rise to 350-550 ℃ at the speed of 5 ℃/min, and roasting at the temperature for 3-5h to prepare the deoxidizer for smelting the metal waste residue.
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Denomination of invention: Deoxidizer for smelting metal waste slag and its preparation method Effective date of registration: 20221021 Granted publication date: 20211102 Pledgee: Wuhu Wanyi District sub branch of China Postal Savings Bank Co.,Ltd. Pledgor: Wuhu County Tianhai Refractory Furnace Charge Co.,Ltd. Registration number: Y2022980019196 |