CN101781707B - Method for preparing non-ferrous metal by thermal reduction of silicon-copper alloy - Google Patents
Method for preparing non-ferrous metal by thermal reduction of silicon-copper alloy Download PDFInfo
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- CN101781707B CN101781707B CN201010125151.1A CN201010125151A CN101781707B CN 101781707 B CN101781707 B CN 101781707B CN 201010125151 A CN201010125151 A CN 201010125151A CN 101781707 B CN101781707 B CN 101781707B
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- silicon
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Abstract
The invention discloses a method for preparing non-ferrous metal by the thermal reduction of silicon-copper alloy, belonging to the filed of metal smelting. The process comprises the following steps: preparing non-ferrous metallic oxide, reducing agent and adjuvant according to chemometry of reduction reaction, wherein the reducing agent is the alloy of silicon with copper, aluminum, manganese and the like; evenly mixing and placing the reactant into a vacuum reduction tank, carrying out vacuum thermal reduction under the conditions that the vacuum degree is 1-20Pa and the temperature is 1000-1250 DEG C; and collecting and condensing reduced metallic vapor to obtain condensed state metal. The method is used for preparing metal with high use ratios of resources and energy sources, and can be applied to the preparation of magnesium, calcium, strontium, lithium and other non-ferrous metal and alloy thereof.
Description
Technical field
The present invention relates to a kind of method that thermal reduction is prepared with non-ferrous metal magnesium or lithium, belong to Metal smelting field.
Background technology
Vacuum metallurgy technology is widely used in smelting field of nonferrous metal, and the thermal reduction that includes non-ferrous metal is extracted and separation, refining, enrichment etc.The non-ferrous metal relating to comprises magnesium, strontium, lithium, calcium etc.
The technique general process of existing vacuum-thermal reduction technology is: the ore of (1) calcining containing metal element, prepare metal oxide, (2) metal oxide is refined as to particle, (3) after being measured in proportion with reductive agent, auxiliary agent, metal oxide mixes and briquetting, (4) lumpy material is put into vacuum reducing tank and reacted, obtain metal vapors and be condensed into condensed state metal.
Mainly there are three problems in existing vacuum silicon reduction process for smelting magnesium, the one, reactant is the block that solid granulates forms, heat between particle and between block transmits, mass transport is not smooth, block central part is difficult to be heated, be difficult to participate in reaction, resource, the energy are difficult to obtain good utilization; The 2nd, in reaction process, the slag of reactant and generation remains static mutually, and the contact rate between reactant is low, even there will be the isolated reactant of slag, hinders the situation that reduction reaction is carried out, and reduction rate and reduction ratio are low; The 3rd, temperature of reaction is high, and long reaction time utilizes the temperature of ferrosilicon refining magnesium up to 1300 ℃, and for up to 8-10 hour, energy consumption is high and have a strong impact on work-ing life of reduction tank.
The invention provides reductive agent in a kind of reduction reaction process and be in a liquid state, the thermal reduction that reaction is carried out between " solid phase-liquid phase " is prepared with non-ferrous metal novel method.
Summary of the invention
The present invention is directed in existing thermal reduction and prepare in the method for metal, between granular reactant, can not fully contact, reaction is difficult for carrying out, reacts and be difficult for the problems such as thorough, and a kind of novel method that can significantly improve reduction rate and reduction ratio is provided.
In order to reach above object, technical scheme of the present invention is:
1) prepare thermal reduction raw material: raw material comprises the oxide compound, reductive agent copper-silicon alloy, auxiliary agent Calcium Fluoride (Fluorspan) of non-ferrous metal to be restored etc.Wherein: the oxide compound of non-ferrous metal to be restored is MgO or Li
2o; Reductive agent copper-silicon alloy consist of silicon 0.5-90%wt, copper 10-99.5%wt, and one or more in iron, aluminium, manganese, its solidus temperature is 500-1250 ℃; In raw material the volume of copper-silicon alloy be other component cumulative volumes 0.5-20 doubly; In copper-silicon alloy the amount of silicon be the theory calculated according to thermal reduction chemical equation need silicon amount 1-20 doubly; The consumption of Calcium Fluoride (Fluorspan) is the 0.5-5%wt of nonmetallic ingredient total amount in raw material.
2) reaction mass packs reduction tank after metering into, in vacuum tightness, is that 1-20Pa, temperature are at 1000-1250 ℃, to carry out thermal reduction, obtains metal vapors.
3) collect metal vapors condensation and obtain condensed state metal.
4), after having reacted, collect remaining metalliferous material in reduction tank and also again for thermal reduction, be prepared with non-ferrous metal flow process, or be separately used as him.
Meanwhile, in reduction reaction process, can be by measures such as stirring reaction material or rotation reduction tanks, forced disturbance reaction mass, promotes reaction to carry out.
Compared with prior art, method provided by the invention has realized reduction reaction transformation to " solid phase-liquid phase " by " solid phase-solid phase " reaction, and then significantly improve heat in reaction process and pass transmission, mass transport condition, improve the dynamic conditions of reduction reaction, realize the significantly lifting of reduction rate and reduction ratio, obtain utilization ratio and the complex art economic benefit of the good energy, resource.
Embodiment
Below in conjunction with embodiment, further illustrate the specific embodiment of the present invention.
Embodiment 1:
(1) ready reaction material, reaction mass is by MgO, copper-silicon alloy, CaO and CaF
2form, wherein in copper-silicon alloy, each constituent atoms ratio is: silicon: copper: iron: manganese=50: 45: 3: 2, the volume of copper-silicon alloy was MgO, CaO and CaF
220 times of volume sum, CaF
2consumption be the 0.5%wt of nonmetallic ingredient in reaction mass, by MgO, CaO and CaF
2grind into powder;
(2) by copper-silicon alloy, MgO, CaO and CaF
2put into vacuum reducing tank, be evacuated to 1Pa, be heated to 1100 ℃, by induction stirring stirring reaction material;
(3) carry out thermal reduction reaction 0.5 hour, obtain magnesium vapor condensation and obtain condensed state MAGNESIUM METAL;
(4) reclaim reaction rear remaining copper-silicon alloy recycle.
Embodiment 2:
(1) ready reaction material, reaction mass is by MgO, CaF
2, copper-silicon alloy forms, wherein in copper-silicon alloy, each constituent atoms ratio is: silicon: copper: iron: manganese=50: 45: 3: 2, the volume of copper-silicon alloy was 20 times of MgO volume, CaF
2consumption be the 0.5%wt of nonmetallic ingredient in reaction mass, MgO is ground into powder;
(2) by copper-silicon alloy, MgO, CaF
2put into vacuum reducing tank, be evacuated to 10Pa, be heated to 1200 ℃, by mechanical stirring reaction mass;
(3) carry out thermal reduction reaction 1 hour, obtain magnesium vapor condensation and obtain condensed state MAGNESIUM METAL;
(4) reclaim reaction rear remaining copper-silicon alloy recycle.
Embodiment 3:
(1) ready reaction material, reaction mass is comprised of MgO, copper-silicon alloy, and wherein in copper-silicon alloy, each constituent atoms ratio is: silicon: copper=50: 50, the volume of copper-silicon alloy is 0.5 times of MgO volume, and MgO is ground into powder;
(2) copper-silicon alloy, MgO are put into vacuum reducing tank, be evacuated to 20Pa, be heated to 1250 ℃, continue revolving reaction tank;
(3) carry out thermal reduction reaction 1 hour, obtain magnesium vapor condensation and obtain condensed state MAGNESIUM METAL;
(4) reclaim reaction rear remaining copper-silicon alloy recycle.
Embodiment 4:
(1) ready reaction material, reaction mass is by Li
2o, copper-silicon alloy form, and wherein in copper-silicon alloy, each constituent atoms ratio is: silicon: copper=0.5: 99.5, and wherein the volume of copper-silicon alloy is Li
220 times of O volume, by Li
2o grinds into powder, and various materials fully mix;
(2) by Li
2o, copper-silicon alloy are put into vacuum reducing tank, are evacuated to 1Pa, are heated to 1000 ℃;
(3) carry out thermal reduction reaction 3 hours, obtain lithium vapor condensation and obtain condensed state metallic lithium;
(4) reclaim reaction rear remaining copper-silicon alloy recycle.
Claims (5)
1. the method for a preparing non-ferrous metal by thermal reduction of silicon-copper alloy magnesium or lithium, raw material is comprised of nonferrous metal oxides, reductive agent and auxiliary agent, raw material is that 1-20Pa, temperature are to carry out thermal reduction in the reduction tank of 1000-1250 ℃ in vacuum tightness, the metal vapors condensation restoring obtains condensed state metal, it is characterized in that, consisting of of reductive agent copper-silicon alloy: silicon 0.5-90%wt, copper 10-99.5%wt, and one or more in iron, aluminium, manganese, its solidus temperature is 500-1250 ℃.
2. the method for a kind of preparing non-ferrous metal by thermal reduction of silicon-copper alloy magnesium according to claim 1 or lithium, it is characterized in that, in raw material the volume of copper-silicon alloy be other component cumulative volumes 0.5-20 doubly, in copper-silicon alloy the amount of silicon be the theory calculated according to thermal reduction chemical equation need silicon amount 1-20 doubly.
3. the method for a kind of preparing non-ferrous metal by thermal reduction of silicon-copper alloy magnesium according to claim 1 or lithium, is characterized in that, described nonferrous metal oxides is MgO or Li
2o.
4. the method for a kind of preparing non-ferrous metal by thermal reduction of silicon-copper alloy magnesium according to claim 1 or lithium, is characterized in that, in reduction reaction process, and the material in stirring reaction material or rotation reduction tank forced disturbance retort.
5. the method for a kind of preparing non-ferrous metal by thermal reduction of silicon-copper alloy magnesium according to claim 1 or lithium, is characterized in that, after having reacted, collects remaining metalliferous material in reduction tank and also again for thermal reduction, is prepared with non-ferrous metal flow process.
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CN101781707B true CN101781707B (en) | 2014-03-19 |
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CN1834270A (en) * | 2006-04-17 | 2006-09-20 | 重庆大学 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
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US4498927A (en) * | 1983-03-10 | 1985-02-12 | Aluminum Company Of America | Thermal reduction process for production of magnesium using aluminum skim as a reductant |
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