CN106222415A - A kind of carbothermic method produces magnesium metal reducing agent and preparation method thereof - Google Patents
A kind of carbothermic method produces magnesium metal reducing agent and preparation method thereof Download PDFInfo
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- CN106222415A CN106222415A CN201610833133.6A CN201610833133A CN106222415A CN 106222415 A CN106222415 A CN 106222415A CN 201610833133 A CN201610833133 A CN 201610833133A CN 106222415 A CN106222415 A CN 106222415A
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- reducing agent
- magnesium metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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Abstract
The invention discloses a kind of carbothermic method and produce magnesium metal reducing agent and preparation method thereof, be made up of waste and old cathode and carbon material according to mass ratio；Waste and old cathode: carbon material=1:0～9.Described preparation method includes: aluminum electrolysis waste cathode is crushed to below 3mm, according to quality than waste and old cathode: the ratio mix homogeneously of carbon material=1:0～9；Prepared mixture being entered ball mill dry grind, prepared granularity is the reducing agent powder of below 100 mesh.The present invention, with aluminum electrolysis waste cathode Substitute For Partial anthracite, coke or petroleum coke, decreases the consumption of these non-renewable resources, reduces reducing agent cost；Containing fluorides such as sodium fluoride, calcium fluoride and cryolites in reducing agent, when carrying out preparing metallic magnesium by carbothermic reduction as reducing agent, it is not necessary to additionally add catalyst, save cost；Containing a certain amount of metallic aluminium in reducing agent, it has stronger reducing activity, can reduce carbon thermal reduction temperature required.
Description
Technical field
The invention belongs to smelting field of nonferrous metal technical field, particularly relate to a kind of carbothermic method and produce magnesium metal use
Reducing agent and preparation method thereof.
Background technology
At present, China's magnesium metal yield has broken through 800,000 tons/year, and the demand of whole world magnesium metal is 600,000 tons/year,
Substantially drug on the market.Price competition fierce between colleague, makes many magnesium metal enterprises enter into the predicament of development, and realizes skill
Art is upgraded, and reducing production cost is the key making relevant enterprise extricate oneself from a plight.The production method of magnesium metal includes electrolysis and heat
Reducing process, wherein thermal reduction occupies critical role in China.Thermal reduction produce magnesium metal can reducing agent include three classes:
Metal (silicon, aluminum, calcium, manganese, lithium etc.), carbon and carbide.The most industrial mainly employing ferrosilicon is forged as reducing agent, reduction
Calcined dolomite produces magnesium metal, i.e. Pidgeon process.Producing one ton of magnesium metal with Pidgeon process, reducing agent ferrosilicon cost accounts for the ratio of totle drilling cost
Example is up to about 45%, and therefore, the reducing agent that a kind of reduction effect is good, with low cost is to reduce thermal reduction to produce magnesium metal one-tenth
This key.Carbon element class reducing agent is compared with ferrosilicon, with low cost, therefore, from last century so far, and the research of carbon thermal reduction refining magnesium
Never interrupt.Progress of research is, under vacuum condition, with CaF at present2、NaF、MgF2It is catalyst in fluoride, with carbon containing also
Former dose (such as anthracite, coke, petroleum coke etc.) reduction magnesium-containing oxide prepares magnesium metal.Relevant reducing agent has a problem in that: 1.
Anthracite, coke, petroleum coke etc. belong to non-renewable resources, and along with the increase of its consumption, the minimizing of reserves, price certainly will have
The trend gone up, and it is unfavorable for sustainable development；2. reduction process needs to add the CaF that price is higher2In fluoride as urging
Agent；3. reducing agent activity need to further enhance, thus reduces reduction temperature.For carbon elements such as coal, coke, petroleum cokes
The cheaper alternative of reducing agent, the most both at home and abroad also in technological gap.
In sum, it is big to there is Renewable resource consumption in existing carbon thermal reduction refining magnesium technology, relatively costly, reducing agent
The problem that activity is low.
Summary of the invention
It is an object of the invention to provide a kind of carbothermic method and produce magnesium metal reducing agent and preparation method thereof, it is intended to
Solve existing carbon thermal reduction refining magnesium technology and there is Renewable resource consumption greatly, relatively costly, the active low problem of reducing agent.
The present invention is achieved in that a kind of carbothermic method produces magnesium metal reducing agent, and described carbothermic method is raw
Produce magnesium metal reducing agent to be made up of waste and old cathode and carbon material according to mass ratio；Waste and old cathode: carbon material=1:0～9.
Another object of the present invention is to the preparation side providing a kind of described carbothermic method to produce magnesium metal reducing agent
Method, described carbothermic method produces the preparation method of magnesium metal reducing agent and comprises the following steps:
Step one, is crushed to below 3mm by aluminum electrolysis waste cathode, according to quality than waste and old cathode: carbon material=1:0
～the ratio mix homogeneously of 9；
Step 2, enters ball mill by prepared mixture and dry grinds, and prepared granularity is the reducing agent powder of below 100 mesh
End.
Further, described carbon material is the charcoals such as anthracite, coke, petroleum coke or aluminum electrolysis waste cathode flotation carbon powder
The mixture of one or more in cellulosic material.
Further, phosphorus content >=75wt% in mixture is made after mixing.
Another object of the present invention is to provide a kind of utilizes described carbothermic method to produce having of magnesium metal reducing agent
Non-ferrous metal smelting process.
Another object of the present invention is to provide a kind of gold utilizing described carbothermic method to produce magnesium metal reducing agent
Belong to Smelting magnesium method.
The carbothermic method that the present invention provides produces magnesium metal reducing agent and preparation method thereof, and aluminum electrolysis waste cathode is
A kind of solid waste that aluminium cell overhaul produces, because wherein the Water-soluble toxic such as soluble fluorine, cyanide material exceedes
The regulation of GB5085.3-2007, is defined as poisonous solid waste, and relevant enterprise have to carry out harmless treatment to it,
Its processing cost per ton is 120～160 dollars, brings white elephant to aluminium electrolysis enterprise.Containing a large amount of in waste and old cathode
Carbon, can be as the succedaneum of reducing agent, fluoride therein such as sodium fluoride, calcium fluoride and cryolite, can as carbon heat
The catalyst of magnesium metal is prepared in reduction, and metallic aluminium therein has higher reducing activity, contributes to the carrying out of reduction reaction, can
To reduce reduction temperature.Therefore, both can alleviate the burden of electrolytic aluminium factory with waste and old cathode Substitute For Partial reducing agent, can drop again
The cost of low preparing metallic magnesium by carbothermic reduction.The problem that the resources such as coal, coke and petroleum coke are day by day exhausted can be alleviated, solve
Carbothermic method needs additionally to add the fluoride problems as catalyst, and can reduce carbothermic method prepares metal simultaneously
The reaction temperature of magnesium.The preparation technology of reducing agent of the present invention is simple, with low cost, constant product quality, it is simple to promote.
The present invention, with aluminum electrolysis waste cathode Substitute For Partial anthracite, coke or petroleum coke, decreases these non-renewable
The consumption of resource 10%～100%, reduces reducing agent cost；Containing fluorine such as sodium fluoride, calcium fluoride and cryolites in reducing agent
Compound, when carrying out preparing metallic magnesium by carbothermic reduction as reducing agent, it is not necessary to additionally adds calcium fluoride, sodium fluoride, Afluon (Asta) etc.
Catalyst, saves carbon thermal reduction magnesium cost about 10%；Containing a certain amount of metallic aluminium in reducing agent, it has stronger going back
Former activity, can be reduced to 1200 DEG C and less by temperature required for carbon thermal reduction.
Accompanying drawing explanation
Fig. 1 is the preparation method flow chart that the carbothermic method that the embodiment of the present invention provides produces magnesium metal reducing agent.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Below in conjunction with the accompanying drawings the application principle of the present invention is explained in detail.
The carbothermic method that the embodiment of the present invention provides produce magnesium metal reducing agent according to mass ratio by waste and old cathode and
Carbon material forms；Waste and old cathode: carbon material=1:0～9.
As it is shown in figure 1, the carbothermic method that the embodiment of the present invention provides produces the preparation method bag of magnesium metal reducing agent
Include following steps:
S101: aluminum electrolysis waste cathode is crushed to below 3mm is cloudy with anthracite, coke, petroleum coke or aluminum electrolysis waste
One or more in the carbon materials such as pole flotation carbon powder, according to quality than waste and old cathode: the ratio of carbon material=1:0～9
Example mix homogeneously；
S102: prepared mixture is entered ball mill and dry grinds, prepared granularity is the reducing agent powder of below 100 mesh.
In described step S101 aluminum electrolysis waste cathode be mainly composed of carbon, sodium fluoride, cryolite, calcium fluoride, aluminium oxide,
Metallic aluminiums etc., additionally possibly together with a small amount of silicate, the compound of ferrum.Its phosphorus content is 35～75wt%, sodium fluoride, cryolite,
The fluoride total contents such as calcium fluoride 15～35wt%, alumina content 5～15wt%, metal aluminum content 2～10wt%, other become
Divide 3～5%.
Waste and old cathode and anthracite, coke, petroleum coke or aluminum electrolysis waste cathode flotation carbon powder in described step S101
After pressing certain mass ratio mixing Deng one or more in carbon material, make phosphorus content >=75wt% in mixture, so that it is guaranteed that
Reducing agent has good reproducibility.
It is 1. to make waste and old cathode composition mix with carbon material that described step S102 carries out the purpose of ball milling to mixed material
Uniformly；2. make reducing agent levigate to 100 mesh, grind the most slightly to be unfavorable for contacting of reducing agent and magnesium-containing ore, grind meticulous
Then waste the energy, the abrasion of aggravation ball mill.
Below in conjunction with specific embodiment, the application principle of the present invention is further described.
Embodiment 1:
(1) aluminum electrolysis waste cathode that phosphorus content is 60% is crushed to below 3mm, with waste and old the moon that phosphorus content is 90%
Pole flotation carbon powder according to quality than waste and old cathode: the mixing of the ratio of flotation carbon powder=1:2, obtain phosphorus content be 80% mixed
Close material；
(2) compound is entered ball mill, make the powder of-100 mesh, standby as reducing agent；
(3) magnesium oxide of MgO mass fraction >=95% is broken for 1-3mm, with above-mentioned reducing agent according to mol ratio C:MgO
=3:1 mixes, and is pressed into the pelletizing of diameter 10-30mm, enters vacuum drying oven, controls vacuum 5～10Pa, is warming up to 1100
DEG C, to react 30 minutes, condensation temperature is 650 DEG C, obtains reguline metal magnesium, and purity is 92%, and reduction degree reaches 85%.
Embodiment 2:
(1) aluminum electrolysis waste cathode that phosphorus content is 50% is crushed to below 3mm, with the coke that phosphorus content is 85% by
According to quality than waste and old cathode: the ratio mixing of coke=1:3, obtain the compound that phosphorus content is 76.3%；
(2) compound is entered ball mill, make the powder of-100 mesh, standby as reducing agent；
(3) the white and above-mentioned reducing agent of forging that MgO mass fraction is 38% is mixed according to mol ratio C:MgO=2.5:1
Close, be pressed into the pelletizing of diameter 10-30mm, enter vacuum drying oven, control vacuum 5～10Pa, be warming up to 1200 DEG C, react 50 points
Clock, condensation temperature is 650 DEG C, obtains reguline metal magnesium, and purity is 91%, and reduction degree reaches 83%.
Embodiment 3:
(1) aluminum electrolysis waste cathode that phosphorus content is 70% is crushed to below 3mm, is the anthracite of 80% with phosphorus content
According to quality than waste and old cathode: the ratio mixing of coke=1:1, obtain the compound that phosphorus content is 75%；
(2) compound is entered ball mill, make the powder of-100 mesh, standby as reducing agent；
(3) basic magnesium carbonate that MgO mass fraction is 41% is entered according to mol ratio C:MgO=3:1 with above-mentioned reducing agent
Row mixing, is pressed into the pelletizing of diameter 10-30mm, enters vacuum drying oven, controls vacuum 5～10Pa, decomposition, close-burning at 700 DEG C
30 minutes, being warming up to 1100 DEG C, react 50 minutes, condensation temperature is 650 DEG C, obtains reguline metal magnesium, and purity is 93%, reduction
Degree reaches 86%.
Embodiment 4:
(1) aluminum electrolysis waste cathode that phosphorus content is 75% is crushed to below 3mm；
(2) aluminum electrolysis waste cathode after crushing enters ball mill, makes the powder of-100 mesh, standby as reducing agent；
(3) the white and above-mentioned reducing agent of forging that MgO mass fraction is 39% is mixed according to mol ratio C:MgO=3:1,
It is pressed into the pelletizing of diameter 10-30mm, enters vacuum drying oven, control vacuum 5～10Pa, be warming up to 1200 DEG C, react 40 minutes, cold
Solidifying temperature is 650 DEG C, obtains reguline metal magnesium, and purity is 92%, and reduction degree reaches 85%.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (6)
1. a carbothermic method produces magnesium metal reducing agent, it is characterised in that described carbothermic method produces magnesium metal and uses
Reducing agent is made up of waste and old cathode and carbon material according to mass ratio；Waste and old cathode: carbon material=1:0～9.
2. the preparation method of a carbothermic method as claimed in claim 1 production magnesium metal reducing agent, it is characterised in that institute
The preparation method stating carbothermic method production magnesium metal reducing agent comprises the following steps:
Step one, is crushed to below 3mm by aluminum electrolysis waste cathode, according to quality than waste and old cathode: carbon material=1:0～9
Ratio mix homogeneously；
Step 2, enters ball mill by prepared mixture and dry grinds, and prepared granularity is the reducing agent powder of below 100 mesh.
3. carbothermic method as claimed in claim 2 produces the preparation method of magnesium metal reducing agent, it is characterised in that described
Carbon material is the one or several in the carbon materials such as anthracite, coke, petroleum coke or aluminum electrolysis waste cathode flotation carbon powder
The mixture planted.
4. carbothermic method as claimed in claim 3 produces the preparation method of magnesium metal reducing agent, it is characterised in that mixing
After make phosphorus content >=75wt% in mixture.
5. one kind utilizes carbothermic method described in claim 1 to produce the non-ferrous metal that magnesium metal reducing agent is smelted.
6. one kind utilizes carbothermic method described in claim 1 to produce the magnesium metal that magnesium metal reducing agent is smelted.
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| CN201610833133.6A CN106222415A (en) | 2016-09-20 | 2016-09-20 | A kind of carbothermic method produces magnesium metal reducing agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113277517A (en) * | 2021-05-24 | 2021-08-20 | 昆明理工大学 | Method for separating electrolyte in waste cathode carbon block of aluminum electrolysis and synchronously producing metal silicon |
| CN113880120A (en) * | 2021-11-22 | 2022-01-04 | 无锡市泽镁新材料科技有限公司 | Preparation method of silicon steel-grade magnesium oxide and silicon steel-grade magnesium oxide protective film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113277517A (en) * | 2021-05-24 | 2021-08-20 | 昆明理工大学 | Method for separating electrolyte in waste cathode carbon block of aluminum electrolysis and synchronously producing metal silicon |
| CN113880120A (en) * | 2021-11-22 | 2022-01-04 | 无锡市泽镁新材料科技有限公司 | Preparation method of silicon steel-grade magnesium oxide and silicon steel-grade magnesium oxide protective film |
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Application publication date: 20161214 |