CN110055409A - A kind of Smelting magnesium technique of exhaust gas waste residue recoverable - Google Patents

A kind of Smelting magnesium technique of exhaust gas waste residue recoverable Download PDF

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Publication number
CN110055409A
CN110055409A CN201910354623.1A CN201910354623A CN110055409A CN 110055409 A CN110055409 A CN 110055409A CN 201910354623 A CN201910354623 A CN 201910354623A CN 110055409 A CN110055409 A CN 110055409A
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exhaust gas
magnesium
waste residue
gas waste
solid state
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张超
付瑾
楚化强
顾明言
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Anhui University of Technology AHUT
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Anhui University of Technology AHUT
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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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/16—Sintering; Agglomerating
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • 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
    • 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
    • C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a kind of Smelting magnesium techniques of exhaust gas waste residue recoverable, belong to magnesium metal smelting technical field.Process flow of the invention are as follows: Step 1: dolomite, magnesite and reducing agent aluminium powder are carried out ingredient according to mass ratio；Step 2: by being calcined after the mixed powder pressed pellet of configuration, the high temperature CO released2Room temperature is down to after the combustion air of delivery heat exchanger preheating reduction furnace；Step 3: also being originated in magnesium reaction in reductive jar, high temperature magnesium vapor and solid state reduction slag are generated；Sodium aluminate solution is generated Step 4: solid state reduction slag is reacted with sodium carbonate liquor, by room temperature CO in step 22It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain sodium carbonate liquor and be re-used in this step.The present invention is by high temperature CO2It is used for the processing of reducing slag after the heat recovery that gas contains, by extracting reducing agent in reducing slag for being recycled, can reduce a ton magnesium coal consumption, reduce the discharge of greenhouse gases and solid state reduction slag, increase economic efficiency.

Description

A kind of Smelting magnesium technique of exhaust gas waste residue recoverable
Technical field
The invention belongs to magnesium metal smelting technical fields, more specifically to a kind of exhaust gas waste residue recoverable Smelting magnesium technique.
Background technique
The former magnesium that Pidgeon process produces in traditional method for smelting magnesium by hot technique accounts for 95% or more total output, is most popular gold Belong to Smelting magnesium technique, it is to produce metal magnesium vapor with reduction by ferrosilicon dolime under high temperature high vacuum condition.However, this Kind of technique there are energy consumptions it is high, greenhouse gases and solid state reduction slag discharge amount are big the problems such as, therefore, it is necessary to traditional smelting silicothermic process Magnesium technology carries out Improvement.Aluminothermic process, as reducing agent, can be such that reduction temperature drops using low-melting aluminium powder substitution ferrosilicon It is low, shorten reduction cycle, but aluminothermic process is the improvement to magnesium process is also originated in, and a large amount of high temperature COs2Gas is forged in dolomite What the burning stage generated, so the problem of discharging a large amount of high temperature greenhouse gases is not resolved, and aluminothermic process is to forging white go back The problem of solid state reduction slag generated when former is difficult to recycling and reusing, discharges a large amount of reducing slags also still remains.
It is difficult to the deficiency recycled for the exhaust gas waste residue generated during carbothermy refining magnesium, has phase in the prior art Technical solution is closed to disclose, such as number of patent application: 2013101627580, the applying date: on May 6th, 2013, invention and created name are as follows: A kind of method that carbon thermal reduction magnesium mine prepares magnesium metal, this application discloses the carbon thermal reduction magnesium mine technique for preparing magnesium metal Process includes: to crush and be uniformly mixed after first measuring magnesium ore, simple substance carbon, carbon containing alloy, auxiliary agent by a certain percentage, is packed into It is thermally decomposed under conditions of 100~101325Pa of vacuum degree, 800~1250 DEG C of temperature in reactor tank；Later vacuum degree 1~ 20Pa, it is heat-treated under conditions of 1000~1250 DEG C of temperature, collects the magnesium vapor of generation and be condensed into the metal of condensed state Magnesium, this method process flow is short, high production efficiency.The metalliferous material collected in reactor tank in this application is re-used for heat-treating The process or otherwise utilized for preparing magnesium metal, reacts CO, CO of generation2It decomposes and heat-treats for magnesium mine and thermal energy is provided, but should Only to CO in application case2Heat difference physically is utilized, not to greenhouse gases CO2It further recycles, energy Source utilization rate remains to be further improved.
For another example number of patent application: 2017103208768, the applying date: on May 9th, 2017, invention and created name are as follows: a kind of Carbothermy produces the technique of magnesium metal and calcium carbide, the preparation step of the program simultaneously are as follows: step 1, according to mass ratio of each component handle Magnesia, calcium oxide, carbonaceous reducing agent, fluorite catalyst carry out ingredient；Configuration material is placed in band by step 2 after mixing Sieve ball mill is ground and is sieved, and the material of different fineness is obtained；Step 3 is uniformly mixed material after screening, is then fed into High pressure para-roller ball pressing machine suppresses balling-up, and dries；Step 4 is placed in pelletizing in vacuum reactor, takes out to vacuum reactor true Sky, certain pressure and at a temperature of produce metal magnesium vapor and calcium carbide calcium carbide.The program can using magnesia and calcium oxide To produce magnesium and calcium carbide simultaneously, the energy is saved, environmental pollution is reduced, has improved raw material availability, but whether need It prepares calcium carbide while preparing magnesium also to need depending on the condition of production, use of the program in enterprise produces still is limited.
Summary of the invention
1. technical problems to be solved by the inivention
It is an object of the invention to overcome the exhaust gas waste residue generated during existing carbothermy refining magnesium to be difficult to recycle Deficiency, provides a kind of Smelting magnesium technique of exhaust gas waste residue recoverable, and this method is by high temperature CO2The heat that gas contains returns It is used for the processing of reducing slag after receipts, by extracting reducing agent in reducing slag for being recycled, can reduce a ton magnesium coal consumption, largely reduce The discharge of greenhouse gases and solid state reduction slag, increases economic efficiency.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention are as follows:
A kind of Smelting magnesium technique of exhaust gas waste residue recoverable of the invention, comprising the following steps:
Step 1: carrying out ingredient according to mass ratio of each component: 60~70 parts of dolomites and 18~25 parts of magnesite composition 8~15 parts of mixed powder, reducing agent aluminium powder, gross mass number are 100 parts；
Step 2: then the qualified mixed powder of dolomite and magnesite and aluminium powder pressed pellet after mixing are sent Enter in reductive jar and calcines, the high temperature CO released2Delivery heat exchanger preheating reduction furnace help hot-air after be down to room temperature；
Step 3: reductive jar is evacuated to absolute pressure lower than 100Pa, it is anti-that adjustment reduction furnace temperature is also originated in magnesium It answers, generates high temperature magnesium vapor and solid state reduction slag；
Sodium aluminate solution is generated Step 4: the solid state reduction slag in step 3 is reacted with sodium carbonate liquor, and by step Two obtained room temperature CO2It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain aluminium hydroxide and sodium carbonate liquor, sodium carbonate liquor It is re-used in this step.
As further improvement of the present invention, calcined aluminium hydroxide obtained in step 4 to obtain aluminium oxide, The metallic aluminium that electrolysis of aluminum oxide obtains is used to prepare the reducing agent aluminium powder in step 1.
As further improvement of the present invention, qualification mixed powder described in step 2 is by dolomite and magnesite Mixed powder is ground and is sieved in band sieve ball mill, and the material that granularity is 100~200 mesh is obtained.
As further improvement of the present invention, the granule size of reducing agent aluminium powder described in step 1 is greater than 150 mesh.
As further improvement of the present invention, reduction furnace temperature is risen to 1100~1200 DEG C in step 3 and is restored It produces magnesium and reacts 30~360min.
As further improvement of the present invention, temperature when pelletizing is calcined in reductive jar in step 2 is 900~ 1000 DEG C, pressure is negative pressure or micro-positive pressure.
As further improvement of the present invention, by dolomite, magnesite qualification mixed powder and aluminium powder in step 2 It is squeezed into pelletizing with ball press after mixing, qualified pelletizing equivalent diameter is no more than 50mm.
As further improvement of the present invention, the sodium carbonate liquor that is reacted in step 4 with solid state reduction slag by the external world into Row supplement.
As further improvement of the present invention, the sodium carbonate liquor concentration that reacts in step 4 with solid state reduction slag For 100~130g/L, solution temperature is 80~95 DEG C.
As further improvement of the present invention, the temperature that aluminium hydroxide obtained in step 4 is calcined is 1000 ~1200 DEG C, calcination time is 120~360min.
3. beneficial effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result:
(1) the Smelting magnesium technique of a kind of exhaust gas waste residue recoverable of the invention, dolomite and magnesite calcining generate High temperature CO2Heat obtains room temperature CO after cooling for the combustion air in preheating reduction furnace after gas delivery heat exchanger2 For the processing of reducing slag, not only reduces a ton magnesium energy consumption and also reduce greenhouse gas emission.
(2) the Smelting magnesium technique of a kind of exhaust gas waste residue recoverable of the invention, CO2It is raw with the Leach reaction of reducing slag At sodium carbonate liquor, it is circularly used for processing solid state reduction slag, the recycling of sodium carbonate liquor is realized, effectively reduces Production cost and the discharge for substantially reducing greenhouse gases and solid-state waste residue.
(3) the Smelting magnesium technique of a kind of exhaust gas waste residue recoverable of the invention, CO2It is raw with the Leach reaction of reducing slag It is calcined to obtain aluminium oxide again at aluminum hydroxide precipitation, after being separated by filtration it, the metallic aluminium that electrolysis of aluminum oxide obtains is available In preparing reducing agent aluminium powder, the recycling of reducing agent is realized.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this A little attached drawings obtain other relevant attached drawings.
Fig. 1 is a kind of process flow chart of the Smelting magnesium technique of exhaust gas waste residue recoverable of the present invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is A part of the embodiment of the present invention, instead of all the embodiments.Therefore, below to the embodiment of the present invention provided in the accompanying drawings Detailed description be not intended to limit the range of claimed invention, but be merely representative of selected embodiment of the invention. Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts all Other embodiments shall fall within the protection scope of the present invention.
To further appreciate that the contents of the present invention, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
In conjunction with Fig. 1, a kind of Smelting magnesium technique of exhaust gas waste residue recoverable of the present embodiment, comprising the following steps:
Step 1: ingredient is carried out according to mass ratio of each component, wherein 60 parts of dolomites and 25 parts of magnesite are uniformly mixed Mixed powder is obtained, then weighs that the reducing agent aluminium powder that 15 parts of granule sizes are 160 mesh, purity is 99% is spare, three kinds of materials Gross mass number is 100 parts；
Step 2: the qualified mixed powder of dolomite and magnesite and 15 parts of aluminium powders are squeezed with ball press after mixing At pelletizing, qualified pelletizing equivalent diameter is 40mm, and then pelletizing is sent into reductive jar and is calcined, when pelletizing is calcined in reductive jar Temperature be 900 DEG C, pressure is negative pressure, the high temperature CO released in calcination process2Reduction furnace is passed through after delivery heat exchanger, heat Amount is for the combustion air in preheating reduction furnace；Qualified mixed powder is by 60 parts of dolomite and 25 parts of water chestnut in the present embodiment Magnesium mine is ground and is sieved in band sieve ball mill, and the material that granularity is 100~200 mesh is obtained；
Step 3: after dolomite in pelletizing and magnesite decompose completely, reductive jar is taken out into sealing and vacuum is to absolute pressure It is lower than 100Pa by force, adjustment reduction furnace temperature rises to 1100 DEG C and also originated in magnesium reaction, and reaction time 50min, reaction generates high Warm magnesium vapor and solid state reduction slag, magnesium vapor are collected to obtain solid metallic magnesium by condensation-crystallization；
Sodium aluminate solution is generated Step 4: the solid state reduction slag in step 3 is reacted with sodium carbonate liquor, and by step Room temperature CO after cooling in two2It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain aluminum hydroxide precipitation and sodium carbonate liquor, carbon The Leach reaction of the reusable reducing slag in this step of acid sodium solution, the sodium carbonate liquor reacted with solid state reduction slag can also Reasonable supplement is carried out by the external world according to actual use situation.
Ore raw materials is dolomite and magnesite in the present embodiment, and chemical molecular formula is respectively dolomite CaCO3· MgCO3, magnesite MgCO3, dolomite and magnesite are weighed first in step 2 by weight ratio and mix and smash and grind into The powdery of 100~200 mesh, it is agglomerating with press machine extruding after then being mixed in proportion with aluminium powder, the pelletizing being pressed into is put into also In former tank, first reductive jar is carried out to be heated to 900 DEG C of calcining 180min.By the conjunction of dolomite, magnesite in the present embodiment Lattice mixed powder and aluminium powder are squeezed into pelletizing after mixing, and qualified pelletizing equivalent diameter is 40mm, and specifically, qualified pelletizing can Think the sphere structure of regular shape, or the bulk of the non-regular shapes such as walnut shape, pincushion, elliposoidal or cylinder is solid Body, equivalent diameter refer to that the diameter of the volume same sphere of blocks of solid is 40mm.
Specifically, the chemical reaction that pelletizing occurs in reductive jar in step 2 in the present embodiment is as follows:
CaCO3·MgCO3→2CO2↑+CaO·MgO
MgCO3→CO2↑+MgO；
The high temperature CO that the process is generated after the reaction was completed2Reduction furnace is passed through after gas delivery heat exchanger, heat is used for Combustion air in preheating reduction furnace obtains room temperature CO after cooling2；
Leach reaction generation sodium aluminate solution occurs for solid state reduction slag and sodium carbonate liquor in step 4, and the chemistry of generation is anti- It should be as follows:
12CaO·7Al2O3+12Na2CO3+33H2O→14NaAl(OH)4+10NaOH+12CaCO3↓；
The sodium carbonate liquor concentration to react in step 4 with solid state reduction slag is 110g/L, and solution temperature is 80 DEG C.
The CaCO generated in the present embodiment3Precipitating and NaAl (OH)4Solution obtains pure sodium aluminate solution by solid-liquor separation Liquid.Step 2 calcination stage is generated at this time and is cooled to the CO of room temperature2Gas, which is passed through in sodium aluminate solution, carries out carbon point point Solution reaction, generates aluminum hydroxide precipitation and sodium carbonate liquor, can obtain solid-state Al (OH) after filtering3And sodium carbonate liquor, carbonic acid The Leach reaction for continuing on for solid state reduction slag can be recycled in sodium solution.The chemical reaction that the process occurs is as follows:
2NaAl(OH)4+CO2→Na2CO3+2Al(OH)3↓+H2O；
The Smelting magnesium technique of a kind of exhaust gas waste residue recoverable of the present embodiment, by aluminium hydroxide obtained in step 4 Precipitating is calcined to obtain aluminium oxide again after being separated by filtration, and the metallic aluminium that electrolysis of aluminum oxide obtains is used to prepare in step 1 Reducing agent aluminium powder realizes the recycling of reducing agent.Specifically, solid-state Al (OH)3150min, Al are calcined at 1000 DEG C (OH)3Al is obtained after calcined dehydration2O3, the chemical reaction of generation is as follows:
2Al(OH)3→Al2O3+3H2O。
Dolomite is calcined with magnesite and also originated in the present embodiment and is completed in magnesium process conformity a to reactor, is mentioned The high utilization rate of equipment；The high temperature CO of generation2It is used for the processing of reducing slag after the heat recovery that gas contains, not only reduces Ton magnesium energy consumption also reduces greenhouse gas emission, realizes the resource utilization of exhaust gas waste residue；Reducing slag and sodium carbonate liquor leach CO after cooling is passed through after reaction2Gas obtains aluminium hydroxide, and aluminium hydroxide calcined dehydration obtains aluminium oxide, then to aluminium oxide Electrolysis obtains metallic aluminium, and metallic aluminium realizes the recycling of reducing agent as the raw material for preparing reducing agent aluminium powder, effective to drop Low production cost, increases economic efficiency.
Embodiment 2
A kind of Smelting magnesium technique of exhaust gas waste residue recoverable of the present embodiment, step is substantially the same manner as Example 1, The difference is that:
Step 1: ingredient is carried out according to mass ratio of each component, wherein 65 parts of dolomites and 20 parts of magnesite are uniformly mixed Mixed powder is obtained, then weighs that the reducing agent aluminium powder that 15 parts of granule sizes are 170 mesh, purity is 99% is spare, three kinds of materials Gross mass number is 100 parts；
Step 2: the qualified mixed powder of dolomite and magnesite and 15 parts of aluminium powders are squeezed with ball press after mixing At pelletizing, qualified pelletizing equivalent diameter is 30mm, and then pelletizing is sent into reductive jar and is calcined, when pelletizing is calcined in reductive jar Temperature be 950 DEG C, pressure is negative pressure, the high temperature CO released in calcination process2Reduction furnace is passed through after delivery heat exchanger, heat Amount is for the combustion air in preheating reduction furnace；Qualified mixed powder is by 65 parts of dolomite and 20 parts of water chestnut in the present embodiment Magnesium mine is ground and is sieved in band sieve ball mill, and the granule size of acquisition is the material of 100~200 mesh；
Step 3: after dolomite in pelletizing and magnesite decompose completely, reductive jar is taken out into sealing and vacuum is to absolute pressure It is lower than 100Pa by force, adjustment reduction furnace temperature rises to 1150 DEG C and also originated in magnesium reaction, reaction time 100min, and reaction generates High temperature magnesium vapor and solid state reduction slag, magnesium vapor are collected to obtain solid metallic magnesium by condensation-crystallization；
Sodium aluminate solution is generated Step 4: the solid state reduction slag in step 3 is reacted with sodium carbonate liquor, and by step Room temperature CO after cooling in two2It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain aluminum hydroxide precipitation and sodium carbonate liquor, carbon The Leach reaction of the reusable reducing slag in this step of acid sodium solution, the sodium carbonate liquor reacted with solid state reduction slag can also Reasonable supplement is carried out by the external world according to actual use situation.
Ore raw materials is dolomite and magnesite in the present embodiment, and chemical molecular formula is respectively dolomite CaCO3· MgCO3, magnesite MgCO3, dolomite and magnesite are weighed first in step 2 by weight ratio and mix and smash and grind into The powdery of 100~200 mesh, it is agglomerating with press machine extruding after then being mixed in proportion with aluminium powder, the pelletizing being pressed into is put into also In former tank, first reductive jar is carried out to be heated to 950 DEG C of calcining 150min.By the conjunction of dolomite, magnesite in the present embodiment Lattice mixed powder and aluminium powder are squeezed into pelletizing after mixing, and qualified pelletizing equivalent diameter is 30mm.Specifically, in the present embodiment The chemical reaction that pelletizing occurs in reductive jar in step 2 is as follows:
CaCO3·MgCO3→2CO2↑+CaO·MgO
MgCO3→CO2↑+MgO；
Leach reaction generation sodium aluminate solution occurs for solid state reduction slag and sodium carbonate liquor in step 4, and the chemistry of generation is anti- It should be as follows:
12CaO·7Al2O3+12Na2CO3+33H2O→14NaAl(OH)4+10NaOH+12CaCO3↓；
The sodium carbonate liquor concentration to react in step 4 with solid state reduction slag is 100g/L, and solution temperature is 90 DEG C.
By the CO after cooling in step 22It is passed through sodium aluminate solution, the chemical reaction which occurs is as follows:
2NaAl(OH)4+CO2→Na2CO3+2Al(OH)3↓+H2O；
Again by solid-state Al (OH)3360min, Al (OH) are calcined at 1150 DEG C3Al is obtained after calcined dehydration2O3, generation It chemically reacts as follows:
2Al(OH)3→Al2O3+3H2O。
Obtained aluminium oxide is further electrolysed in the present embodiment and obtains metallic aluminium, as the original for preparing reducing agent aluminium powder Material.
A kind of Smelting magnesium technique of exhaust gas waste residue recoverable of the present embodiment, substantially reduces greenhouse gases and solid-state The discharge of waste residue efficiently uses the exhaust gas waste residue generated in process of producing product, simplifies entire process route, realizes process product And energy recycles.
Embodiment 3
A kind of Smelting magnesium technique of exhaust gas waste residue recoverable of the present embodiment, step is substantially the same manner as Example 1, The difference is that:
Step 1: ingredient is carried out according to mass ratio of each component, wherein 70 parts of dolomites and 18 parts of magnesite are uniformly mixed Mixed powder is obtained, then weighs that the reducing agent aluminium powder that 12 parts of granule sizes are 170 mesh, purity is 99% is spare, three kinds of materials Gross mass number is 100 parts；
Step 2: the qualified mixed powder of dolomite and magnesite and 12 parts of aluminium powders are squeezed with ball press after mixing At pelletizing, qualified pelletizing equivalent diameter is 50mm, and then pelletizing is sent into reductive jar and is calcined, when pelletizing is calcined in reductive jar Temperature be 1000 DEG C, pressure is micro-positive pressure, calcination time 200min, the high temperature CO released in calcination process2Import heat Heat is for the combustion air in preheating reduction furnace after exchanger；Qualified mixed powder is by 70 parts of dolomite in the present embodiment Magnesite with 18 parts is ground and is sieved in band sieve ball mill, and the granule size of acquisition is the material of 100~200 mesh；
Step 3: after dolomite in pelletizing and magnesite decompose completely, reductive jar is taken out into sealing and vacuum is to absolute pressure It is lower than 100Pa by force, adjustment reduction furnace temperature rises to 1200 DEG C and also originated in magnesium reaction, reaction time 120min, and reaction generates High temperature magnesium vapor and solid state reduction slag, magnesium vapor are collected to obtain solid metallic magnesium by condensation-crystallization；
Sodium aluminate solution is generated Step 4: the solid state reduction slag in step 3 is reacted with sodium carbonate liquor, and by step Room temperature CO after cooling in two2It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain aluminum hydroxide precipitation and sodium carbonate liquor, carbon The Leach reaction of the reusable reducing slag in this step of acid sodium solution, the sodium carbonate liquor reacted with solid state reduction slag can also Reasonable supplement is carried out by the external world according to actual use situation；Further, in this embodiment react with solid state reduction slag Sodium carbonate liquor concentration is 120g/L, and solution temperature is 85 DEG C.
The solid-state Al (OH) for again obtaining step 4 in the present embodiment3200min, Al (OH) are calcined at 1100 DEG C3Calcining Al is obtained after dehydration2O3, Al2O3Further electrolysis obtains metallic aluminium, as the raw material for preparing reducing agent aluminium powder.
Embodiment 4
A kind of Smelting magnesium technique of exhaust gas waste residue recoverable of the present embodiment, step is substantially the same manner as Example 1, The difference is that:
Step 1: ingredient is carried out according to mass ratio of each component, wherein 70 parts of dolomites and 22 parts of magnesite are uniformly mixed Obtain mixed powder, then weigh that the reducing agent aluminium powder that 8 parts of granule sizes are 165 mesh, purity is 99% is spare, three kinds of materials it is total Mass fraction is 100 parts；
Step 2: the qualified mixed powder of dolomite and magnesite and 8 parts of aluminium powders are squeezed with ball press after mixing At pelletizing, qualified pelletizing equivalent diameter is 35mm, and then pelletizing is sent into reductive jar and is calcined, when pelletizing is calcined in reductive jar Temperature be 1000 DEG C, pressure is micro-positive pressure, calcination time 110min, the high temperature CO released in calcination process2Import heat Heat is for the combustion air in preheating reduction furnace after exchanger；Qualified mixed powder is by 70 parts of dolomite in the present embodiment Magnesite with 22 parts is ground and is sieved in band sieve ball mill, and the granule size of acquisition is the material of 100~200 mesh；
Step 3: after dolomite in pelletizing and magnesite decompose completely, reductive jar is taken out into sealing and vacuum is to absolute pressure It is lower than 100Pa by force, adjustment reduction furnace temperature rises to 1200 DEG C and also originated in magnesium reaction, reaction time 220min, and reaction generates High temperature magnesium vapor and solid state reduction slag, magnesium vapor are collected to obtain solid metallic magnesium by condensation-crystallization；
Sodium aluminate solution is generated Step 4: the solid state reduction slag in step 3 is reacted with sodium carbonate liquor, and by step Two kinds of room temperature CO after cooling2It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain aluminum hydroxide precipitation and sodium carbonate liquor, carbon The Leach reaction of the reusable reducing slag in this step of acid sodium solution, the sodium carbonate liquor reacted with solid state reduction slag can also Reasonable supplement is carried out by the external world according to actual use situation；Further, in this embodiment react with solid state reduction slag Sodium carbonate liquor concentration is 130g/L, and solution temperature is 95 DEG C.
The solid-state Al (OH) for again obtaining the step in the present embodiment3300min, Al (OH) are calcined at 1200 DEG C3Calcining Al is obtained after dehydration2O3, Al2O3Further electrolysis obtains metallic aluminium, as the raw material for preparing reducing agent aluminium powder.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.

Claims (10)

1. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable, it is characterised in that: the following steps are included:
Step 1: carrying out ingredient: the mixing of 60~70 parts of dolomites and 18~25 parts of magnesite composition according to mass ratio of each component 8~15 parts of powder, reducing agent aluminium powder, gross mass number are 100 parts；
Step 2: the qualified mixed powder of dolomite and magnesite and aluminium powder pressed pellet after mixing are then fed into also It is calcined in former tank, the high temperature CO released2Room temperature is down to after the combustion air of delivery heat exchanger preheating reduction furnace；
Step 3: reductive jar is evacuated to absolute pressure lower than 100Pa, adjustment reduction furnace temperature is also originated in magnesium reaction, Generate high temperature magnesium vapor and solid state reduction slag；
Sodium aluminate solution is generated Step 4: the solid state reduction slag in step 3 is reacted with sodium carbonate liquor, and step 2 is obtained The room temperature CO arrived2It is passed through sodium aluminate solution and carries out carbon point decomposition, obtain aluminium hydroxide and sodium carbonate liquor, sodium carbonate liquor repeats It is used in this step.
2. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: by step Aluminium hydroxide obtained in four is calcined to obtain aluminium oxide, and the metallic aluminium that electrolysis of aluminum oxide obtains is used to prepare in step 1 Reducing agent aluminium powder.
3. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 2 Described in qualification mixed powder be that the mixed powder of dolomite and magnesite is ground and sieved in band sieve ball mill, obtain Obtain the material that granularity is 100~200 mesh.
4. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 1 Described in reducing agent aluminium powder granule size be greater than 150 mesh.
5. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 3 It is middle will reduction furnace temperature rise to 1100~1200 DEG C also originated in magnesium react 30~360min.
6. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 2 Temperature when middle pelletizing is calcined in reductive jar is 900~1000 DEG C, and pressure is negative pressure or micro-positive pressure.
7. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 2 It is middle that dolomite, magnesite qualification mixed powder and aluminium powder are squeezed into pelletizing, qualified pelletizing etc. with ball press after mixing It imitates diameter and is no more than 50mm.
8. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 4 In the sodium carbonate liquor that is reacted with solid state reduction slag supplemented by the external world.
9. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 1, it is characterised in that: step 4 In the sodium carbonate liquor concentration that reacts with solid state reduction slag be 100~130g/L, solution temperature is 80~95 DEG C.
10. a kind of Smelting magnesium technique of exhaust gas waste residue recoverable according to claim 2, it is characterised in that: to step The temperature that aluminium hydroxide obtained in rapid four is calcined is 1000~1200 DEG C, and calcination time is 120~360min.
CN201910354623.1A 2019-04-29 2019-04-29 A kind of Smelting magnesium technique of exhaust gas waste residue recoverable Pending CN110055409A (en)

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JP2005213652A (en) * 2000-02-24 2005-08-11 Fujitsu Ltd Method for recycling magnesium alloy material and recycling system
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