CN108998612A - A kind of method that boron, iron, magnesium recycle in paigeite - Google Patents

A kind of method that boron, iron, magnesium recycle in paigeite Download PDF

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Publication number
CN108998612A
CN108998612A CN201810908457.0A CN201810908457A CN108998612A CN 108998612 A CN108998612 A CN 108998612A CN 201810908457 A CN201810908457 A CN 201810908457A CN 108998612 A CN108998612 A CN 108998612A
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magnesium
iron
paigeite
boron
recycle
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黄伟军
刘亚静
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Hebei University of Engineering
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Hebei University of Engineering
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/006Starting from ores containing non ferrous metallic oxides
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/002Use of waste materials, e.g. slags
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/0066Preliminary conditioning of the solid carbonaceous reductant
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/008Use of special additives or fluxing agents
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21BMANUFACTURE OF IRON OR STEEL
    • C21B13/00Making spongy iron or liquid steel, by direct processes
    • C21B13/08Making spongy iron or liquid steel, by direct processes in rotary furnaces
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20Obtaining alkaline earth metals or magnesium
    • C22B26/22Obtaining magnesium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/06Dry methods smelting of sulfides or formation of mattes by carbides or the like
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/16Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a kind of methods that boron, iron, magnesium recycle in paigeite, belong to field of metallurgy, including smelting in rotary kiln, vacuum reduction separation.The present invention can be such that the elements such as iron, boron, magnesium in paigeite are efficiently separated, and improve the grade and recovery rate of iron, magnesium, while the boracic tailings generated is recycled, and the comprehensive utilization of complicated paigeite is promoted.

Description

A kind of method that boron, iron, magnesium recycle in paigeite
Technical field
The present invention relates to metallurgical slag comprehensive utilization of resources, especially a kind of processing method of paigeite belongs to field of metallurgy.
Background technique
Currently, boron magnesium ore of the boron rock production mainly from Liaoning metamorphosed sedimentary type, but such mine only accounts for national boron and always stores up The 8.98% of amount, and by the development and utilization of many years, for the reserves of boron magnesium ore less than 2,000,000 tons, boron magnesium ore resource is closely exhausted, With the development of national economy, for the demand of boron in rapid growth, available boron resource is not able to satisfy the need of all trades and professions It asks.However, China's paigeite is resourceful, only the ferro-boron ore reserves of Liaoning Area is just up to 2.8 hundred million tons, wherein with B2O3Count reserves 21840000 tons, mainly there are boromagnesite-magnetic iron ore-serpentine type and the boromagnesite of ludwigite containing ulrichile-magnetic iron ore type two Kind.
China's ferro-boron Ore performance: (1) complicated composition, it has been found that more than paragenous mineral 60, major metal mineral are magnet Mine, boromagnesite, ulrichile and ludwigite, in addition there are a small amount of magnetic iron ore, pyrite, chalcopyrites etc.;Nonmetallic mineral Predominantly serpentine, followed by mica, feldspar, calcite, quartz etc..(2) the close symbiosis of magnetic iron ore, boromagnesite, ludwigite, With the close adhesion such as serpentine, magnetic iron ore, mica, symbiosis is close, and crystal stock is sufficiently complex.(3) mineral in particulate not Uniform embedding cloth, physicochemical properties difference between mineral.Paigeite is pointed, and for granularity in 0.001~0.01mm, boromagnesite is more For threadiness, granularity is in 0.003~0.06mm, and magnetic iron ore granularity is usually 0.002~0.1mm, therefore comprehensive development and utilization is multiple Miscellaneous ferro-boron ore resources have become a top priority.
Currently, having wet separation technique, fire concentrate technique and traditional Mineral separation work to the main smelting process of paigeite Skill etc..The method of wet separation technique mainly uses acid, alkali, salt solution, then boric acid is extracted from leachate, and phase analysis is through magnetic Choosing obtains iron ore concentrate, separates ferro-boron.Paigeite fire concentrate technique mainly extracts metal or gold using high temperature from ore Belong to the method for oxide, feature is that process flow is short, equipment is simple, good in economic efficiency, and paigeite fire concentrate method mainly has Blast furnace process, reduction-magnetic separation separating technology, direct-reduction-fusing separating technology etc..Traditional ore-dressing technique mainly passes through fine grinding- Magnetic separation obtains iron ore concentrate and boracic tailings.This three kinds of schemes can complete the separation of iron and boron in paigeite to a certain extent, Former scheme can reach the spilling of preferable iron, the boron rate of recovery and boron oxide, but process flow is long, and pollution is big;Latter two side Case iron, boron separating effect are not fine.In addition, content of magnesium is higher in paigeite, boron concentrate is seriously affected after ferro-boron separation It further smelts, and under the conditions of current smelting process, the utilization rate of magnesium is relatively low, is substantially discharged with form of waste, Not only land occupation has an effect on environment.Up to the present there has been no a kind of effective smeltings that can separate and recover iron in paigeite, boron, magnesium simultaneously Smelting method.Therefore, how the research of high-efficiency comprehensive utilization paigeite is that China's boron, iron, be becoming tight magnesium ore resources day tool to alleviating There is great meaning.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of methods that boron, iron, magnesium recycle in paigeite, can The elements such as the iron in paigeite, boron, magnesium are efficiently separated, improve the grade and recovery rate of iron, magnesium, while what is generated contains Boron tailings is recycled, and the comprehensive utilization of complicated paigeite is promoted.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
A kind of method that boron, iron, magnesium recycle in paigeite, including smelting in rotary kiln, vacuum reduction separation.
Technical solution of the present invention further improvement lies in that the following steps are included:
A. mixing: paigeite powder, iron reducer, modification agent are uniformly mixed;
B. smelting in rotary kiln: the powder after mixing is packed into rotary kiln, is heated and is kept the temperature;
C. separate metal sponge iron: after heat preservation, magnetic separation separation obtains metal sponge iron and boron magnesium tailings;
D. vacuum reduction separates: boron magnesium tailings, magnesium reducing agent being uniformly mixed, is placed in vacuum high temperature furnace and is heated simultaneously Heat preservation, the gas phase generated in insulating process is condensed step by step, separates magnesium metal;
E. it recycles tailings: recycling high boron tailings.
Technical solution of the present invention further improvement lies in that: paigeite powder granularity≤100 mesh.
Technical solution of the present invention further improvement lies in that: in step A iron reducer be low-sulfur coal or coke breeze, iron reduction The additional amount of agent is the 10~15% of paigeite powder gross mass;Magnesium reducing agent is CaC in step D2, the additional amount of magnesium reducing agent is The 30~40% of paigeite powder gross mass;The granularity of iron reducer and magnesium reducing agent≤100 mesh.
Technical solution of the present invention further improvement lies in that: modification agent is calcium oxide in step A, and the additional amount of modification agent is The 4~6% of paigeite powder gross mass, granularity≤100 mesh.
Technical solution of the present invention further improvement lies in that: in step B, be heated to be microwave heating, heating temperature 1000 ~1200 DEG C, soaking time is 1~1.5 hour.
Technical solution of the present invention further improvement lies in that: in step C magnetic separation separate magnetic induction intensity be 1~2T.
Technical solution of the present invention further improvement lies in that: in step D, heating temperature is 1150~1250 DEG C, when heat preservation Between 1.5~2 hours, high-temperature vacuum furnace pressure be 3~10Pa.
Technical solution of the present invention further improvement lies in that: in step D, gas phase is condensed into step by step starts to be cooled to 350 DEG C Collect the magnesium metal of condensation;350 DEG C or less are collected the metallic sodium and metallic potassium condensed.
Technical solution of the present invention further improvement lies in that: metal sponge iron as steel-making or Magnetite (processed) raw material;Magnesium metal It is used to prepare magnesium alloy, magnesium compound or is used as deoxidier, desulfurizing agent;High boron tailings is used to prepare alkali-free glass or borax.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
The method that boron in a kind of paigeite provided by the invention, iron, magnesium recycle, can make iron in paigeite, boron, The elements such as magnesium are efficiently separated, and improve the grade and recovery rate of iron, magnesium, while the boracic tailings generated has obtained circulation benefit With promoting the comprehensive utilization of complicated paigeite.
The present invention restores the oxide of iron in paigeite to obtain metal sponge iron using microwave heating technique, then uses Magnetic separation carries out separation metal sponge iron.Wave is inhaled with containing boron oxide compound (boromagnesite) using oxides-containing iron in paigeite (magnetic iron ore) The difference of ability heats paigeite using microwave, is conducive to generate thermal stress between magnetic iron ore, boromagnesite, is formed brilliant Between crackle, promote iron, boron separation;Simultaneously through aoxidizing calcium desulfurizing, smelting in rotary kiln can be continuously produced the metal of low-sulfur high quality Sponge iron can reach the purpose of separation and concentration metal sponge iron through magnetic separation;Furthermore the boron magnesium tailings after magnetic separation through vacuum reduction at Reason can be such that boron, magnesium is efficiently separated.When raw ore microwave heating is to 1000~1200 DEG C, heat preservation 1~1.5 hour obtains after magnetic separation To metal sponge iron in Iron grade be up to 90% or more, iron recovery is up to 80% or more;Boron magnesium tailings is 1150~1250 DEG C, soaking time is 1.5~2 hours, and after vacuum reduction is handled, the rate of recovery of magnesium is up to 85% or more, and the grade of magnesium is up to 95% or more.Entire reaction process homogeneous heating, heating speed are fast, not only shorten heating and soaking time, have also speeded up anti- The discharge answered rate, reduce pollutant has few simple production process, equipment investment, high production efficiency, energy-saving and environment-friendly excellent Point.
The present invention joined modification agent and iron reducer in the reduction of ferriferous oxide, when modification agent is calcium oxide, additional amount It is the 4~6% of paigeite powder gross mass, when granularity≤100 mesh, can effectively removes the sulphur in iron, obtain low-sulfur sponge iron, be used for Magnetite (processed) or steelmaking feed.When iron reducer is low-sulfur coal or coke breeze, additional amount is the 10~15% of paigeite powder gross mass, When granularity≤100 mesh, boromagnesite, serpentine are decomposed, and the oxide of iron is quickly and effectively restored, and are convenient for subsequent separation, are improved The rate of recovery of iron.In addition, low-sulfur coal or coke breeze are cheap and easy to get, production cost is reduced.It is chemically reacted during reduced iron It is as follows:
2MgBO2(OH)=2MgOB2O3+H2O (1)
2Mg3Si2O5(OH)4=3Mg2SiO4+SiO2+4H2O (2)
3Fe2O3+ CO=2Fe3O4+CO2 (3)
Fe3O4+ CO=3FeO+CO2 (4)
Fe3O4+ C=3FeO+CO (5)
FeO+C=Fe+CO (6)
SiO2+ xCaO=xCaOSiO2(3≥x≥0.5) (7)
CaO+S+C=CaS+CO (8)
SiO2+ 2MgO=2MgOSiO2 (9)
Magnesium reducing agent is added in boron magnesium tailings of the present invention after separating iron, when magnesium reducing agent is CaC2, magnesium reducing agent plus Enter 30~40% that amount is paigeite powder gross mass, when granularity≤100 mesh, MgO can be made to restore rapidly, is obtained convenient for subsequent Boron, magnesium separation, improve the rate of recovery of magnesium.Occur such as to issue during vacuum reduction and answer:
2MgO·B2O3+2CaC2+ CaO=3CaOB2O3+4C+2Mg (10)
MgO+CaC2=CaO+2C+Mg (11)
3MgO+CaC2=CaO+2CO+3Mg (12)
2MgO·SiO2+4CaC2=4CaO+SiC+7C+2Mg (13)
2MgO·SiO2+2CaC2=2CaO+SiC+2CO+C+2Mg (14)
The present invention is separated using vacuum reduction, easy to operate, and non-exhaust emission.Gas phase cooling procedure be from 1150~ 1250 DEG C gradually cooling down, cooling initial stage, the high magnesium metal cooled and solidified of boiling point are collected, are boiled when cooling down to a certain extent The low sodium of point, potassium condensation remove.The boiling point of Mg is 1107 DEG C, and fusing point is 648 DEG C, collects 350 DEG C or more liquid or solids and is Magnesium metal;The boiling point of sodium is 883 DEG C, and fusing point is 97.72 DEG C;The boiling point of potassium be 770 DEG C, fusing point be 63 DEG C, vacuum degree be 3~ When 10Pa, sodium, potassium are condensed out with liquid phase at 345 DEG C or less, and have 99.98% or more metal at 350 DEG C or more Magnesium condenses.Therefore, enriched in metals Mg is condensed when since cooling to 350 DEG C, then in 350 DEG C or less condensation enriched in metals Sodium, potassium can achieve good separating effect.
Present invention paigeite to be processed is complicated compound paigeite powder, processing through the invention, so that largely having Valence resource is fully used, and current iron, boron, magnesium resource anxiety problem are alleviated.When granularity≤100 mesh so that raw material with Reducing agent, modification agent mix more uniform, convenient for the reduction of subsequent iron with separate.
Adaptability to raw materials of the present invention is strong, is applicable to the paigeite of heterogeneity range, and iron recovery is high, up to 80% with On;The rate of recovery of magnesium is up to 85% or more, the magnesium metal of generation can be used for preparing magnesium alloy, magnesium compound or be used as deoxidier, Desulfurizing agent;Boracic tailings can be used for alkali-free glass processed, borax, and tailings is fully used, and efficiently solve waste residue land occupation Problem, realizing turns waste into wealth and the utilization of the efficient circulation of resource.
The present invention by microwave heating, carbon bathe low-temperature reduction, oxidation calcium desulfurizing and magnetic separation separation reach in paigeite iron with Boron, magnesium separate, and Iron grade is up to 90% or more in metal sponge iron, and the rate of recovery of iron is up to 80% or more, can be used for Magnetite (processed) Or steelmaking feed, and the grade of boron magnesium has compared with raw ore and is significantly promoted in the tailings after magnetic separation, furthermore tailings is through CaC2Vacuum is also Utilization can be further processed in original place reason, the magnesium products for efficiently separating the valuable elements such as boron, magnesium, and obtaining, and boracic tailings can quilt Effective use.
The present invention solves paigeite because iron, boron, the phase composition of magnesium mine and embedding cloth relationship are complicated, it is difficult to utilize traditional mining and metallurgy Technology realizes the problem of complex utilization of such ore, so that a large amount of intractable ferro-boron ore resources are fully used.Entirely Production process reaction rate is fast, high production efficiency, reduces the discharge of pollutant, improves product quality, economic and environment-friendly.
Specific embodiment
Here is certain specific embodiments of the invention, to be described in further detail.
A kind of method that boron, iron, magnesium recycle in paigeite, including smelting in rotary kiln, vacuum reduction separation, including with Lower step:
A. mixing: paigeite powder, iron reducer, modification agent are added in batch mixer, mixed well.Paigeite powder granularity≤ 100 mesh;Iron reducer is low-sulfur coal or coke breeze, and the additional amount of iron reducer is the 10~15% of paigeite powder gross mass, grain Spend≤100 mesh;Modification agent is calcium oxide, and the additional amount of modification agent is the 4~6% of paigeite powder gross mass, granularity≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, microwave heating to 1000~1200 DEG C, heat preservation 1~ 1.5 hours, the oxide of iron is restored.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 1~2T magnetic induction intensity, obtain metal sea Continuous iron and boron magnesium tailings.
D. vacuum reduction separates: boron magnesium tailings, magnesium reducing agent being added in batch mixer and be uniformly mixed, is placed in vacuum high temperature furnace In be heated to 1150~1250 DEG C, keep the temperature 1.5~2 hours, high-temperature vacuum furnace pressure is 3~10Pa, by the oxidation of magnesium Object reduction.Magnesium reducing agent is CaC2, the additional amount of magnesium reducing agent is the 30~40% of paigeite powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge iron is as steel-making or Magnetite (processed) raw material;Magnesium metal is used to prepare magnesium alloy, magnesium compound or is used as de- Oxygen agent, desulfurizing agent;High boron tailings is used to prepare alkali-free glass or borax.
Embodiment 1
Using somewhere 1# paigeite, chemical component TFe:34.30%, Fe3O4: 28.34%, FeO:17.70%, B2O3: 8.73%, MgO:28.05%, SiO2: 15.22%, CaO:0.75%, other oxides: 1.21%.
Method that boron in paigeite, iron, magnesium recycle the following steps are included:
A. mixing: paigeite powder, low-sulfur coal, calcium oxide are added in batch mixer, mixed well.The additional amount of low-sulfur coal is The 13% of paigeite powder gross mass, the additional amount of calcium oxide are the 6% of paigeite powder gross mass, paigeite powder, low-sulfur coal, oxidation Calcium grain degree≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, and microwave heating keeps the temperature 1.2 hours to 1200 DEG C, will The oxide of iron restores.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 1.5T magnetic induction intensity, obtain metal sponge Iron and boron magnesium tailings.
D. vacuum reduction separates: by boron magnesium tailings, CaC2It is added in batch mixer and is uniformly mixed, be placed in vacuum high temperature furnace and add Heat keeps the temperature 1.5 hours to 1200 DEG C, and high-temperature vacuum furnace pressure is 3Pa, and the oxide of magnesium is restored.CaC2Additional amount be The 40% of paigeite powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge Iron grade is 94%, the rate of recovery 85%, the raw material as steel-making;Magnesium metal grade up to 96% with On, the rate of recovery 86% is used to prepare magnesium alloy;Boracic tailings grade can be used for preparing alkali-free glass up to 13% or more.
Embodiment 2
Using somewhere 1# paigeite, chemical component TFe:34.30%, Fe3O4: 28.34%, FeO:17.70%, B2O3: 8.73%, MgO:28.05%, SiO2: 15.22%, CaO:0.75%, other oxides: 1.21%.
Method that boron in paigeite, iron, magnesium recycle the following steps are included:
A. mixing: paigeite powder, coke breeze, calcium oxide are added in batch mixer, mixed well.The additional amount of low-sulfur coal is The 15% of paigeite powder gross mass, the additional amount of calcium oxide are the 5% of paigeite powder gross mass, paigeite powder, low-sulfur coal, oxidation Calcium grain degree≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, and microwave heating keeps the temperature 1.5 hours to 1000 DEG C, will The oxide of iron restores.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 1.2T magnetic induction intensity, obtain metal sponge Iron and boron magnesium tailings.
D. vacuum reduction separates: by boron magnesium tailings, CaC2It is added in batch mixer and is uniformly mixed, be placed in vacuum high temperature furnace and add Heat keeps the temperature 2 hours to 1150 DEG C, and high-temperature vacuum furnace pressure is 5Pa, and the oxide of magnesium is restored.CaC2Additional amount be boron The 38% of Iron Ore Powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge Iron grade is 95%, the rate of recovery 88%, the raw material as Magnetite (processed);Magnesium metal grade up to 98% with On, the rate of recovery 88% is used to prepare magnesia;Boracic tailings grade can be used for preparing borax up to 13% or more.
Embodiment 3
Using somewhere 2# paigeite, chemical component TFe:25.52%, Fe3O4: 24.42%, FeO:9.44%, B2O3: 10.97%, MgO:23.50%, SiO2: 20.29%, CaO:0.92%, other oxides: 10.46%.
Method that boron in paigeite, iron, magnesium recycle the following steps are included:
A. mixing: paigeite powder, low-sulfur coal, calcium oxide are added in batch mixer, mixed well.The additional amount of low-sulfur coal is The 10% of paigeite powder gross mass, the additional amount of calcium oxide are the 4% of paigeite powder gross mass, paigeite powder, low-sulfur coal, oxidation Calcium grain degree≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, and microwave heating keeps the temperature 1 hour, by iron to 1200 DEG C Oxide reduction.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 1.5T magnetic induction intensity, obtain metal sponge Iron and boron magnesium tailings.
D. vacuum reduction separates: by boron magnesium tailings, CaC2It is added in batch mixer and is uniformly mixed, be placed in vacuum high temperature furnace and add Heat keeps the temperature 2 hours to 1150 DEG C, and high-temperature vacuum furnace pressure is 7Pa, and the oxide of magnesium is restored.CaC2Additional amount be boron The 30% of Iron Ore Powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge Iron grade is 92%, the rate of recovery 89%, the raw material as steel-making;Magnesium metal grade up to 97% with On, the rate of recovery 86% is used to prepare magnesium chloride;Boracic tailings grade can be used for preparing alkali-free glass up to 13% or more.
Embodiment 4
Using somewhere 2# paigeite, chemical component TFe:25.52%, Fe3O4: 24.42%, FeO:9.44%, B2O3: 10.97%, MgO:23.50%, SiO2: 20.29%, CaO:0.92%, other oxides: 10.46%.
Method that boron in paigeite, iron, magnesium recycle the following steps are included:
A. mixing: paigeite powder, coke breeze, calcium oxide are added in batch mixer, mixed well.The additional amount of low-sulfur coal is The 12% of paigeite powder gross mass, the additional amount of calcium oxide are the 5% of paigeite powder gross mass, paigeite powder, low-sulfur coal, oxidation Calcium grain degree≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, and microwave heating keeps the temperature 1.5 hours to 1100 DEG C, will The oxide of iron restores.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 1T magnetic induction intensity, obtain metal sponge iron With boron magnesium tailings.
D. vacuum reduction separates: by boron magnesium tailings, CaC2It is added in batch mixer and is uniformly mixed, be placed in vacuum high temperature furnace and add Heat keeps the temperature 1.8 hours to 1200 DEG C, and high-temperature vacuum furnace pressure is 10Pa, and the oxide of magnesium is restored.CaC2Additional amount be The 35% of paigeite powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge Iron grade is 95%, the rate of recovery 87%, the raw material as Magnetite (processed);Magnesium metal grade up to 98% with On, the rate of recovery 88% is used to prepare magnesium hydroxide;Boracic tailings grade can be used for preparing borax up to 13% or more.
Embodiment 5
Using somewhere 3# paigeite, chemical component TFe:31.02%, Fe3O4: 29.73%, FeO:11.56%, B2O3: 9.34%, MgO:27.40%, SiO2: 14.90%, CaO:0.75%, other oxides: 6.32%.
Method that boron in paigeite, iron, magnesium recycle the following steps are included:
A. mixing: paigeite powder, low-sulfur coal, calcium oxide are added in batch mixer, mixed well.The additional amount of low-sulfur coal is The 12% of paigeite powder gross mass, the additional amount of calcium oxide are the 5% of paigeite powder gross mass, paigeite powder, low-sulfur coal, oxidation Calcium grain degree≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, and microwave heating keeps the temperature 1.5 hours to 1100 DEG C, will The oxide of iron restores.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 1.2T magnetic induction intensity, obtain metal sponge Iron and boron magnesium tailings.
D. vacuum reduction separates: by boron magnesium tailings, CaC2It is added in batch mixer and is uniformly mixed, be placed in vacuum high temperature furnace and add Heat keeps the temperature 2 hours to 1180 DEG C, and high-temperature vacuum furnace pressure is 6Pa, and the oxide of magnesium is restored.CaC2Additional amount be boron The 37% of Iron Ore Powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge Iron grade is 95%, the rate of recovery 82%, as Magnetite (processed) raw material;Fractional condensaion magnesium grade is up to 97% More than, the rate of recovery 87%, as the raw material of industry;Boracic tailings grade can be used for preparing borax up to 13% or more.
Embodiment 6
Using somewhere 3# paigeite, chemical component TFe:31.02%, Fe3O4: 29.73%, FeO:11.56%, B2O3: 9.34%, MgO:27.40%, SiO2: 14.90%, CaO:0.75%, other oxides: 6.32%.
Method that boron in paigeite, iron, magnesium recycle the following steps are included:
A. mixing: paigeite powder, coke breeze, calcium oxide are added in batch mixer, mixed well.The additional amount of low-sulfur coal is The 15% of paigeite powder gross mass, the additional amount of calcium oxide are the 6% of paigeite powder gross mass, paigeite powder, low-sulfur coal, oxidation Calcium grain degree≤100 mesh.
B. smelting in rotary kiln: being packed into rotary kiln for the powder after mixing, and microwave heating keeps the temperature 1.2 hours to 1200 DEG C, will The oxide of iron restores.
C. it separates metal sponge iron: after reduction, carrying out magnetic separation separation with 2T magnetic induction intensity, obtain metal sponge iron With boron magnesium tailings.
D. vacuum reduction separates: by boron magnesium tailings, CaC2It is added in batch mixer and is uniformly mixed, be placed in vacuum high temperature furnace and add Heat keeps the temperature 1.8 hours to 1250 DEG C, and high-temperature vacuum furnace pressure is 8Pa, and the oxide of magnesium is restored.CaC2Additional amount be The 35% of paigeite powder gross mass, granularity≤100 mesh.
The gas phase generated in insulating process is condensed step by step, starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350℃ The metallic sodium and metallic potassium of condensation are collected below.
E. it recycles tailings: recycling high boron tailings.
Metal sponge Iron grade is 93%, the rate of recovery 85%, as Magnetite (processed) raw material;Fractional condensaion magnesium grade is up to 98% More than, the rate of recovery 86%, as the raw material of industry;Boracic tailings grade can be used for preparing borax up to 13% or more.

Claims (10)

1. a kind of method that boron, iron, magnesium recycle in paigeite, it is characterised in that: including smelting in rotary kiln, vacuum reduction point From.
2. the method that boron in a kind of paigeite according to claim 1, iron, magnesium recycle, it is characterised in that including with Lower step:
A. mixing: paigeite powder, iron reducer, modification agent are uniformly mixed;
B. smelting in rotary kiln: the powder after mixing is packed into rotary kiln, is heated and is kept the temperature;
C. separate metal sponge iron: after heat preservation, magnetic separation separation obtains metal sponge iron and boron magnesium tailings;
D. vacuum reduction separates: boron magnesium tailings, magnesium reducing agent being uniformly mixed, is placed in vacuum high temperature furnace and is heated and protected Temperature condenses the gas phase generated in insulating process step by step, separates magnesium metal;
E. it recycles tailings: recycling high boron tailings.
3. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: paigeite Powder Particle Size≤100 mesh.
4. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: step A Middle iron reducer is low-sulfur coal or coke breeze, and the additional amount of iron reducer is the 10 ~ 15% of paigeite powder gross mass;Magnesium in step D Reducing agent is CaC2, the additional amount of magnesium reducing agent is the 30 ~ 40% of paigeite powder gross mass;The grain of iron reducer and magnesium reducing agent Spend≤100 mesh.
5. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: step A In, modification agent is calcium oxide, and the additional amount of modification agent is the 4 ~ 6% of paigeite powder gross mass, granularity≤100 mesh.
6. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: step B In, it is heated to be microwave heating, heating temperature is 1000 ~ 1200 DEG C, and soaking time is 1 ~ 1.5 hour.
7. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: step C The magnetic induction intensity of middle magnetic separation separation is 1 ~ 2T.
8. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: step D In, heating temperature is 1150 ~ 1250 DEG C, and soaking time 1.5 ~ 2 hours, high-temperature vacuum furnace pressure was 3 ~ 10Pa.
9. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: step D In, gas phase is condensed into step by step starts to be cooled to 350 DEG C of magnesium metals for collecting condensation;350 DEG C or less collect condensation metallic sodium and Metallic potassium.
10. the method that boron, iron, magnesium recycle in a kind of paigeite according to claim 2, it is characterised in that: metal Sponge iron is as steel-making or Magnetite (processed) raw material;Magnesium metal is used to prepare magnesium alloy, magnesium compound or is used as deoxidier, desulfurizing agent; High boron tailings is used to prepare alkali-free glass or borax.
CN201810908457.0A 2018-08-10 2018-08-10 A kind of method that boron, iron, magnesium recycle in paigeite Pending CN108998612A (en)

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Application publication date: 20181214