CN107670815B - A method of iron in recycling material containing fayalite is leached using mechanical ball mill - Google Patents

A method of iron in recycling material containing fayalite is leached using mechanical ball mill Download PDF

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CN107670815B
CN107670815B CN201710883480.4A CN201710883480A CN107670815B CN 107670815 B CN107670815 B CN 107670815B CN 201710883480 A CN201710883480 A CN 201710883480A CN 107670815 B CN107670815 B CN 107670815B
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iron
fayalite
material containing
ball mill
magnetic
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CN107670815A (en
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刘恢
王忠兵
彭兵
柴立元
赵宗文
李燕春
朱顺
梁彦杰
陈玉洁
刘德刚
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Central South University
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Central South University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00—Disintegrating plant with or without drying of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C25/00—Control arrangements specially adapted for crushing or disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00—Magnetic separation
    • B03C1/02—Magnetic separation acting directly on the substance being separated

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of methods for leaching iron in recycling material containing fayalite using mechanical ball mill.This method is that will contain after fayalite material is crushed, is sieved, and with hydrogen peroxide mixing and ball milling, obtains product containing magnetic iron oxide, to get Armco magnetic iron concentrate, nonmagnetic portion is tailings gangue for magnetic separation separation.This method by fayalite class metallurgical slag can not reuse iron resource orientation regulation be converted into recyclable iron ore concentrate, realize minimizing and the secondary resource of metallurgical slag, it solves waste residue terminal open circuit, domestic high grade iron ore resource scarcity and problem of environmental pollution, opens a Green Sustainable road for the processing of metallurgy industry waste residue.

Description

A method of iron in recycling material containing fayalite is leached using mechanical ball mill
Technical field
The present invention relates to iron recovery methods in material containing fayalite, in particular to a kind of to utilize mechanical ball mill to fuming The recovery method of iron in the materials containing fayalite such as slag, copper ashes, nickel slag；Belong to metallurgical engineering and field of environment engineering.
Background technique
China is the first in the world steel big producer, but China's iron ore deposit is poor, and a large amount of iron ore deposit is by external Import, China's iron ore rely on import continuous 6 years more than 60%.At the same time, China generates a large amount of metallurgical slags every year, According to statistics, China's copper ashes yield in 2016 is about ten thousand tons of 1688-2550；Nickel slag is about 5,000,000 tons；Lead skim is about 3,000,000 tons. The a large amount of iron resource of association in these metallurgical slags, iron-content 30-60%.Much higher than the average product for smelting iron ore 29.1% Position is a kind of potential iron resource, but 80% or more iron mutually exists in such slag with fayalite, and disseminated grain size is superfine, ferrosilicon It is difficult to separate, causes iron in such ferrosilicon composite oxides that cannot reasonably recycle, give up as the unavailable iron of industry always Abandoning does not have to.These waste residues are largely stored up at present, cause environmental pollution and the wasting of resources.Recycle the iron olives such as copper ashes, lead skim, nickel slag Minimizing and iron resource of the iron resource for metallurgical slag in stone class metallurgical slag, make up the long-term short of China's iron ore resource It lacks and is of great significance.
Since fayalite property is stablized, in the existing recovery method reported both at home and abroad, need mostly in high temperature and atmosphere Lower Roasting Decomposition, then through the isolated iron ore concentrate of magnetic separation.Such as poplar Chinese toon, Zhang Linnan are reported first by copper ashes on 1100 DEG C of left sides Right progress oxidizing roasting 1-2h, then magnetic iron ore is obtained through magnetic separation.Zhao Kai etc. is roasted using carbon direct-reduction process at 900 DEG C, control Calcining time, then simple substance crude iron or magnetic iron ore are obtained through magnetic separation.Li Yanchun etc. (Chinese Patent Application No. 201510572205.1) By fayalite class metallurgical slag in SO2+O2It is roasted under mixed atmosphere at 600-700 DEG C, then obtains bloodstone through magnetic separation. Li Yanchun etc. (Chinese Patent Application No. 201510568445.4) is by pyrite and fayalite class metallurgical slag under oxygen atmosphere With 300-1100 DEG C of progress oxidizing roasting, bloodstone then is obtained using magnetic separation.
In conclusion the recovery method of iron resource has high energy consumption in fayalite class metallurgical slag at present, easily cause Secondary pollution problems.The recycling of iron resource is that metallurgy and environmental area letter are to be solved in fayalite class metallurgical slag Problem, there is an urgent need to a kind of iron moneys of association in energy conservation, the process recycling fayalite class metallurgical slag that efficient, process is short Source.
Summary of the invention
It is asked to solve high energy consumption, secondary pollution existing for the recovery method of iron etc. in existing fayalite class metallurgical slag Topic, the purpose of the invention is to provide a kind of low energy consumption, clean and environmental protection, can efficiently realize fayalite class metallurgical slag The method of enrichment and the recycling of middle iron, this method realize the recycling benefit of the waste residues such as fuming slag, copper ashes, nickel slag under the conditions of normality With.
In order to achieve the above technical purposes, recycling object containing fayalite is leached using mechanical ball mill the present invention provides a kind of The method of iron in material, this method are that will contain after fayalite material is crushed, is sieved, and with hydrogen peroxide mixing and ball milling, are contained Magnetic iron oxide product, magnetic separation separate to get Armco magnetic iron concentrate.
Preferred scheme, the material containing fayalite include at least one of copper ashes, nickel slag, fuming slag.Iron content olive The selection of stone material is not limited to this, and generally the material of the phase of mine containing fayalite can be implemented using the method for the present invention, Such as low-grade mineral containing fayalite.
Preferred scheme, the material containing fayalite take minus sieve material, preferably by being crushed, crossing 100~300 meshes To cross 150~250 meshes.To contain fayalite be crushed to appropriate granularity be conducive to improve ball-milling reaction efficiency.
Preferred scheme, the hydrogen peroxide concentration are 15%~30%, preferably 20~25%.
Preferred scheme, in mechanical milling process: the liquid-solid ratio of material containing fayalite and hydrogen peroxide is 1~5mL:1g；Ball milling Revolving speed is 300~600r/min, and Ball-milling Time is 3~8h.More preferably scheme, rotational speed of ball-mill are 450~550r/min, ball milling Time is 3.5~4.5h.
Preferred scheme, the magnetic field strength that the magnetic separation separation uses is 1.0~1.6 ten thousand Gauss.More preferably magnetic field is strong Degree is 1.1~1.3 ten thousand Gausses.
The ball grinder and abrading-ball that mechanical milling process of the invention uses is the materials do not reacted with hydrogen peroxide.Preferably agate material Matter.
Technical solution of the present invention key is that will contain fayalite material reacts with hydrogen peroxide progress high-energy ball milling Process, under the mechanical energy effect that high energy ball mill provides, fayalite mineral phase structure is destroyed, with pair with strong oxidizing property Oxygen water carries out oxidation reaction, obtains the ferric oxide product with weak magnetic, then separate using strong magnetic separation, available iron essence Mine, in Process During High Energy Ball Milling, the reaction mainly occurred is as follows:
Fe2SiO4+H2O2+ (mechanical energy)=Fe2O3+SiO2+H2O (1)
3Fe2SiO4+2H2O2+ (mechanical energy)=2Fe3O4+3SiO2+2H2O (2)
Compared with the prior art, technical solution of the present invention bring the utility model has the advantages that
1, technical solution of the present invention uses ball grinding technique to handle the waste residue material of the phase of mine containing fayalite for the first time, It can realize that being converted into for fayalite mine phase can be separated with other metals and non magnetic ore in a mild condition Magnetic iron ore, compare existing pyrolytic semlting treatment process, have apparent low energy consumption, mild condition, easy to operate, environmentally friendly etc. Advantage.
2, the efficiently concentrating of iron and recycling in the waste residue of class containing fayalite, iron recycling may be implemented in technical solution of the present invention Rate reaches 80% or more, and recycling iron ore grade reaches 60% or more.
3, method of the invention low energy consumption, process flow is short, it is easy to operate and without exhaust gas generate, be conducive to environmental protection.
4, method of the invention can realize the minimizing of fayalite class metallurgical slag about 40%, and it is useless to substantially increase metallurgy The secondary resourceization of slag utilizes.
Detailed description of the invention
[Fig. 1] is the process flow chart of the method for the present invention.
The XRD:A that [Fig. 2] copper ashes does not use mechanical ball mill that hydrogen peroxide is directly utilized directly to leach copper ashes) copper ashes raw material；B) Copper ashes: the direct leached mud of the non-ball milling of hydrogen peroxide 1:2.
The XRD:A that [Fig. 3] fuming slag does not use the direct mechanical ball mill of hydrogen peroxide to leach) fuming slag raw material；B) fuming slag: pure Water=1:2 ball milling leached mud.
The XRD:A that [Fig. 4] fuming slag is leached using mechanical ball mill+hydrogen peroxide) fuming slag raw material；B) fuming slag: hydrogen peroxide =1:2 ball milling leached mud.
The XRD:A that [Fig. 5] copper ashes is leached using mechanical ball mill+hydrogen peroxide) copper ashes raw material；B) copper ashes: hydrogen peroxide=1:2 ball Grind leached mud.
The XRD diagram of [Fig. 6] magnetic concentrate.
Specific embodiment
The present invention is described in further details combined with specific embodiments below, specific embodiment described herein is only used In explaining the present invention, it is not intended to restrict the invention.
Comparative example 1
Copper ashes is crushed first, crosses 200 meshes (74 μm), weighs copper ashes 30g, copper ashes main component is shown in Table 1.It is solid according to liquid 20% hydrogen peroxide 60mL of concentration is measured than 2:1.Copper ashes is mixed with hydrogen peroxide, stirs 4h using magnetic particle blender.Then it crosses Filter drying.Its product X RD figure is shown in Fig. 2.Under the premise of non-mechanical ball mill, hydrogen peroxide does not react substantially with copper ashes, main object Mutually remain as fayalite.
The main component percentage composition of 1 copper ashes of table
Comparative example 2
Fuming slag is crushed first, crosses 200 meshes (74 μm), weighs fuming slag 30g, fuming slag main component is shown in Table 2.It presses 30% hydrogen peroxide 60mL of concentration is measured according to liquid-solid ratio 2:1.Fuming slag is mixed with hydrogen peroxide, is stirred using magnetic particle blender 5h.Then filtering drying.Under the premise of non-mechanical ball mill, hydrogen peroxide does not react equally with fuming slag substantially, main object phase Remain as amorphous state object phase.
The main component percentage composition of 2 fuming slag of table
Comparative example 3
Fuming slag is crushed first, crosses 200 meshes (74 μm), weighs fuming slag 30g, fuming slag main component is shown in Table 2.It presses Pure water 60mL mixing is measured according to liquid-solid ratio 2:1.Being put into material is agate jar and pearl, under 500r/min revolving speed, ball milling 4h.Then filtering drying.Its product X RD figure is shown in Fig. 3.Under the premise of mechanical ball mill does not add hydrogen peroxide, main object phase is still For amorphous fayalite.
Embodiment 1
Copper ashes is crushed first, crosses 200 meshes (74 μm), weighs copper ashes 30g, copper ashes main component is shown in Table 1.It is solid according to liquid 20% hydrogen peroxide 60mL of concentration is measured than 2:1.Being put into material is agate jar and pearl, under 400r/min revolving speed, ball milling 4h.After use wet high-intensity magnetic separation, magnetic field strength be 1.2 ten thousand Gausses.Magnetisable material filtering drying can obtain iron ore concentrate.Leaching Material XRD diagram is shown in Fig. 4 out, and gained iron ore concentrate XRD diagram is as shown in Figure 6.The rate of recovery of iron reaches 85.3% or more, in magnetic concentrate The content of iron reaches 63.1% or more.
Embodiment 2
Fuming slag is crushed first, crosses 200 meshes (74 μm), weighs copper ashes 30g, fuming slag main component is shown in Table 2.According to Liquid-solid ratio 2:1 measures 30% hydrogen peroxide 60mL of concentration.Being put into material is agate jar and pearl, under 500r/min revolving speed, Ball milling 4h.After use wet high-intensity magnetic separation, magnetic field strength be 1.2 ten thousand Gausses.Magnetisable material filtering drying can obtain iron essence Mine.It leaches material XRD diagram and sees Fig. 5, gained iron ore concentrate XRD diagram is as shown in Figure 6.The rate of recovery of iron reaches 83% or more, magnetic separation essence The content of iron reaches 62.8% or more in mine.
Embodiment 3
Copper ashes is crushed first, crosses 200 meshes (74 μm), weighs copper ashes 30g, copper ashes main component is shown in Table 1.It is solid according to liquid 30% hydrogen peroxide 30mL of concentration is measured than 1:1.Being put into material is agate jar and pearl, under 500r/min revolving speed, ball milling 5h.After use wet high-intensity magnetic separation, magnetic field strength be 1.3 ten thousand Gausses.Magnetisable material filtering drying can obtain iron ore concentrate.Iron The rate of recovery reach 79.4% or more, the content of iron reaches 56.4% or more in magnetic concentrate.
Embodiment 4
Fuming slag is crushed first, crosses 200 meshes (74 μm), weighs copper ashes 30g, fuming slag main component is shown in Table 2.According to Liquid-solid ratio 1:1 measures 30% hydrogen peroxide 60mL of concentration.Being put into material is agate jar and pearl, under 500r/min revolving speed, Ball milling 5h.After use wet high-intensity magnetic separation, magnetic field strength be 1.3 ten thousand Gausses.Magnetisable material filtering drying can obtain iron essence Mine.The rate of recovery of iron reaches 80.3% or more, and the content of iron reaches 59.7% or more in magnetic concentrate.
By above embodiments as it can be seen that using the method for the present invention, the rate of recovery of iron in metallurgical slag can be made to reach 80% or more, The content of iron reaches 60% or more in magnetic concentrate.

Claims (6)

1. a kind of method for leaching iron in recycling material containing fayalite using mechanical ball mill, it is characterised in that: by iron content olive After stone material is crushed, is sieved, with hydrogen peroxide mixing and ball milling, product containing magnetic iron oxide is obtained, magnetic separation separates to get magnetism Iron ore concentrate；The hydrogen peroxide concentration is 15%~30%；
In mechanical milling process: the liquid-solid ratio of material containing fayalite and hydrogen peroxide is 1~5mL:1g；Rotational speed of ball-mill is 300~600r/ Min, Ball-milling Time are 3~8h.
2. a kind of method for leaching iron in recycling material containing fayalite using mechanical ball mill according to claim 1, Be characterized in that: the material containing fayalite includes at least one of copper ashes, nickel slag, fuming slag.
3. a kind of method for leaching iron in recycling material containing fayalite using mechanical ball mill according to claim 2, Be characterized in that: the material containing fayalite takes minus sieve material by being crushed, crossing 100~300 meshes.
4. a kind of method for leaching iron in recycling material containing fayalite using mechanical ball mill according to claim 1, Be characterized in that: rotational speed of ball-mill is 450~550r/min, and Ball-milling Time is 3.5~4.5h.
5. a kind of method for leaching iron in recycling material containing fayalite using mechanical ball mill according to claim 1, Be characterized in that: the magnetic field strength that the magnetic separation separation uses is 1.0~1.6 ten thousand Gauss.
6. a kind of method for leaching iron in recycling material containing fayalite using mechanical ball mill according to claim 5, Be characterized in that: the magnetic field strength that the magnetic separation separation uses is 1.1~1.3 ten thousand Gauss.
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