CN107739816A - A kind of method that pyrite cinder prepares iron powder - Google Patents

A kind of method that pyrite cinder prepares iron powder Download PDF

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Publication number
CN107739816A
CN107739816A CN201710971102.1A CN201710971102A CN107739816A CN 107739816 A CN107739816 A CN 107739816A CN 201710971102 A CN201710971102 A CN 201710971102A CN 107739816 A CN107739816 A CN 107739816A
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CN
China
Prior art keywords
iron powder
pyrite cinder
prepares iron
powder
prepares
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710971102.1A
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Chinese (zh)
Inventor
刘娟
王东生
韩可喜
李凯茂
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Application filed by Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd filed Critical Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
Priority to CN201710971102.1A priority Critical patent/CN107739816A/en
Publication of CN107739816A publication Critical patent/CN107739816A/en
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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • 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
    • C22B5/10Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents

Abstract

The invention belongs to iron powder preparation field, and in particular to a kind of method that pyrite cinder prepares iron powder.The technical problems to be solved by the invention are to provide a kind of method that pyrite cinder prepares iron powder.This method comprises the following steps:A, in 1100~1200 DEG C of roastings under nitrogen or inert atmosphere after pyrite cinder and reducing agent being mixed;B, roasting terminates to be cooled to room temperature under rear vacuum or inert atmosphere, then grinding, magnetic separation.The iron powder function admirable that the inventive method is prepared, disclosure satisfy that the requirement of sulfate process titanium dioxide production iron powder.

Description

A kind of method that pyrite cinder prepares iron powder
Technical field
The present invention relates to the technology that a kind of pyrite cinder prepares reduction iron powder, the iron powder is especially suitable for sulfate process titanium dioxide Increase titanium white whiteness in production process.
Background technology
China is sulfuric acid big country, and sulphurite and other Sulfur reserves are few, and gas washing in SA production raw material is with natural resources Dilution and exhausted and environmental consciousness gradual reinforcement, the comprehensive utilization of pyrite cinder receives to be paid attention to and achieves well extensively Achievement, overseas utilization rate have typically all reached 80%, and Countries are even up to 100%.Research of the China to pyrite cinder is begun In in the 1960s, still China's pyrite cinder physicochemical property and complicated, utilization rate only has 30% or so.At present, sulphur Sour slag is mainly used as helping flux, brickmaking, producing iron oxide pigment, prepare ferrous sulfate, prepare polyaluminum sulfate for manufacture of cement Iron, prepare sponge iron, recovery noble metal, production Iron concentrate etc..It is limited sulfate slag dosage to be more or less present in above method, in slag The shortcomings of noble metal added value is low, complex process, energy consumption are big, sulfate slag treatment effect is bad.
The first step of sulfate process titanium dioxide production is that ilmenite and sulfuric acid carried out into acidolysis reaction, that is, by ilmenite and sulphur Acid reaction, the titanium in mineral is transformed into the sulfate of solubility, so that same other impurities separate.The solid matter warp generated Cross after water logging washes, become sulfur acid oxygen titanium, ferrous sulfate and a large amount of Fe3+, the solution (i.e. acidolysis titanium liquid) of impurity, in production process A certain amount of iron is must be added to, by Fe3+Become separable Fe2+And remove.If these Fe are not removed3+Impurity and direct hydrolysis, Titanium dioxide product best in quality cannot be obtained.Typically using iron sheet (or laminar iron filings) as reduction in traditional handicraft Agent.Due to its variable thickness, impurity and greasy dirt content are larger, and DTPA-Fe is low, have a strong impact on normal production and titanium white silty Amount, non-ferrous metal impurity particularly therein can influence the colourity of product.And in practical operation in use, adding difficult, meter Amount is inaccurate, ultimately results in the qualification rate of acidolysis titanium liquid and reduces.And replace iron sheet to make Producing Titanium Dioxide reducing agent with iron powder, have anti- Should fully, the recovery time is short, consumption is less and the advantages that good product quality, substantially increase the stability of titanium dioxide product quality.
Therefore, the present invention proposes a kind of method that new pyrite cinder prepares iron powder, and this method production procedure is short, technique It is easily achieved, gained iron powder uses in sulfate process titanium dioxide production process as reducing agent has preferable applicability, is sulfuric acid A new approach is opened up in the utilization of slag.
The content of the invention
For the problem of remaining solid thing pyrite cinder is not used effectively caused by gas washing in SA production factory, the invention provides A kind of method that pyrite cinder prepares iron powder, iron powder function admirable obtained by this method, disclosure satisfy that sulfate process titanium dioxide production iron The requirement of powder.
The technical problems to be solved by the invention are to provide a kind of method that pyrite cinder prepares iron powder.This method include with Lower step:
A, in 1100~1200 DEG C of roastings under nitrogen or inert atmosphere after pyrite cinder and reducing agent being mixed;
B, roasting terminates to be cooled to room temperature under rear vacuum or inert atmosphere, then grinding, magnetic separation.
Preferably, above-mentioned pyrite cinder is prepared in the method and step a of iron powder, and the reducing agent is coke powder.
Further, above-mentioned pyrite cinder is prepared in the method and step a of iron powder, the fixation carbon content of the coke powder for 85~ 90%.
Preferably, above-mentioned pyrite cinder is prepared in the method and step a of iron powder, and the granularity of the coke powder is -200 mesh.
Preferably, above-mentioned pyrite cinder is prepared in the method and step a of iron powder, and the mass ratio of the pyrite cinder and coke powder is 1 ︰ 1.2.
Specifically, above-mentioned pyrite cinder is prepared in the method and step a of iron powder, the roasting time is 1.5~2h.
Preferably, above-mentioned pyrite cinder is prepared in the method and step a of iron powder, and the flow velocity of the inert gas is 10~15m/ s。
Preferably, above-mentioned pyrite cinder is prepared in the method and step b of iron powder, and the granularity that is ground to is in -200 mesh.
Preferably, above-mentioned pyrite cinder is prepared in the method and step b of iron powder, metal Ferrum content in iron powder obtained by the magnetic separation 70~75%.
Specifically, above-mentioned pyrite cinder is prepared in the method and step b of iron powder, the magnetic separation is using periodic dry type for height Gradient magnetic separator.
Further, above-mentioned pyrite cinder is prepared in the method and step b of iron powder, and the condition of the magnetic separator is:Excitatory electricity Stream is set as that 1600A, excitation voltage are set as 25V, magnetic field intensity 1.5T, the control of rectifier cooling water pressure 0.05~ 0.15Mpa, leaving water temperature are controlled below 50~60 DEG C.
The inventive method is set using pyrite cinder as raw material by rational technique, simple to operate, safe and pollution-free, energy Consume low, and be finally obtained iron powder of the metal Ferrum content more than 75%.The iron powder can be in sulfate process titanium dioxide production process Being used as reducing agent has preferable applicability, meets the requirement to iron powder in sulfuric acid Producing Titanium Dioxide.
Embodiment
A kind of method that pyrite cinder prepares iron powder, comprises the following steps:
A, pyrite cinder and reducing agent are mixed after 1.5~2h of roasting under 1100~1200 DEG C of nitrogen or inert atmosphere;
B, in order to prevent the iron that restores from by secondary oxidation, terminating to be cooled to room temperature under rear vacuum or inert atmosphere;
C, in order to ensure good magnetic separation effect, the material after roasting is ground to 200 eye mesh screens can be crossed, then made Magnetic separation is carried out with magnetic separator, gained iron powder containing metal iron amount is 70-75%.
Reducing agent is iron oxide therein is reduced into metallic iron in the inventive method.Conventional reduction agent.Due to Jiao Powder Particle Size is thin, can accelerate reaction speed, and fixed carbon content is high, and reducing activity is good, and preferably coke powder is as reducing agent.In order to Ash content or volatile matter are as low as possible in coke powder, reduce the influence to product of the present invention, the fixation carbon content of the coke powder for 85~ 90% or so, granularity was the screenings of 200 eye mesh screens.Pyrite cinder of the present invention refers to Raw material, produce the slag discharged in sulfuric acid process, including a small amount of dust or dirt mud.Its main component is Fe2O3And TFe, content point Wei 70% or so and 50% or so.More than the mesh of granularity+200 about 30%.
In the inventive method, it is weight ratio not make specified otherwise, the content, ratio etc..
Embodiment 1
The coke powder that fixed carbon content is 85% or so is subjected to sizing, 200 mesh screenings is crossed and is used as reducing agent.Weigh Quality is 75g pyrite cinder, is in mass ratio 1:1.2 ratio is mixed into coke powder, and both are well mixed.By pyrite cinder and Coke powder mixture is added in crucible, and crucible is placed under 1100 DEG C of nitrogen protection atmospheres in Muffle furnace, nitrogen flow rate 10m/ S, it is calcined 2 hours under the high temperature conditions.Product takes out from Muffle furnace after roasting, baffle plate is covered in crucible surface, for completely cutting off Air, prevent to aoxidize, and be air-cooled to room temperature.Product after air cooling is ground, after grinding material particle size 200 mesh with Under.Levigate product of roasting is put into periodic dry type vibratory high-gradient magnetic separator and carries out magnetic separation, exciting curent is set as 1600A, excitation voltage are set as 25V, magnetic field intensity 1.5T, and rectifier cooling water pressure is controlled in 0.05~0.15Mpa, water outlet Temperature control is below 60 DEG C.Metal Ferrum content is 75% or so in reduced iron powder after magnetic separation, available for sulfate process titanium dioxide It is used as reduced iron powder in production.
Embodiment 2
The coke powder that fixed carbon content is 85% or so is subjected to sizing, 200 mesh screenings is crossed and is used as reducing agent.Weigh Quality is 75g pyrite cinder, is in mass ratio 1:1.2 ratio is mixed into coke powder, and both are well mixed.By pyrite cinder and Coke powder mixture is added in crucible, and crucible is placed under 1200 DEG C of nitrogen protection atmospheres in Muffle furnace.Nitrogen flow rate is 10m/ S, it is calcined 1.5 hours under the high temperature conditions.Product is taken out from Muffle furnace after roasting, and baffle plate is covered in crucible surface, for every Exhausted air, prevent to aoxidize, and be air-cooled to room temperature.Product after air cooling is ground, after grinding material particle size 200 mesh with Under.Levigate product of roasting is put into periodic dry type vibratory high-gradient magnetic separator and carries out magnetic separation, exciting curent is set as 1600A, excitation voltage are set as 25V, magnetic field intensity 1.5T, and rectifier cooling water pressure is controlled in 0.05~0.15Mpa, water outlet Temperature control is below 60 DEG C.Metal Ferrum content is 79% or so in reduced iron powder after magnetic separation, available for sulfate process titanium dioxide It is used as reduced iron powder in production.

Claims (9)

1. the method that pyrite cinder prepares iron powder, it is characterised in that:Comprise the following steps:
A, in 1100~1200 DEG C of roastings under nitrogen or inert atmosphere after pyrite cinder and reducing agent being mixed;
B, roasting terminates to be cooled to room temperature under rear vacuum or inert atmosphere, then grinding, magnetic separation.
2. the method that pyrite cinder according to claim 1 prepares iron powder, it is characterised in that:In step a, the reducing agent For coke powder;The fixation carbon content of the coke powder is 85~90%;The granularity of the coke powder is -200 mesh.
3. the method that pyrite cinder according to claim 2 prepares iron powder, it is characterised in that:In step a, the sulfuric acid burns The mass ratio of slag and coke powder is 1 ︰ 1.2.
4. the method that pyrite cinder according to claim 1 prepares iron powder, it is characterised in that:In step a, during the roasting Between be 1.5~2h.
5. the method that pyrite cinder according to claim 1 prepares iron powder, it is characterised in that:In step a, the indifferent gas The flow velocity of body is 10~15m/s.
6. the method that pyrite cinder according to claim 1 prepares iron powder, it is characterised in that:It is described to be ground in step b Granularity is in -200 mesh.
7. the method that pyrite cinder according to claim 1 prepares iron powder, it is characterised in that:In step b, the magnetic separation institute In iron powder metal Ferrum content 70~75%.
8. the method that pyrite cinder according to claim 1 prepares iron powder, it is characterised in that:In step b, the magnetic separation is adopted High gradient magnetic separator is directed to periodic dry type.
9. the method that pyrite cinder according to claim 8 prepares iron powder, it is characterised in that:In step b, the magnetic separator Condition be:Exciting curent is set as that 1600A, excitation voltage are set as 25V, magnetic field intensity 1.5T, rectifier cooling water pressure Control is controlled at 50~60 DEG C in 0.05~0.15Mpa, leaving water temperature.
CN201710971102.1A 2017-10-18 2017-10-18 A kind of method that pyrite cinder prepares iron powder Pending CN107739816A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424875A (en) * 2011-12-31 2012-04-25 湖南有色金属研究院 Method for preparing sponge iron from sulfate cinder
CN103746115A (en) * 2013-12-13 2014-04-23 灵宝金源矿业股份有限公司 Method for preparing cell-grade lithium iron phosphate from pyrite slag
CN105907948A (en) * 2016-06-27 2016-08-31 东北大学 Magnetic separation method for low-grade chromium-containing vanadium titanium magnetite metalized pellet
CN106319127A (en) * 2016-09-30 2017-01-11 江西理工大学 Method for producing directly reduced ion and titanium nitride by using vanadium titano-magnetite concentrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424875A (en) * 2011-12-31 2012-04-25 湖南有色金属研究院 Method for preparing sponge iron from sulfate cinder
CN103746115A (en) * 2013-12-13 2014-04-23 灵宝金源矿业股份有限公司 Method for preparing cell-grade lithium iron phosphate from pyrite slag
CN105907948A (en) * 2016-06-27 2016-08-31 东北大学 Magnetic separation method for low-grade chromium-containing vanadium titanium magnetite metalized pellet
CN106319127A (en) * 2016-09-30 2017-01-11 江西理工大学 Method for producing directly reduced ion and titanium nitride by using vanadium titano-magnetite concentrate

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Application publication date: 20180227

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