CN108842056A - A kind of oolitic hematite quickly heats the method that reduction prepares reduced iron powder - Google Patents

A kind of oolitic hematite quickly heats the method that reduction prepares reduced iron powder Download PDF

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CN108842056A
CN108842056A CN201811041529.2A CN201811041529A CN108842056A CN 108842056 A CN108842056 A CN 108842056A CN 201811041529 A CN201811041529 A CN 201811041529A CN 108842056 A CN108842056 A CN 108842056A
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iron powder
pelletizing
agent
reduction
reaction
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CN108842056B (en
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雷鹰
何思奇
王雪松
陈雯
李�雨
何文浩
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Anhui University of Technology AHUT
Changsha Research Institute of Mining and Metallurgy Co Ltd
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Anhui University of Technology AHUT
Changsha Research Institute of Mining and Metallurgy Co Ltd
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    • 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
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24Binding; Briquetting ; Granulating
    • C22B1/2406Binding; Briquetting ; Granulating pelletizing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/008Organic compounds containing oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/06Depressants

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention discloses a kind of oolitic hematites quickly to heat the method that reduction prepares reduced iron powder, belongs to direct reduction processes of Iron ores field.The present invention is first by iron ore fine grinding, pelletizing after being mixed with a certain amount of reducing agent, rush reducing agent and Dephosphorising agent, dry green-ball is placed in microwave reaction cavity by means of crucible, first it is warming up to 700 DEG C, then 10 minutes are kept the temperature, continues thereafter with and is kept the temperature after being warming up to 1150 DEG C~1300 DEG C, carry out 10~15min of microwave reaction, regulating system power after reaction, make pelletizing with etc. 5~8 DEG C/min of rates carry out cooling down;It is ground after reaction pelletizing is taken out, the powder that grinding obtains is oriented capture, flotation to get the metallic iron powder for arriving high-purity.By using technical solution of the present invention, the mill after capable of producing the reduction of purity is high selects product, and device therefor and easy to operate, expends that the time is shorter, and energy consumption of reaction is low, and environmental pollution is small, at low cost, high-efficient.

Description

A kind of oolitic hematite quickly heats the method that reduction prepares reduced iron powder
Technical field
The invention belongs to direct reduction processes of Iron ores field more particularly to a kind of utilization microwave direct-reduction Gao Lin Caviar shape are red The iron smelting method of iron ore.
Background technique
In recent years, China's steel and iron industry develops rapidly, and iron ore demand is caused rapidly to increase.Due to the high-quality iron ore in China Scarcity of resources, Refractory iron ore stone utilization rate are low and domestic iron ore manufacturing enterprise production capacity is insufficient, cause domestic iron ore Serious supply falls short of demand state is presented in market.Domestic majority large iron and steel enterprises are had to give a long price for Australia, Brazil, print The iron ore of Du Deng state.For China's imported Fe ore in 2010 up to 6.19 hundred million t, external dependence degree is up to 62.5%.China in 2010 Imported Fe ore is to 128.4 dollars/t of bank average price, and compared with 2009 year-on-years rise 60.6%, imported Fe ore total amount is up to 794.27 hundred million dollars, increased by 58.39% compared with 2009.Iron ore spot price was once breaking through 190 dollars/t, imported iron ore within 2011 Stone substantial appreciation of prices, this not only causes to seriously affect to China's steel industry, also constitutes to the healthy and sustainable development of national economy Grave danger.Thus reinforce the Efficient Development research on utilization of China's Refractory iron ore stone, the degree of self-sufficiency for improving iron ore has Significance.
In the above context, some to think that exploit the opposite lean ore utilized and reluctant iron ore had originally The value of development and utilization, wherein Gao Lin Caviar shape bloodstone is exactly one and typical represents.But Gao Lin Caviar shape is red for a long time Iron ore is always because be difficult to sort and phosphorus grade therein is difficult to decrease and cannot develop and use well.Currently, existing Gao Lin Caviar shape bloodstone all carries out small-scale production using high-temperature heating mostly in technology, although can also reach preferable technology Index, but due to above method low output, energy consumption is higher, it is seriously polluted, forbidden in plain text by many countries, and conventional Beneficiation method is helpless to this kind of sample ore.Therefore, how economical, effectively realize iron-phosphorus separation, improve available iron product Position is the key problem for realizing oolitic hematite comprehensive utilization.Around this proposition, the country has had researcher to do greatly In-depth study is measured, it is several that these research work are concentrated mainly on floatation, wet-leaching method, directly/drastic reduction-separating method etc. A aspect.
Wherein, floatation refers to by selecting suitable collecting agent, inhibitor the reverse flotation separation for realizing part phosphorus, but Since iron mineral disseminated grain size is superfine in oolitic hematite, and with the close symbiosis of phosphorus ore containing and easy argillization etc., using physics The problems such as generally existing concentrate Iron grade of floatation is low, yield is low, phosphorus removal effect is poor.Wet-leaching method be using inorganic acid/ The aqueous solutions of organic acids that the aqueous solution of alkali or microbial metabolism generate enters moieties dissolution in material as leaching agent In solution, the dephosphorization technology of valuable mineral component phosphorus content reduction after separation of solid and liquid.It can be obtained using wet-leaching higher Dephosphorization rate, but its there are reagent consumptions the problems such as big, waste liquid is difficult to recycles, environmental pollution is serious, leaching cycle is long.
Directly/drastic reduction-separating method refers at a certain temperature, and bloodstone is reduced into metallic iron using reducing agent, also Dephosphorising agent is added during former to separate to control the trend and distribution of phosphorus, then by magnetic separation, is realized the removing of phosphorus, is obtained reduced iron Powder or the pig iron.Zhu Deqing etc. exists《The enrichment behavioral study of iron and phosphorus in high-phosphor oolitic hematite reduction roasting-magnetic separation》In with Na2CO3And Na2SO4For Dephosphorising agent, high-phosphor oolitic hematite high temperature had studied at 1350 DEG C quickly restore and obtain high-purity iron powder, Obtain the iron ore concentrate of Iron grade 94.06%, phosphorus content 0.25%, whole process iron recovery 91.37%, dephosphorization rate 91.79%; Yan Fangxing etc. exists《High-phosphor oolitic hematite direct-reduction-magnetic separation experimental study》In using No. 1 Dephosphorising agent as additive, at 1100 DEG C Under have studied the coal base reduction magnetic separation of oolitic hematite and mention iron dephosphorization, recovery time 9h obtains metallic iron Iron grade 84.56%, Iron recovery is 87%, phosphorus content 0.056%.But in above-mentioned existing research using reduction-separating method to oolitic hematite into When row processing, the separating effect of iron and phosphorus is not still very well that when reduction temperature is excessively high, phosphorus is easy to be again introduced into shape in iron crystal grain At interphase.
Han Yue new issue group carries out somewhere high-phosphor oolitic hematite using drastic reduction technology at 1270~1370 DEG C Research, obtains the reducing material of degree of metalization 95~97%, up to 85~88.24%, iron recovery reaches concentrate grade after magnetic separation 92% or more, and the trend of phosphorus is analyzed;But in the research process, the reaction time is too long, dephosphorization in reaction process Effect it is unstable.Zhou Jicheng etc. handles high-phosphor oolitic hematite using drastic reduction technology, has studied reduction temperature, slag phase Basicity, interior carbon ratio of matching are to the rate of recovery of iron and the influence of dephosphorization rate;But the experiment flow is longer, phosphorus and iron during reduction reaction Separating effect be not highly desirable.
The above result of study shows that existing direct/drastic reduction-separating method is imitated in product Iron grade, the rate of recovery and dephosphorization Be better than reverse flotation and wet-leaching technique in terms of rate, but its there are Dephosphorising agent consumptions big (15%wt, even higher) no Foot, while higher reduction temperature also results in that phosphorus ore containing is reduced, part phosphorus is entered in reduced iron with simple substance form, thus Dephosphorization effect is caused to be affected.Therefore it is necessary to try to explore new while continuing to reinforce existing Process ba- sis research Iron-phosphorus separation to the technique that obtains high-purity iron powder.
Summary of the invention
1. technical problems to be solved by the inivention
It is an object of the invention to improve oolitic hematite to carry out the method that reduction prepares reduced iron powder, a kind of roe is provided Shape bloodstone quickly heats the method that reduction prepares reduced iron powder.By using technical solution of the present invention, purity can be produced Mill after high reduction selects product, and device therefor and easy to operate, expends that the time is shorter, and energy consumption of reaction is low, environmental pollution It is small, it is at low cost, it is high-efficient.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention is:
A kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, includes the following steps:
Step 1: pelletizing is prepared
Iron ore adds reductive coke agent, Dephosphorising agent thereto after broken, fine grinding and promotees reducing agent, by all raw materials one It rises and grind and pelletizing drying after mixing, while adding a certain amount of calcium oxide thereto to control basicity and being 0.4~1.2;
Step 2: microwave segmentally heating restores
Dry green-ball is placed in microwave reaction cavity by means of crucible, 700 DEG C is first warming up to, then keeps the temperature 10 minutes, It continues thereafter with and is kept the temperature after being warming up to 1150 DEG C~1300 DEG C, carry out 10~15min of microwave reaction, adjust system after reaction Unite power, make pelletizing with etc. 5~8 DEG C/min of rates carry out cooling down;
Step 3: broken apart flotation
It is ground after reaction pelletizing is taken out, it is high-purity to get arriving that the powder that grinding obtains is oriented capture, flotation The metallic iron powder of degree.
Further, the Dephosphorising agent is any one of sodium carbonate, sodium sulphate, calcium hydroxide and calcium chloride, Additive amount accounts for the 2.5%~7.5% of pelletizing total amount.
Further, the additive amount of the reducing agent is to react the desired amount of 1.4~1.6 times, the rush reducing agent For iron powder, additive amount is the 4%~5% of ground hematite content.
Further, after dry green-ball being placed in crucible, crucible, Zhi Houzai are filled with the coke grain of even particle size It is placed in microwave reaction cavity.
Further, the temperature that microwave reaction is controlled in step 2 is 1250 DEG C, reaction time 10min.
Further, the powder that grinding obtains is placed in aqueous solution in step 3 and is stirred, adjusting pH value is 10~12, Then certain inhibitor, activator and agent for capturing are added thereto, and carry out flotation.
Further, the inhibitor uses cassava ative starch, content 60mg/L, and activator uses Ca ion Activator, content 100mg/L, agent for capturing use enuatrol.
Further, in the pelletizing of the step 1 various additives be at least ground to before pelletizing 200 mesh with Under.
3. beneficial effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result:
(1) a kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, by by iron ore Pelletizing processing is carried out after grinding together with certain reducing agent, Dephosphorising agent and rush reducing agent, and places it in microwave and is added Thermal reduction, while the temperature and time of microwave heating is optimized, so as to effectively improve rate of reduction and reduction Efficiency, and be conducive to the separation of Fe and P, while invention also reduces the reduction temperature of ferriferous oxide, it can effectively avoid also Fe after original is at high temperature with P in conjunction with being further ensured that the separating effect of Fe and P.
(2) a kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, passes through Dephosphorising agent The P elements being added in , Shi Caviar shape structure can be detached under microwave condition with ferro element, form phosphate, be convenient for subsequent experimental It is separated in step with ferro element;And the addition by promoting reducing agent then can provide forming core core in reduction process, Neng Gouming It is aobvious to promote reaction rate, reduction process is rapidly completed.
(3) a kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, by Dephosphorising agent It is optimized with the additive amount of reducing agent and the basicity of pelletizing, to be conducive to be further ensured that the abundant of iron in pelletizing The full Iron grade of reduction, final gained reduced iron powder is greater than 90%, and improves the separating effect of Fe and P.
(4) a kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, and microwave heating is not to Commaterial has the distinguishing feature selectively heated, and ten subcontracts close the characteristic of Caviar shape bloodstone, so as to so that mineral facies are preferential It is heated, substance to be restored is rapidly heated reaction, and the phosphorus content that can be effectively reduced in bloodstone, improve iron in mineral facies Reduction rate guarantees the Iron grade of gained reduced iron powder product.
(5) a kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, by adding to microwave The technique of heat optimizes, and is first warming up to 700 DEG C, then keeps the temperature 10 minutes, continues thereafter with and be warming up to 1150 DEG C~1300 Kept the temperature after DEG C, carry out 10~15min of microwave reaction, regulating system power after reaction, make pelletizing with etc. rates 5~8 DEG C/min progress cooling down, so that the abundant reduction of iron in mineral facies on the one hand can be promoted, and advantageously reduce reduction temperature Degree improves rate of reduction, on the other hand Fe/P phase interface can be promoted sufficiently to dissociate, and is conducive to the removal effect for further increasing P Fruit, realization reduced iron powder product and slag are sufficiently separated.
(6) a kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, reacts pelletizing through grinding Capture, flotation are oriented after mill, the pH value by treating flotation fluid carries out strict control, and adds cassava ative starch thereto As inhibitor, while certain Ca ion activation agent is added, thereby may be ensured that and effectively inhibit bloodstone and quartz in style It reacts, and is conducive to the separating-purifying of Fe.
Detailed description of the invention
Fig. 1 is the XRD diagram that oolitic hematite microwave reduction prepares reduced iron powder in the present invention;
Fig. 2 and Fig. 3 is respectively SEM figure of this Fa Ming Zhong Caviar shape hematite powder under different amplification.
Specific embodiment
A kind of oolitic hematite of the invention quickly heats the method that reduction prepares reduced iron powder, includes the following steps:
Step 1: pelletizing is prepared
Iron ore (is at least ground to 200 mesh hereinafter, can destroy iron ore as far as possible in this way in shattering process through broken Caviar shape structure in stone, while increasing relative interface area between reactant promotes reaction rate to increase), after fine grinding thereto Adding reductive coke agent, Dephosphorising agent and rush reducing agent, (various additives are ground to 200 mesh hereinafter, can mix so in advance Shi Jinliang is uniform, so that mutual contact surface is bigger at high temperature, reacts rapider), wherein Dephosphorising agent is sodium carbonate, sulfuric acid Any one of sodium, calcium hydroxide and calcium chloride, additive amount account for the 2.5%~7.5% of pelletizing total amount, the addition of reducing agent Amount for react it is the desired amount of 1.4~1.6 times, the rush reducing agent be iron powder, additive amount be ground hematite content 4%~ 5%.All raw materials are carried out to grind together and pelletizing is dried after mixing, while also adding a certain amount of calcium oxide in pelletizing To control basicity as 0.4~1.2.
The present invention under microwave condition can by adding the P elements in certain Dephosphorising agent , Shi Caviar shape structure into pelletizing Enough and ferro element is detached from, and phosphate is formed, convenient for separating in subsequent experimental procedure with ferro element;And the addition by promoting reducing agent Forming core core can be then provided in reduction process, reaction rate can be obviously promoted, reduction process is rapidly completed.Wherein take off The basicity of the additive amount and pelletizing of phosphorus agent and reducing agent is affected to the reduction rate and Fe, P separating effect of pelletizing, inventor The basicity of pelletizing and the additive amount of Dephosphorising agent are optimized by experimental study, so as to prepare high metal While rate iron powder, from the phosphorus content largely reduced in iron, efficiently separating for Fe and P is realized.In addition, as dephosphorization Sodium carbonate that agent is added etc. can also play the role of binder in the balling stage of mixed material simultaneously, and balling stage does not need separately Outer addition binder, saves production cost.
Step 2: microwave segmentally heating restores
Dry green-ball is placed in heat-resisting crucible, crucible is filled with the coke grain of even particle size, is placed in again later micro- In wave reaction cavity, so that it is guaranteed that pelletizing can be good at the microwave of absorption equipment generation during the reaction, make in crucible Temperature rapid increase, to achieve the purpose that rapid reduction of carbonaceous pelletizing.Heating cycle is set, is first warming up to 700 DEG C, then protects Temperature 10 minutes continues thereafter with and is warming up to 1150 DEG C~1300 DEG C, and adjusting electric current remains unchanged temperature, carries out at this temperature micro- Wave reacts 10~15min, it is furthermore preferred that the temperature of control microwave reaction is 1250 DEG C, reaction time 10min, reaction terminates Regulating system power afterwards, make pelletizing with etc. 5~8 DEG C/min of rates carry out cooling down.
Inventor passes through lot of experiments, final choice microwave reduction mode, since there is microwave selectivity to add The distinguishing feature of heat, energy conversion regime in situ makes material microcell obtain quick energy accumulation, so that in oolitic hematite Valuable mineral be preferentially heated, cause uneven distribution of the complex ore system temperature on micro- ruler.Microwave selective adds Thermogenetic thermal stress to generate a large amount of gap and crackle inside pelletizing.The coupled resonance of oolitic hematite and microwave is formed Hot spot is reacted, quickly reduction forms a large amount of iron nucleus, accelerates the reduction of ferriferous oxide, is macroscopically showing to reduce reduction temperature Degree accelerates reduction reaction rate, strengthens the reduction of metalliferous mineral in inclusion enclave, improves degree of metalization;It is shown on microcosmic Two-phase interface forms crack and fragment, promotes ore phase reconstruction, inclusion enclave is promoted to dissociate.
Specifically, Fe reduction rate is fast using technical solution of the present invention, it is high-efficient, while microwave heating also reduces The reduction temperature of ferriferous oxide, the Fe after capable of effectively avoiding reduction is at high temperature with P in conjunction with to make Fe, P separating effect It is further ensured that.In addition, the present invention selects microwave heating to also help ore phase reconstruction, and improve the metal of reduzate Rate, entire method discharge exhaust gas is few, and consumption quantity of energy is low, and reaction process is short, be very suitable for difficult Caviar shape bloodstone. It should also be noted that, the concrete technology of microwave heating has larger impact for the reduction rate and Fe, P separating effect of Fe, Inventor optimizes microwave heating process by many experiments, by selecting reasonable temperature schedule, thus a side Face can promote the abundant reduction of iron in mineral facies, and advantageously reduce reduction temperature, improve rate of reduction, on the other hand can be with Promote Fe/P phase interface sufficiently to dissociate, be conducive to the removal effect for further increasing P, realizes the abundant of reduced iron powder product and slag Separation.In addition, being kept the temperature by first rising to 700 DEG C, it is ensured that pelletizing integrally reaches the reaction temperature of preheating, is convenient for subsequent heat preservation In the process, the selectivity heating energy homogeneous reaction of wave substance is inhaled in pelletizing, and after reaction by controlling reasonable cooler System refines crystal grain, adjusts tissue, eliminate tissue defects to make to restore style reduction deformation and crackle tendency.
Step 3: broken apart flotation
200~300 mesh are ground to after reaction pelletizing is taken out, the powder that grinding obtains are oriented capture, flotation, i.e., Obtain the metallic iron powder of high-purity.It is stirred specifically, first the powder that grinding obtains is placed in aqueous solution, adjusting pH value is 10 ~12, then according to volumetric concentration 60mg/L addition cassava ative starch as inhibitor, so as to inhibit red in style very well Iron ore and quartz react, and make quartzy work according still further to volumetric concentration 100mg/L addition Ca ion activation agent after addition inhibitor Change.Activation process is by CaO or Ca2+Ca (OH) is formed after being dissolved in water2, then Ca (OH)2It hydrolyzes in water, ionize life At Ca (OH)+Quartz surfaces are adsorbed on, and make collecting agent that chemisorption further occur in quartz surfaces by means of this absorption.Add Add and continue to add enuatrol after activator as agent for capturing, oleic acid root easily with the Ca (OH) that is adsorbed on quartz surfaces+It has an effect, Make quartz surfaces hydrophobization, realizes the floating of quartz.
To further appreciate that the contents of the present invention, now in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The Iron grade of certain Gao Lin Caviar shape hematite is 43.5%, and phosphorus content is bloodstone in 0.85% , Caviar shape bloodstone Granularity is superfine, and often mutually wraps up with eel chlorite and phosphorus ore containing such as collophane or symbiosis, is difficult useless using iron ore solid Object blast furnace ash iron content, ferriferous oxide is mainly based on bloodstone.The condition of Wei Bo Jia Re Caviar shape bloodstone is:Iron ore 100g, 1.5 times of reductive coke agent about 21g, mass fraction account for the sodium carbonate of pelletizing gross weight 2.5%, the rush of ground hematite content 4% Reducing agent iron powder, basicity 0.4.700 DEG C are first warming up to, then 10 minutes is kept the temperature, continues thereafter with and kept the temperature after being warming up to 1250 DEG C 10min, then with the cooling 4h of 5 DEG C/min after, obtain reduzate.Material is milled to 200 mesh on crusher for preparing specimens, powder is set It is stirred in aqueous solution, adjusting pH value is 10, then sequentially adds cassava ative starch, the agent of Ca ion activation and enuatrol agent for capturing It is oriented capture, flotation, obtains the iron powder that degree of metalization is 93.77%.The present embodiment restore to obtain the XRD spectrum of iron powder and Scanned picture is as shown in Figure 1-Figure 3, and as seen from the figure, iron content is high in the product obtained by this method, without other Significantly it is attached to product and impurity, purity is high.
Embodiment 2
The Iron grade of certain Gao Lin Caviar shape hematite is 43.5%, and phosphorus content is bloodstone in 0.85% , Caviar shape bloodstone Granularity is superfine, and often mutually wraps up with eel green mud stone ore or symbiosis, is difficult to utilize iron ore solid waste blast furnace ash iron content, iron oxygen Compound is mainly based on bloodstone.The condition of Wei Bo Jia Re Caviar shape bloodstone is:Iron ore 100g, 1.5 times of reductive cokes Agent about 21g, mass fraction account for the calcium chloride of pelletizing gross weight 5%, the rush reducing agent iron powder of ground hematite content 5%, basicity 0.4. 700 DEG C are first warming up to, then 10 minutes is kept the temperature, continues thereafter with and keep the temperature 15min after being warming up to 1150 DEG C, then is cooling with 8 DEG C/min After 4h, reduzate is obtained.Material is milled to 200 mesh on crusher for preparing specimens, powder is placed in aqueous solution and is stirred, adjusts PH Value is 12, then sequentially adds cassava ative starch, the agent of Ca ion activation and enuatrol agent for capturing and is oriented capture, flotation, obtains The iron powder for being 96.47% to degree of metalization.
Embodiment 3
The Iron grade of certain Gao Lin Caviar shape hematite is 43.5%, and phosphorus content is bloodstone in 0.85% , Caviar shape bloodstone Granularity is superfine, and often mutually wraps up with phosphorus ore containing such as collophane or symbiosis, is difficult to be contained using iron ore solid waste blast furnace ash Iron, ferriferous oxide is mainly based on bloodstone.The condition of Wei Bo Jia Re Caviar shape bloodstone is:Iron ore 100g, 1.6 times of cokes Charcoal reducing agent, mass fraction account for the calcium hydroxide of pelletizing gross weight 7.5%, the rush reducing agent iron powder of ground hematite content 4.5%, alkali Degree 0.6.700 DEG C are first warming up to, then keeps the temperature 10 minutes, continues thereafter with and keeps the temperature 10min after being warming up to 1300 DEG C again with 7 DEG C/min After cooling 3h, reduzate is obtained.Material is milled to 200 mesh on crusher for preparing specimens, powder is placed in aqueous solution and is stirred, is adjusted Saving pH value is 11, then sequentially adds cassava ative starch, the agent of Ca ion activation and enuatrol agent for capturing and is oriented capture, floats Choosing obtains the iron powder that degree of metalization is 98.91%.
Embodiment 4
The Iron grade of certain Gao Lin Caviar shape hematite is 43.5%, and phosphorus content is bloodstone in 0.85% , Caviar shape bloodstone Granularity is superfine, and often mutually wraps up with eel chlorite and phosphorus ore containing such as collophane or symbiosis, is difficult useless using iron ore solid Object blast furnace ash iron content, ferriferous oxide is mainly based on bloodstone.The condition of Wei Bo Jia Re Caviar shape bloodstone is:Iron ore 100g, 1.4 times of reductive coke agent, mass fraction account for the sodium sulphate of pelletizing gross weight 2.5%, the rush reduction of ground hematite content 5% Agent iron powder, basicity 1.2.700 DEG C are first warming up to, then 10 minutes is kept the temperature, continues thereafter with and keep the temperature 10min after being warming up to 1250 DEG C, After cooling down 5h again with 6 DEG C/min, reduzate is obtained.Material is milled to 200 mesh on crusher for preparing specimens, powder is placed in water-soluble It is stirred in liquid, adjusting pH value is 10, then sequentially adds cassava ative starch, the agent of Ca ion activation and enuatrol agent for capturing and is determined To capture, flotation, the iron powder that degree of metalization is 94.63% is obtained.

Claims (8)

1. a kind of oolitic hematite quickly heats the method that reduction prepares reduced iron powder, which is characterized in that include the following steps:
Step 1: pelletizing is prepared
Iron ore adds reductive coke agent, Dephosphorising agent thereto after broken, fine grinding and promotees reducing agent, by all raw materials together into Row grinding and pelletizing is dried after mixing, at the same add thereto a certain amount of calcium oxide with control basicity for 0.4~ 1.2;
Step 2: microwave segmentally heating restores
Dry green-ball is placed in microwave reaction cavity by means of crucible, 700 DEG C is first warming up to, then keeps the temperature 10 minutes, then It is kept the temperature after being continuously heating to 1150 DEG C~1300 DEG C, carries out 10~15min of microwave reaction, after reaction regulating system function Rate, make pelletizing with etc. 5~8 DEG C/min of rates carry out cooling down;
Step 3: broken apart flotation
Will reaction pelletizing take out after grind, the obtained powder of grinding is oriented capture, flotation to get arriving high-purity Metallic iron powder.
2. a kind of oolitic hematite according to claim 1 quickly heats the method that reduction prepares reduced iron powder, feature It is:The Dephosphorising agent is any one of sodium carbonate, sodium sulphate, calcium hydroxide and calcium chloride, and it is total that additive amount accounts for pelletizing The 2.5%~7.5% of amount.
3. a kind of oolitic hematite according to claim 1 quickly heats the method that reduction prepares reduced iron powder, feature It is:The additive amount of the reducing agent is to react the desired amount of 1.4~1.6 times, and the rush reducing agent is iron powder, additive amount It is the 4%~5% of ground hematite content.
4. a kind of oolitic hematite according to any one of claim 1-3 quickly heats the side that reduction prepares reduced iron powder Method, it is characterised in that:After dry green-ball is placed in crucible, crucible is filled with the coke grain of even particle size, is placed in again later In microwave reaction cavity.
5. a kind of oolitic hematite according to any one of claim 1-3 quickly heats the side that reduction prepares reduced iron powder Method, it is characterised in that:The temperature that microwave reaction is controlled in step 2 is 1250 DEG C, reaction time 10min.
6. a kind of oolitic hematite according to any one of claim 1-3 quickly heats the side that reduction prepares reduced iron powder Method, it is characterised in that:The powder that grinding obtains is placed in aqueous solution in step 3 and is stirred, adjusting pH value is 10~12, then Certain inhibitor, activator and agent for capturing are added thereto, and carry out flotation.
7. a kind of oolitic hematite according to claim 6 quickly heats the method that reduction prepares reduced iron powder, feature It is:The inhibitor uses cassava ative starch, content 60mg/L, and activator uses the agent of Ca ion activation, and content is 100mg/L, agent for capturing use enuatrol.
8. a kind of oolitic hematite according to claim 6 quickly heats the method that reduction prepares reduced iron powder, feature It is:Various additives are at least ground to 200 mesh or less before pelletizing in the pelletizing of the step 1.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110773750A (en) * 2019-12-16 2020-02-11 重庆优钛新材料科技有限公司 Method and device for preparing high-purity superfine metal powder

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1931437A (en) * 2006-10-12 2007-03-21 武汉科技大学 Ore dressing process of oolitic high phosphorus hematite
US20090324440A1 (en) * 2006-03-03 2009-12-31 Anglo Operations Limited Reduction Processing of Metal-Containing Ores in The Presence of Microwave and RF Energy
CN102382920A (en) * 2010-09-02 2012-03-21 辽宁科技大学 Method for decreasing phosphorus of high-phosphorus iron ore by adopting microwave reduction-magnetic separation
CN102978320A (en) * 2012-11-23 2013-03-20 武钢集团昆明钢铁股份有限公司 Method for preparing direct-reduction iron by reducing carbon-containing iron ore powder in microwave heating manner
CN102978318A (en) * 2012-12-12 2013-03-20 北京科技大学 Method for realizing phosphorus removal of oolitic high-phosphorus iron ores by combining enhanced gas-based reduction and high-temperature smelting separation
CN103014212A (en) * 2012-12-21 2013-04-03 北京科技大学 Technical method for producing metal iron powder by using carbon-containing high-phosphorus oolitic hematite pellet
CN103131815A (en) * 2013-03-19 2013-06-05 李学文 Technique for producing spongy iron and nickel iron by microwave high-temperature continuous reduction
CN104099465A (en) * 2014-07-25 2014-10-15 北京科技大学 Method for producing reduced iron power by self-catalysis reduction of high-phosphorus oolitic hematite
CN105969979A (en) * 2016-06-03 2016-09-28 新疆星塔矿业有限公司 Method for treating complex gold concentrate cyanidation tailings through microwave chloridizing roasting and volatilization
CN106498185A (en) * 2016-11-01 2017-03-15 深圳市中启新材料有限公司 A kind of method that vacuum microwave refines magnesium
WO2018014093A1 (en) * 2016-07-21 2018-01-25 Крассимир ИОНКОВ Method for obtaining iron from iron ores containing phosphorus

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090324440A1 (en) * 2006-03-03 2009-12-31 Anglo Operations Limited Reduction Processing of Metal-Containing Ores in The Presence of Microwave and RF Energy
CN1931437A (en) * 2006-10-12 2007-03-21 武汉科技大学 Ore dressing process of oolitic high phosphorus hematite
CN102382920A (en) * 2010-09-02 2012-03-21 辽宁科技大学 Method for decreasing phosphorus of high-phosphorus iron ore by adopting microwave reduction-magnetic separation
CN102978320A (en) * 2012-11-23 2013-03-20 武钢集团昆明钢铁股份有限公司 Method for preparing direct-reduction iron by reducing carbon-containing iron ore powder in microwave heating manner
CN102978318A (en) * 2012-12-12 2013-03-20 北京科技大学 Method for realizing phosphorus removal of oolitic high-phosphorus iron ores by combining enhanced gas-based reduction and high-temperature smelting separation
CN103014212A (en) * 2012-12-21 2013-04-03 北京科技大学 Technical method for producing metal iron powder by using carbon-containing high-phosphorus oolitic hematite pellet
CN103131815A (en) * 2013-03-19 2013-06-05 李学文 Technique for producing spongy iron and nickel iron by microwave high-temperature continuous reduction
CN104099465A (en) * 2014-07-25 2014-10-15 北京科技大学 Method for producing reduced iron power by self-catalysis reduction of high-phosphorus oolitic hematite
CN105969979A (en) * 2016-06-03 2016-09-28 新疆星塔矿业有限公司 Method for treating complex gold concentrate cyanidation tailings through microwave chloridizing roasting and volatilization
WO2018014093A1 (en) * 2016-07-21 2018-01-25 Крассимир ИОНКОВ Method for obtaining iron from iron ores containing phosphorus
CN106498185A (en) * 2016-11-01 2017-03-15 深圳市中启新材料有限公司 A kind of method that vacuum microwave refines magnesium

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110773750A (en) * 2019-12-16 2020-02-11 重庆优钛新材料科技有限公司 Method and device for preparing high-purity superfine metal powder

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