CN107572596A - A kind of high-phosphor oolitic hematite prepares high-purity iron oxide red method - Google Patents
A kind of high-phosphor oolitic hematite prepares high-purity iron oxide red method Download PDFInfo
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- CN107572596A CN107572596A CN201710824640.8A CN201710824640A CN107572596A CN 107572596 A CN107572596 A CN 107572596A CN 201710824640 A CN201710824640 A CN 201710824640A CN 107572596 A CN107572596 A CN 107572596A
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- oolitic hematite
- phosphor oolitic
- iron oxide
- oxide red
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Abstract
High-purity iron oxide red method is prepared the invention discloses a kind of high-phosphor oolitic hematite.High-phosphor oolitic hematite is mixed with coal dust, 90 150min are calcined under conditions of 1,000 1100 DEG C and obtain composite ore, the composite ore ore grinding of acquisition accounts for 90% to 74 μm, magnetic separation obtains magnetic concentrate under the conditions of 0.1 0.15T magnetic field intensity, then by 17% 20% sulfuric acid with the magnetic concentrate that obtains according to volume mass than 9:1‑11:1ml/g is mixed, under conditions of low whipping speed is 100 300r/min, the 35min of normal-temperature reaction 25, and the solidliquid mixture of acquisition；It is 5 5.5 to add ammoniacal liquor and adjust pH, and filtrate is obtained after filtering；The addition of gained filtrate is oxidizing, and adds under conditions of ammoniacal liquor holding pH is 4 and precipitate, filtration washing；Gained sediment is calcined 40 60min at 750 850 DEG C, obtains high-purity mangesium oxide iron oxide red.High-purity mangesium oxide iron oxide red is prepared as using the high-phosphor oolitic hematite being difficult by as raw material, is turned waste into wealth；The too high problem for influenceing to utilize of phosphorus content in processing high-phosphor oolitic hematite；Solves the problems, such as high-phosphor oolitic hematite leaching.
Description
Technical field
The invention belongs to technical field of resource comprehensive utilization, and in particular to a kind of high-phosphor oolitic hematite prepares high pure zirconia
The method of iron oxide red.
Background technology
China's high-phosphor oolitic hematite rich reserves, up to 37.2 hundred million tons.Such iron ore main ferrous mineral is bloodstone,
Next is combined in the form of the silicate such as chamosite with the presence of part iron with sial.Bloodstone is primarily present in roe shape concentric ring
Banded structure, oolith particle diameter are generally 0.01-0.30mm.Bloodstone is more to form concentric zonary structure, roe with chamosite alternating layers
Core is then predominantly quartzy, is secondly bloodstone.Apatite is most important Phosphate minerals in the ore, mainly in irregular embedding cloth
In other gangue mineral gaps or oolitic hematite particulate interspaces, it is seen that apatite exists with oolith core form, it is seen that phosphorus
Lime stone is in the form of roe ring with bloodstone mutually in concentric zonary structure composition oolith；Preceding two parts apatite granularity is thicker, passes through
Appropriate ore grinding can be removed by mechanical beneficiation method, behind two kinds of forms apatite granularity it is all very thin, be generally less than
0.015mm, it is difficult to be will be completely dissociated in grinding process with bloodstone, easily enter in iron ore concentrate.
Phosphorous more steel, in use, easy embrittlement under room temperature or lower temperature.
The method of comprehensive utilization of high-phosphor oolitic hematite mainly has two kinds at present：One kind is with magnetizing roast --- magnetic
Choosing --- dephosphorization is the handling process of core to obtain the relatively low iron ore concentrate of phosphorus content, and one kind is in direct-reduction roast --- magnetic
Dephosphorising agent is added while selecting technique and carries out dephosphorization treatment acquisition reduced iron powder for use as electric furnace smelting.Taken off although with reverse flotation
Phosphorus, acidleach dephosphorization, it is about 0.2% that ultrasonic wave acidleach dephosphorization, which also has the dephosphorization technologies such as Microorganism Leaching to obtain phosphorus content, but iron
The iron ore concentrate that grade is about 60%；Iron concentrate grade is not high first, and dephosphorization is still secondly faced in follow-up processing procedure
Problem.And second of processing mode can obtain the reduced iron powder that phosphorus content is about 0.08%, this reduced iron powder is used for electric furnace smelting
Still it is higher to there is phosphorus content.
High-phosphor oolitic hematite is because of its special oolitic texture, when also having nitric acid leaching using single sulfuric acid, hydrochloric acid not
Higher leaching rate can be obtained, iron leaching rate is less than 40%；The mass fraction of increase acid can improve leaching rate to 60%.It is although high
Phosphorus oolitic hematite can be mixed by a variety of strong acid and leached, and obtain higher leaching rate；But nitration mixture leaches and equipment occurs
Corrosion and a large amount of impurity enter leachate increase cost of equipment maintenance and leachate removal of impurities cost.Direct acidleach after raw ore preenrichment
Have that iron recovery is not high, the problems such as also oolitic texture is to the adverse effect of acidleach.
The content of the invention
The purpose of the present invention is the problem of presence for existing high-phosphor oolitic hematite Resource comprehensive utilization method, explores profit
With the new way of high-phosphor oolitic hematite, there is provided a kind of high-phosphor oolitic hematite prepares high-purity iron oxide red method.
The present invention proposes the method that iron oxide red is prepared using high-phosphor oolitic hematite, utilizes lower temperature（1050 DEG C of left sides
It is right）Direct Reduction Technology change Fe clusters.Collophane meeting decomposed at this temperature, a small number of phosphorus enter iron phase and form Fe/P
Alloy, and the oxide of other phosphorus is then relatively stable；The transfer of phosphorus need not be paid close attention to when then leaching.
The present invention proposes the method that iron oxide red is prepared using high-phosphor oolitic hematite, improves the leaching rate of iron.It is first
Direct-reduction processing changes Fe clusters and causes magnetic concentrate to have good leaching rate in single sulfuric acid leaching, and a large amount of impurity enter
In leached mud；Most of oolitic texture is destroyed simultaneously cracked between iron ore composition granule and gangue mineral all improves leaching
Go out efficiency.More than the 90% iron leaching rate that magnetic concentrate after processing can obtain.
To realize goal of the invention, technical solution of the invention is：A kind of high-phosphor oolitic hematite prepares high pure zirconia
The method of iron oxide red, high-phosphor oolitic hematite is mixed with coal dust, 90-150min is calcined under conditions of 1000-1100 DEG C and is obtained
Composite ore, the composite ore ore grinding of acquisition extremely account for 90% for -74 μm, the magnetic separation acquisition magnetic separation essence under the conditions of 0.1-0.15T magnetic field intensity
Ore deposit, then by 17%-20% sulfuric acid with obtain magnetic concentrate according to volume mass than 9:1-11:1ml/g is mixed, in stirring speed
Spend under conditions of 100-300r/min, normal-temperature reaction time 25-35min, the solidliquid mixture of acquisition；Adding ammoniacal liquor tune pH is
5-5.5, filtrate is obtained after filtering；The addition of gained filtrate is oxidizing, and adds under conditions of ammoniacal liquor holding pH is 4 and precipitate, mistake
Filter washing；Gained sediment is calcined 40-60min at 750-850 DEG C, obtains high-purity mangesium oxide iron oxide red.
Specifically, phosphorus oolitic hematite is with coal dust mixed proportion：100 parts of high-phosphor oolitic hematite, 30 ~ 40 parts of coal dust.
Preferably, 1050 DEG C of the sintering temperature that high-phosphor oolitic hematite mixes with coal dust, roasting time 120min.
Preferably, the mass concentration 18% of sulfuric acid；The volume mass of sulfuric acid and magnetic concentrate is than 10：1ml/g.
Preferably, the mixing normal-temperature reaction time 30min of sulfuric acid and magnetic concentrate.
Preferably, the sediment after oxidation filtering, sintering temperature is 800 DEG C, time 60min.
Specifically, oxidant is hydrogen peroxide.
The beneficial effects of the invention are as follows：The high-phosphor oolitic hematite being difficult by is prepared as high-purity mangesium oxide as raw material
Iron oxide red, turn waste into wealth；The too high problem for influenceing to utilize of phosphorus content in processing high-phosphor oolitic hematite；Solves high-phosphor oolitic hematite
The problem of leaching.
Brief description of the drawings
Fig. 1 is the production technological process of the present invention.
Embodiment
The present invention is described further below in conjunction with the accompanying drawings.
Embodiment 1, comprises the following steps：It is 47.6% by high-phosphor oolitic hematite and fixed carbon that full Iron grade is 42.3%
Coal dust according to Fe and C mass ratio be 2.39:1 mixing, i.e., the ratio between mass fraction of high-phosphor oolitic hematite and coal dust is
100:37；It is placed in furnace for testing room under conditions of 1050 DEG C and is calcined 120min, water cooling after taking-up；Ore after roasting is straight
Connect extremely -74 μm of ore grinding and account for 90%, and using drum magnetic separator magnetic separation under conditions of field strength is 0.12T, obtaining Iron grade is
61.25% magnetic concentrate, main component are fe；It in the ratio of sulfuric acid solution and magnetic concentrate is 10 to take 18% sulfuric acid:
1ml/g hybrid reactions 25min；It is 5 that ammoniacal liquor is added into mixed liquor and adjusts pH, is filtered to get filtrate；Add oxidizing peroxidating
It is 4 that hydrogen simultaneously keeps pH value simultaneously, and filtering, which precipitates, simultaneously washs；Precipitation, which is placed in furnace for testing room under conditions of 750 DEG C, to be calcined
50min is finished product, Fe2O3Content is up to 98.23%.
Embodiment 2, comprises the following steps：It is 47.6% by high-phosphor oolitic hematite and fixed carbon that full Iron grade is 42.3%
Coal dust according to Fe and C mass ratio be 2.7:1 mixing, i.e. the ratio between mass fraction of high-phosphor oolitic hematite and coal dust are 100:
33；It is placed in furnace for testing room under conditions of 1000 DEG C and is calcined 150min, water cooling after taking-up；Ore after roasting is directly ground
Extremely -74 μm of ore deposit accounts for 90%, and using drum magnetic separator magnetic separation under conditions of field strength is 0.12T, it is 60.85% to obtain Iron grade
Magnetic concentrate；It in the ratio of sulfuric acid solution and magnetic concentrate is 11 to take 18% sulfuric acid:1ml/g hybrid reactions 35min；To mixing
It is 5.5 that ammoniacal liquor is added in liquid and adjusts pH, is filtered to get filtrate；Add it is oxidizing and keep simultaneously pH value be 4, filtering precipitate simultaneously washes
Wash；It is finished product that precipitation, which is placed in furnace for testing room under conditions of 800 DEG C and is calcined 60min, Fe2O3Content is up to 99.23%.
Embodiment 3, comprises the following steps：It is 49.6% by high-phosphor oolitic hematite and fixed carbon that full Iron grade is 40.3%
Coal dust according to Fe and C mass ratio be 2.6:1 mixing, the i.e. mass ratio of high-phosphor oolitic hematite and coal dust are 100:31；
It is placed in furnace for testing room under conditions of 1050 DEG C and is calcined 120min, water cooling after taking-up；By the direct ore grinding of ore after roasting
90% is accounted for -74 μm, and using drum magnetic separator magnetic separation under conditions of field strength is 0.10T, obtains the magnetic that Iron grade is 61.85%
Concentrate selection；It in the ratio of sulfuric acid solution and magnetic concentrate is 11 to take 20% sulfuric acid:1ml/g hybrid reactions 30min；To mixed liquor
It is 5.5 that middle addition ammoniacal liquor, which adjusts pH, is filtered to get filtrate；Add it is oxidizing and keep simultaneously pH value be 4, filtering precipitate simultaneously washes
Wash；It is finished product that precipitation, which is placed in furnace for testing room under conditions of 850 DEG C and is calcined 60min, Fe2O3Content is up to 99.36%.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (7)
1. a kind of high-phosphor oolitic hematite prepares high-purity iron oxide red method, high-phosphor oolitic hematite is mixed with coal dust,
90-150min is calcined under conditions of 1000-1100 DEG C and obtains composite ore, the composite ore ore grinding of acquisition extremely accounts for 90% for -74 μm,
Magnetic separation obtains magnetic concentrate under the conditions of 0.1-0.15T magnetic field intensity, it is characterised in that also comprises the following steps：
By 17%-20% sulfuric acid and the magnetic concentrate obtained according to volume mass than 9:1-11:1ml/g is mixed, low whipping speed
Under conditions of 100-300r/min, normal-temperature reaction 25-35min, the solidliquid mixture of acquisition；It is 5-5.5 to add ammoniacal liquor and adjust pH,
Filtrate is obtained after filtering；The addition of gained filtrate is oxidizing, and adds under conditions of ammoniacal liquor holding pH is 4 and precipitate, filtration washing；
Gained sediment is calcined 40-60min at 750-850 DEG C, obtains high-purity mangesium oxide iron oxide red.
2. a kind of high-phosphor oolitic hematite according to claim 1 prepares high-purity iron oxide red method, it is characterised in that
High-phosphor oolitic hematite is with coal dust mixed proportion：100 parts of high-phosphor oolitic hematite, 30 ~ 40 parts of coal dust.
3. a kind of high-phosphor oolitic hematite according to claim 1 prepares high-purity iron oxide red method, it is characterised in that
Preferably 1050 DEG C of the sintering temperature that high-phosphor oolitic hematite mixes with coal dust, the preferred 120min of roasting time.
4. a kind of high-phosphor oolitic hematite according to claim 1 prepares high-purity iron oxide red method, it is characterised in that
The mass concentration of sulfuric acid preferably 18%；The volume mass ratio preferably 10 of sulfuric acid and magnetic concentrate：1ml/g.
5. a kind of high-phosphor oolitic hematite according to claim 1 prepares high-purity iron oxide red method, it is characterised in that
The mixing normal-temperature reaction time preferred 30min of sulfuric acid and magnetic concentrate.
6. a kind of high-phosphor oolitic hematite according to claim 1 prepares high-purity iron oxide red method, it is characterised in that
The oxidant is hydrogen peroxide.
7. a kind of high-phosphor oolitic hematite according to claim 1 prepares high-purity iron oxide red method, it is characterised in that
Sediment after oxidation filtering, preferably sintering temperature are 800 DEG C, time 60min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255628A (en) * | 2019-05-24 | 2019-09-20 | 中南民族大学 | The method that high-phosphor oolitic hematite prepares high-purity polymeric ferric sulfate flocculant |
| CN113912130A (en) * | 2021-11-29 | 2022-01-11 | 龙佰集团股份有限公司 | Iron oxide red and preparation method thereof |
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| EP0487479A2 (en) * | 1990-11-22 | 1992-05-27 | A/S Sydvaranger | A method for purifying iron oxide |
| CN101264876A (en) * | 2008-04-21 | 2008-09-17 | 中南大学 | Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite |
| CN105803189A (en) * | 2016-05-16 | 2016-07-27 | 贵州大学 | Method for efficiently removing phosphorus from high-phosphorus oolitic hematite |
| CN106906327A (en) * | 2017-03-24 | 2017-06-30 | 贵州大学 | A kind of method that high-phosphor oolitic hematite efficiently carries iron |
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| EP0487479A2 (en) * | 1990-11-22 | 1992-05-27 | A/S Sydvaranger | A method for purifying iron oxide |
| CN101264876A (en) * | 2008-04-21 | 2008-09-17 | 中南大学 | Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite |
| CN105803189A (en) * | 2016-05-16 | 2016-07-27 | 贵州大学 | Method for efficiently removing phosphorus from high-phosphorus oolitic hematite |
| CN106906327A (en) * | 2017-03-24 | 2017-06-30 | 贵州大学 | A kind of method that high-phosphor oolitic hematite efficiently carries iron |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255628A (en) * | 2019-05-24 | 2019-09-20 | 中南民族大学 | The method that high-phosphor oolitic hematite prepares high-purity polymeric ferric sulfate flocculant |
| CN113912130A (en) * | 2021-11-29 | 2022-01-11 | 龙佰集团股份有限公司 | Iron oxide red and preparation method thereof |
| CN113912130B (en) * | 2021-11-29 | 2023-07-07 | 龙佰集团股份有限公司 | Iron oxide red and preparation method thereof |
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Application publication date: 20180112 Assignee: Wuhan University of science and Technology Business Incubator Co.,Ltd. Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000003 Denomination of invention: A method for preparing high purity iron oxide red from high phosphorus oolitic hematite Granted publication date: 20200218 License type: Common License Record date: 20201021 |
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Assignee: Wuhan University of science and Technology Business Incubator Co.,Ltd. Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000003 Date of cancellation: 20230505 |