CN103910382B - Method for preparing artificial rutile - Google Patents
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Abstract
The invention provides a method for preparing an artificial rutile. The method comprises the following steps: performing three-stage leaching on modified ilmenite obtained by virtue of oxidation-strong reduction treatment, wherein the first stage of leaching is mixed leaching of a leachate obtained after the second stage of leaching is completed and a modified titanium raw material, the second stage of leaching refers to a mixed reaction of a leachate obtained after the third stage of leaching is completed and a solid phase material obtained after the first stage of leaching, and the third stage refers to a mixed reaction of a 18-36wt% new prepared hydrochloric acid and a solid phase material obtained after the second stage of leaching; finally, carrying out filtering, washing and drying to obtain a high-grade artificial at the grade of 90-95wt%. The method is used for preparing the high-grade, low-impurity content artificial rutile product with the titanium dioxide content of 90-95wt% by using the ilmenite as the raw material, and the production of waste acid is reduced and the purposes of saving energy and reducing emission are achieved.
Description
Technical field
The present invention relates to titanium white preparation field, more particularly, relate to the technique that a kind of hydrochloric acid method prepares artificial rutile.
Background technology
Rutile title originates from Latin, and the ore of main component that to be a kind of titanium dioxide be, contained titanium dioxide crystal belongs to tetragonal system.Rutile is mainly used in extracting titanium and manufacturing white pigment, is essential industry raw material, is applied to the field such as metallurgy, chemical industry.The maximum country of natural rutile reserves is Australia, is secondly South Africa, India, plug Lapie gram, Ukraine etc.Rutile reserves only forty-two million t has been verified in the current whole world.This can not meet the demand of people far away, and then people adopt different technique to prepare artificial rutile to replace natural rutile, and the artificial rutile output of current global major country exceedes natural rutile.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to solve in above-mentioned prior art the one or more problems existed.
An object of the present invention is that providing a kind of is preparing the method for artificial rutile, to leach impurity in titanium material preferably (such as, iron, calcium, magnesium, manganese, aluminium) make titanium preferably enrichment, and lower the spent acid amount produced in leaching process, reach the object of energy-saving and emission-reducing.
To achieve these goals, the invention provides a kind of method preparing artificial rutile.Said method comprising the steps of: be oxidized and reduction treatment ilmenite, obtain Modified Titanium raw material, wherein, the oxidizing temperature of described oxide treatment is 900 ~ 1100 DEG C, and the reduction temperature of described reduction treatment is 800 ~ 1000 DEG C; Normal pressure leaching is carried out to Modified Titanium raw material, wherein, described the step that Modified Titanium raw material carries out normal pressure leaching to be comprised:
First time leaches when producing in the following ways, is that hydrochloric acid and the Modified Titanium raw material of 18 ~ 36% reacts 180 ~ 360min under the temperature condition of 80 ~ 110 DEG C by mass percentage concentration, obtains first paragraph leach liquor and first paragraph leaching solid materials; The hydrochloric acid being 18 ~ 36% again by mass percentage concentration by described first paragraph leaching solid materials leaches 120 ~ 180min under the temperature condition of 80 ~ 110 DEG C, obtains second segment leach liquor and second segment leaching solid materials.
Leach in the following ways in production process after first time production, Modified Titanium raw material is mixed with first paragraph leaching liquid and carries out first paragraph leaching, obtain first paragraph leach liquor and first paragraph leaching solid materials; Described first paragraph leaching solid materials is mixed with the second leaching liquid and carries out second segment leaching, obtain second segment leach liquor and second segment leaching solid materials; Described second segment is leached solid materials and carries out three stages acid leach with the mixed in hydrochloric acid newly configured, obtain three stages acid leach liquid and three stages acid leach solid materials, the mass percentage concentration of the hydrochloric acid of described new configuration is 18 ~ 36%; Wherein, the first paragraph leaching liquid adopted when second time is produced is described first time produce the first paragraph leach liquor obtained, and second segment leaching liquid is described first time produce the second segment leach liquor obtained; The first paragraph leaching liquid that production process after second time adopts is the last second segment leach liquor producing gained, and second segment leaching liquid is the last three stages acid leach liquid producing gained; Described first time the second segment of producing gained leach solid materials or described first time produce after production process gained three stages acid leach solid materials after filtration, washing and drying obtain artificial rutile product.
An embodiment of the method for artificial rutile produced according to the present invention, in production process after described first time produces, described first paragraph leaches, described second segment leaches and the extraction temperature of described three stages acid leach is 70 ~ 110 DEG C, and extraction time is 30 ~ 180min.
An embodiment of the method for artificial rutile produced according to the present invention, in the production process after described first time produces, the weight ratio that described first paragraph leaches the hydrochloric acid of Modified Titanium raw material used and the new configuration used of described three stages acid leach is 5 ~ 50%.
An embodiment of the method for artificial rutile produced according to the present invention, in described ilmenite, content of titanium dioxide is 44 ~ 60wt%, TFe content is 32.50 ~ 34.63wt%, FeO content is 34.09 ~ 37.74wt%, and granularity is 60 ~ 200 orders.
An embodiment of the method for artificial rutile produced according to the present invention, in described artificial rutile product, content of titanium dioxide is 90 ~ 95wt%.
An embodiment of the method for artificial rutile produced according to the present invention, carries out described oxide treatment under oxidizing atmosphere 30 ~ 50% conditions more than needed, then under reducing atmosphere 30 ~ 50% conditions more than needed, carries out reduction treatment.
An embodiment of the method for artificial rutile produced according to the present invention, preferably, described oxidizing temperature is 950 ~ 1000 DEG C, and described reduction temperature is 850 ~ 950 DEG C.
An embodiment of the method for artificial rutile produced according to the present invention, described oxidation and reduction treatment carry out ground under fluidising conditions.
An embodiment of the method for artificial rutile produced according to the present invention, described filtration step adopts solid-liquid separating equipment to filter.
An embodiment of the method for artificial rutile produced according to the present invention, described method also comprises the step of described artificial rutile product being carried out to magnetic separation.
An embodiment of the method for artificial rutile produced according to the present invention, comprises TFe32.50 ~ 34.63wt% in Modified Titanium iron ore, FeO38.17 ~ 41.39wt% and TiO
244 ~ 60wt%, the granularity of described Modified Titanium raw material is 60 ~ 200 orders.
Compared with prior art, the present invention can be that raw material is prepared content of titanium dioxide and reached the higher-grade of 90 ~ 95wt%, the artificial rutile product of low impurity content with ilmenite, and reduces the generation of spent acid, reaches the object of energy-saving and emission-reducing.
Embodiment
Hereinafter, will describe in detail in conjunction with exemplary embodiment according to the method preparing artificial rutile of the present invention.
Prepare the method for artificial rutile according to an exemplary embodiment of the present invention, comprise the following steps:
(1) in fluidizing reactor, Strong oxdiative and strong reduction treatment are carried out to ilmenite, obtain Modified Titanium raw material (i.e. Modified Titanium iron ore).Wherein, ilmenite can be ilmenitite ore deposit, ferrotianium placer etc., and such as, the ilmenite handled by this example comprises TFe32.50 ~ 34.63wt%, TiO
244 ~ 60wt%, FeO34.09 ~ 37.74wt%, SiO
22.71 ~ 3.49wt%, and the granularity of ilmenite is 60 ~ 200 orders.The ore deposit of ilmenite is based on ilmenite mutually, usually with the ferrous FeTiO of metatitanic acid
3represent.
Wherein, ilmenite adds generation oxidizing reaction in fluidization region that the inherent oxygenant (such as, air) of fluidizing reactor formed, and in oxidation processes, controlled oxidization temperature of reaction is 900 ~ 1100 DEG C, oxidizing atmosphere affluence 30% ~ 50%.The main purpose of carrying out oxide treatment within the scope of above-mentioned oxidizing reaction temperature is transformed mutually ilmenite ores, particularly, ferro element is moved to particle surface, thing after conversion shows sagenite structure in leaching process, rutile thing is insoluble to hydrochloric acid mutually, in leaching process still solids mutually in, impurity element such as magnesium, calcium, the iron etc. of solubility enter in liquid phase, reach being separated of titanium dioxide and impurity element magnesium, calcium, iron etc., titanium is able to enriching for adult and makes rutile; If oxidizing reaction temperature is greater than 1100 DEG C, then exceedes thing phase transition temperature and in addition equipment damaged and waste energy, if oxidizing reaction temperature is less than 900 DEG C, do not reached thing phase transition temperature, can powder phenomenon-tion have been produced when the follow-up leaching of Modified Titanium concentrate.Preferably, oxidizing reaction temperature is 950 ~ 1000 DEG C.
Oxidizing atmosphere is imbued with 30 ~ 50% for strong oxidizing property atmosphere, and it refers to that such as, complete oxidation needs 7m in the air capacity air capacity basis required for ilmenite complete oxidation increasing by 30 ~ 50%
3air so oxidizing atmosphere more than needed 30% use 9.1m exactly
3air, oxidizing atmosphere more than needed 50% is exactly use 10.5m
3air.Under strong oxidizing property atmospheric condition, carry out the contact that oxidizing reaction can make ilmenite normal fluidization be conducive to material and air improve rate of oxidation and oxidation ratio.
Reduction treatment is that ilmenite after making oxide treatment is at reductive agent (such as, CO, H
2deng) formation reducing atmosphere fluidised form region in occur reduction reaction, in reduction treatment process, control reduction reaction temperature be 800 ~ 1000 DEG C, reducing atmosphere affluence 30 ~ 50%.The object of carrying out reduction treatment within the scope of above-mentioned reduction reaction temperature the ferro element be oxidized in oxidation reaction process is reduced into iron to be at a low price beneficial to follow-up leaching, improves leaching rate; If reduction reaction temperature is greater than 1000 DEG C, then increase equipment cost and cause energy dissipation, if reduction reaction temperature is less than 850, reduction ratio is low, affects product grade.Preferably, reduction reaction temperature is 850 ~ 950 DEG C.
Reducing atmosphere is imbued with 30 ~ 50% for strong reducing property atmosphere, increase by 30 ~ 50% on its theoretical addition amount basis referring to the reductive agent of ferric iron back needed for ferrous iron in the ilmenite after by oxide treatment.
In addition, the Strong oxdiative of this example and strong reduction treatment carry out ground under fluidising conditions, adopt fluidization technology to work continuously, the frequent therefore mass transfer of the relativity between fluidization technology particle and fluid and heat transfer efficiency high and the reaction of condition harshness can be competent at.
In this example, TFe (full iron) 32.50 ~ 34.63wt%, FeO38.17 ~ 41.39wt% and TiO is comprised in gained Modified Titanium iron ore
244 ~ 60wt%, its granularity is 60 ~ 200 orders.
(2) three stages acid leach is carried out to Modified Titanium raw material, particularly:
First paragraph leaches: the second segment leach liquor of Modified Titanium raw material with last consignment of Modified Titanium raw material is mixed and heated, holding temperature requires at 70 ~ 110 DEG C, soaking time 30 ~ 180min, obtains first paragraph leach liquor (or being called leaching mother liquor) and first paragraph leaches solid materials.
Second segment leaches: first paragraph is leached gained solid materials and mix with the three stages acid leach liquid of last consignment of Modified Titanium raw material and heat, holding temperature requires at 70 ~ 110 DEG C, soaking time 30 ~ 180min, obtains second segment leach liquor and second segment leaches solid materials.
Three stages acid leach: second segment is leached gained solid materials with the mixed in hydrochloric acid newly configure and heat, holding temperature requirement is at 70 ~ 110 DEG C, soaking time 30 ~ 180min, obtains three stages acid leach liquid and three stages acid leach solid materials.
Wherein, the Modified Titanium raw material that adds of first paragraph Leaching reaction and three stages acid leach react the hydrochloric acid of the new configuration of heating is 5 ~ 50% by weight; The hydrochloric acid of the said new configuration of the application refers to that mass percentage concentration is the hydrochloric acid of 18 ~ 36%; Leaching process can be normal pressure leaching.
(3) three stages acid leach gained solid materialss after filtration, washing and drying finally obtain artificial rutile product, artificial rutile product content of titanium dioxide 90 ~ 95wt%.Wherein, described filtration step adopts solid-liquid separating equipment to filter, such as vacuum band-type filter machine, Plate Filtration etc.Drying temperature can be 450 DEG C ~ 600 DEG C, dry 3 ~ 8h.Namely the application does not carry out magnetic separation process artificial rutile product grade can reach 90 ~ 95wt%, if add that its grade of magnetic separation step can rise 2 percentage points again.
The present invention adopts three stages acid leach Modified Titanium raw material, the impurity such as the calcium in Modified Titanium raw material, magnesium, iron and hydrochloric acid reaction also enter hydrochloric acid soln, titanium elements stays the object reaching enrichment titanium in solids, method products obtained therefrom according to the present invention is of high grade, and leach liquor recycle in leaching process, save the consumption of hydrochloric acid, for acid regeneration reduces pressure.In addition, ensure extraction time and the temperature of three stages acid leach, obtain best preparation effect, and can not have a negative impact.
In addition, if first production, be namely when processing first Modified Titanium raw material, above-mentioned steps (2) only adopts two sections of leachings, particularly:
First paragraph leaches: first under the temperature condition of 80 ~ 110 DEG C, react 180 ~ 360min with the hydrochloric acid newly configured and Modified Titanium raw material, obtains first paragraph leach liquor and first paragraph leaching solid materials.Wherein, first paragraph leach liquor is applied to the first paragraph leaching of next time producing and makes leaching liquid.
Second segment leaches: the solid materials of first paragraph leaching gained leaches 120 ~ 180min with new complex salt acid again under the temperature condition of 80 ~ 110 DEG C, obtains second segment leach liquor and second segment leaching solid materials.Wherein, the second segment leach liquor of gained is applied to the second segment leaching of next time producing and makes leaching liquid.Second segment leaches the solid materials of gained and directly carries out filtering, to wash and drying obtains artificial rutile product.
In order to understand above-mentioned exemplary embodiment of the present invention better, below in conjunction with concrete example, it is further described.
Example 1
The main chemical compositions of the ilmenite handled by this example is content of titanium dioxide is the full iron of 45wt%, TFe() content be 32.50wt%, FeO content is 34.09wt%, granularity is 60 ~ 200 orders.
Added by ilmenite in fluidizing reactor and carry out Strong oxdiative and strong reduction treatment, wherein, the feeding quantity of ilmenite is 1.2 tons/hour, during oxide treatment, and controlled oxidization temperature of reaction is 950 DEG C, and the intake of air is 188m
3; During reduction treatment, controlling reduction reaction temperature is 950 DEG C, and the intake of reducing gas is 150m
3.The composition of gained Modified Titanium iron ore and granularity are in table 1.
Table 1 Modified Titanium iron ore component and granularity
Weigh in the leach liquor obtained after second segment that 5t Modified Titanium iron ore joins last consignment of Modified Titanium concentrate under the condition constantly stirred has leached, carry out normal pressure leaching, be warming up to 70 DEG C, insulation 30min completes first paragraph leaching; First paragraph leach three stages acid leach that gained solid formation joins last consignment of Modified Titanium concentrate under the condition constantly stirred complete after gained leach liquor in, carry out normal pressure leaching, be warming up to 110 DEG C, insulation 120min completes second segment and leaches; Second segment leaches gained solid formation and join 54m under the condition constantly stirred
3technical hydrochloric acid is with addition of 40m
3the mass concentration that water obtains is in the hydrochloric acid soln of 20%, carry out normal pressure leaching, be warmed up to 80 DEG C, insulation 180min completes three stages acid leach, and filter, wash and dry acquisition artificial rutile, the grade of gained artificial rutile is 92wt% after testing, and CaO content 0.421%, content of MgO 0.255%, MnO content 0.025%, SiO
2content 4.12%, Al
2o
3content 0.254%, Fe
2o
3content 1.35%.
Example 2
Ilmenite content of titanium dioxide handled by this example is 53wt%, TFe content be 34.63wt%, FeO content is 37.74wt%, and granularity is 60 ~ 200 orders.
Added by ilmenite in fluidizing reactor and carry out Strong oxdiative and strong reduction treatment, wherein, the feeding quantity of ilmenite is 1.5 tons/hour, during oxide treatment, and controlled oxidization temperature of reaction is 980 DEG C, and the intake of air is 254m
3; During reduction treatment, controlling reduction reaction temperature is 850 DEG C, and the intake of reducing gas is 162m
3.Gained Modified Titanium iron ore composition and granularity thereof are in table 2.
Table 2 Modified Titanium iron ore component and granularity
Weigh in the leach liquor obtained after second segment that 8t Modified Titanium iron ore joins last consignment of Modified Titanium iron ore under the condition constantly stirred has leached and carry out normal pressure leaching, be warmed up to 110 DEG C, insulation 180min completes first paragraph leaching; First paragraph leaches in the leach liquor obtained after three stages acid leach that gained solid formation joins last consignment of Modified Titanium iron ore under the condition constantly stirred completes and carries out normal pressure leaching, and be warmed up to 70 DEG C, insulation 30min completes second segment and leaches; Second segment leaches gained solid formation and join 5m under the condition constantly stirred
3technical hydrochloric acid is with addition of 3m
3the mass concentration of water gained is carry out normal pressure leaching in the hydrochloric acid soln of 22%, be warmed up to 110 DEG C, insulation 30min completes three stages acid leach, filter, wash and dry acquisition artificial rutile, after testing, the grade of gained artificial rutile is 93wt%, and CaO content 0.419%, content of MgO 0.257%, MnO content 0.025%, SiO
2content 3.12%, Al
2o
3content 0.245%, Fe
2o
3content 1.359%.
Example 3
Ilmenite content of titanium dioxide handled by this example is 44wt%, TFe content be 33wt%, FeO content is 36.45wt%, and granularity is 60 ~ 200 orders.
Added by ilmenite in fluidizing reactor and carry out Strong oxdiative and strong reduction treatment, wherein, the feeding quantity of ilmenite is 2.0 tons/hour, during oxide treatment, and controlled oxidization temperature of reaction is 980 DEG C, and the intake of air is 360m
3; During reduction treatment, controlling reduction reaction temperature is 860 DEG C, and the intake of reducing gas is 234m
3.Gained Modified Titanium iron ore composition and granularity thereof are in table 3.
Table 3 Modified Titanium iron ore component and granularity
Weigh second segment that 10t Modified Titanium iron ore joins last consignment of Modified Titanium iron ore under the condition constantly stirred has leached after gained leach liquor in carry out normal pressure leaching, be warmed up to 90 DEG C, insulation 120min completes first paragraph leaching; First paragraph leach three stages acid leach that gained solid formation joins last consignment of Modified Titanium iron ore under the condition constantly stirred complete after gained leach liquor in, carry out normal pressure leaching, be warmed up to 90 DEG C, insulation 180min completes second segment and leaches; Second segment leaches gained solid formation and join 28m under the condition constantly stirred
3technical hydrochloric acid is with addition of 2m
3the mass concentration of water gained is in the hydrochloric acid soln of concentration 30%, carry out normal pressure leaching, be warmed up to 70 DEG C, insulation 120min completes three stages acid leach, filters, washs and dry acquisition artificial rutile, after testing, the grade of gained artificial rutile is 90wt%, and CaO content 0.664%, content of MgO 0.544%, MnO content 0.027%, SiO
2content 4.78%, Al
2o
3content 0.269%, Fe
2o
3content 2.14%.
Example 4
Ilmenite content of titanium dioxide handled by this example is 57wt%, TFe content be 34wt%, FeO content is 37.12wt%, and granularity is 60 ~ 200 orders.
Added by ilmenite in fluidizing reactor and carry out Strong oxdiative and strong reduction treatment, wherein, the feeding quantity of ilmenite is 2.0 tons/hour, during oxide treatment, and controlled oxidization temperature of reaction is 1000 DEG C, and the intake of air is 360m
3; During reduction treatment, controlling reduction reaction temperature is 900 DEG C, and the intake of reducing gas is 234m
3.Gained Modified Titanium iron ore composition and granularity are in table 4.
Table 4 Modified Titanium iron ore component and granularity
Weigh second segment that 20t Modified Titanium iron ore joins last consignment of Modified Titanium iron ore under the condition constantly stirred has leached after gained leach liquor in carry out normal pressure leaching, be warmed up to 100 DEG C, insulation 60min completes first paragraph leaching; First paragraph leach three stages acid leach that gained solid formation joins last consignment of Modified Titanium iron ore under the condition constantly stirred complete after gained leach liquor in, carry out normal pressure leaching, be warmed up to 100 DEG C, insulation 60min completes second segment and leaches; Second segment leaches gained solid formation and join 36m technical hydrochloric acid with addition of 14m under the condition constantly stirred
3the mass concentration of water concentration gained is in the hydrochloric acid soln of 26%, carry out normal pressure leaching, be warmed up to 100 DEG C, insulation 60min completes three stages acid leach, filters, washs and dry acquisition artificial rutile, after testing, the grade of gained artificial rutile is 95wt%, and CaO content 0.341%, content of MgO 0.267%, MnO content 0.019%, SiO
2content 2.51%, Al
2o
3content 0.242%, Fe
2o
3content 1.20%.
Example 5
Ilmenite content of titanium dioxide handled by this example is 54wt%, TFe content be 32.8wt%, FeO content is 36.89wt%, and granularity is 60 ~ 200 orders.
Added by ilmenite in fluidizing reactor and carry out Strong oxdiative and strong reduction treatment, wherein, the feeding quantity of ilmenite is 2.0 tons/hour, during oxide treatment, and controlled oxidization temperature of reaction is 990 DEG C, and the intake of air is 336m
3; During reduction treatment, controlling reduction reaction temperature is 870 DEG C, and the intake of reducing gas is 218m
3.Gained Modified Titanium iron ore composition and granularity are in table 5.
Table 5 Modified Titanium iron ore component and granularity
Weigh second segment that 20t Modified Titanium iron ore joins last consignment of Modified Titanium iron ore under the condition constantly stirred has leached after hydrochloric acid soln in, carry out normal pressure leaching, be warmed up to 100 DEG C, insulation 60min completes first paragraph leaching; First paragraph leach three stages acid leach that gained solid formation joins last consignment of Modified Titanium iron ore under the condition constantly stirred complete after gained leach liquor in carry out normal pressure leaching, be warmed up to 100 DEG C, insulation 60min completes second segment and leaches; Second segment leaches gained solid formation and join 36m under the condition constantly stirred
3technical hydrochloric acid is with addition of 14m
3the mass concentration of water gained is carry out normal pressure leaching in the hydrochloric acid soln of concentration 26%, be warmed up to 100 DEG C, insulation 60min completes three stages acid leach, filter, wash and dry acquisition artificial rutile, after testing, the grade of gained artificial rutile is 92wt%, and CaO content 0.421%, content of MgO 0.255%, MnO content 0.025%, SiO
2content 4.12%, Al
2o
3content 0.254%, Fe
2o
3content 1.35%.
As can be seen from example 1 to example 5, the artificial rutile grade (i.e. content of titanium dioxide) that method according to the present invention prepares reaches 90 ~ 95wt%.
In sum, the present invention can be that artificial rutile prepared by raw material with ilmenite, pyrotic smelting de-iron is required no in preparation process, and directly leach through Strong oxdiative and strong reduction and multistage the artificial rutile product being drying to obtain high-quality, multistage leaches and not only can upgrade, and can reduce spent acid output.That is, the present invention can be not only the artificial rutile product that raw material prepares that grade of titanium dioxide is high, foreign matter content is few with ilmenite, and reduces the generation of spent acid, reaches the object of energy-saving and emission-reducing.
Although above by describing the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that when not departing from the spirit and scope that claim limits, various amendment and change can be carried out to exemplary embodiment of the present invention.
Claims (9)
1. prepare a method for artificial rutile, it is characterized in that, said method comprising the steps of:
Be oxidized and reduction treatment ilmenite, obtain Modified Titanium raw material, wherein, the oxidizing temperature of described oxide treatment is 900 ~ 1100 DEG C, and the reduction temperature of described reduction treatment is 800 ~ 1000 DEG C;
Normal pressure leaching is carried out to Modified Titanium raw material, wherein, described the step that Modified Titanium raw material carries out normal pressure leaching to be comprised:
First time leaches when producing in the following ways, is that hydrochloric acid and the Modified Titanium raw material of 18 ~ 36% reacts 180 ~ 360min under the temperature condition of 80 ~ 110 DEG C by mass percentage concentration, obtains first paragraph leach liquor and first paragraph leaching solid materials; The hydrochloric acid being 18 ~ 36% again by mass percentage concentration by described first paragraph leaching solid materials leaches 120 ~ 180min under the temperature condition of 80 ~ 110 DEG C, obtains second segment leach liquor and second segment leaching solid materials;
Leach in the following ways in production process after first time production, Modified Titanium raw material is mixed with first paragraph leaching liquid and carries out first paragraph leaching, obtain first paragraph leach liquor and first paragraph leaching solid materials; Described first paragraph leaching solid materials is mixed with the second leaching liquid and carries out second segment leaching, obtain second segment leach liquor and second segment leaching solid materials; Described second segment is leached solid materials and carries out three stages acid leach with the mixed in hydrochloric acid newly configured, obtain three stages acid leach liquid and three stages acid leach solid materials, the mass percentage concentration of the hydrochloric acid of described new configuration is 18 ~ 36%; Wherein, the first paragraph leaching liquid adopted when second time is produced is described first time produce the first paragraph leach liquor obtained, and second segment leaching liquid is described first time produce the second segment leach liquor obtained; The first paragraph leaching liquid that production process after second time adopts is the last second segment leach liquor producing gained, and second segment leaching liquid is the last three stages acid leach liquid producing gained;
Described first time the second segment of producing gained leach solid materials or described first time produce after production process gained three stages acid leach solid materials after filtration, washing and drying obtain artificial rutile product;
In production process after described first time produces, described first paragraph leaches, described second segment leaches and the extraction temperature of described three stages acid leach is 70 ~ 110 DEG C, and extraction time is 30 ~ 180min.
2. the method preparing artificial rutile according to claim 1, it is characterized in that, in production process after described first time produces, the weight ratio that described first paragraph leaches the hydrochloric acid of Modified Titanium raw material used and the new configuration used of described three stages acid leach is 5 ~ 50%.
3. the method preparing artificial rutile according to claim 1, it is characterized in that, in described ilmenite, content of titanium dioxide is 44 ~ 60wt%, TFe content is 32.50 ~ 34.63wt%, FeO content is 34.09 ~ 37.74wt%, and granularity is 60 ~ 200 orders.
4. the method preparing artificial rutile according to claim 1, is characterized in that, in described artificial rutile product, content of titanium dioxide is 90 ~ 95wt%.
5. the method preparing artificial rutile according to claim 1, is characterized in that, under oxidizing atmosphere 30 ~ 50% conditions more than needed, carry out described oxide treatment, then under reducing atmosphere 30 ~ 50% conditions more than needed, carries out reduction treatment.
6. the method preparing artificial rutile according to claim 1, is characterized in that, described oxidizing temperature is 950 ~ 1000 DEG C, and described reduction temperature is 850 ~ 950 DEG C.
7. the method preparing artificial rutile according to claim 1, is characterized in that, described oxidation and reduction treatment carry out ground under fluidising conditions.
8. the method preparing artificial rutile according to claim 1, is characterized in that, described filtration step adopts solid-liquid separating equipment to filter.
9. the method preparing artificial rutile according to claim 1, is characterized in that, comprises TFe 32.50 ~ 34.63wt% in Modified Titanium iron ore, FeO 38.17 ~ 41.39wt% and TiO
244 ~ 60wt%, the granularity of described Modified Titanium raw material is 60 ~ 200 orders.
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| CN105648207A (en) * | 2016-02-25 | 2016-06-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method for reduced ilmenite powder |
| CN107955885B (en) * | 2017-11-21 | 2020-09-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of modified titanium concentrate |
| CN110627118A (en) * | 2019-10-31 | 2019-12-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for solving refining of artificial rutile |
| CN112266015B (en) * | 2020-10-28 | 2022-07-19 | 山东鲁北企业集团总公司 | System and method for producing artificial rutile by continuous acid leaching of titanium white waste acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1114364A (en) * | 1994-06-29 | 1996-01-03 | 冶金工业部长沙矿冶研究院 | Method and equipment for producing titanium-rich material |
| US5885324A (en) * | 1996-07-26 | 1999-03-23 | Tiomin Resources, Inc. | Method for the production of synthetic rutile |
| CN101244841A (en) * | 2008-03-25 | 2008-08-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing synthetic rutile |
| CN103482696A (en) * | 2013-09-02 | 2014-01-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for preparing titanium solution from fluidized acidolysis titanium-containing material |
-
2014
- 2014-04-01 CN CN201410128606.3A patent/CN103910382B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1114364A (en) * | 1994-06-29 | 1996-01-03 | 冶金工业部长沙矿冶研究院 | Method and equipment for producing titanium-rich material |
| US5885324A (en) * | 1996-07-26 | 1999-03-23 | Tiomin Resources, Inc. | Method for the production of synthetic rutile |
| CN101244841A (en) * | 2008-03-25 | 2008-08-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing synthetic rutile |
| CN103482696A (en) * | 2013-09-02 | 2014-01-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for preparing titanium solution from fluidized acidolysis titanium-containing material |
Non-Patent Citations (2)
| Title |
|---|
| "制取人造金红石工艺技术的新进展";邓国珠等;《钢铁钒钛》;20040331;第25卷(第1期);44-50 * |
| "氧化方式对盐酸浸出攀枝花钛铁矿的影响";梁相博等;《过程工程学报》;20101031;第10卷(第5期);939-943 * |
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