CN109825701A - The method for preparing rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite - Google Patents

The method for preparing rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Download PDF

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CN109825701A
CN109825701A CN201910284780.XA CN201910284780A CN109825701A CN 109825701 A CN109825701 A CN 109825701A CN 201910284780 A CN201910284780 A CN 201910284780A CN 109825701 A CN109825701 A CN 109825701A
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ilmenite
titanium dioxide
leaching
chloride
rich
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CN109825701B (en
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李化全
孙鹏
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SHANDONG DOGUIDE GROUP CO Ltd
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Abstract

The invention belongs to new material technology fields, are specifically related to a kind of method for preparing rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite.Leaching and filtering including ilmenite, the drying calcining preparation rich-titanium material of filter cake, washing lotion recycle, and mother liquor concentrations prepare iron oxide red and ammonium chloride.This method by using Titanium Dioxide Produced by Chloride Procedure produce in the waste hydrochloric acid that discharges, it is comprehensively utilized, reduce environmental pollution and control expense, the new method using waste hydrochloric acid preparation rich-titanium material and by-product iron oxide red and ammonium chloride is realized, the existing irretrievable problem of Titanium Dioxide Produced by Chloride Procedure waste hydrochloric acid can be eradicated, realize the recycling of waste, process flow and easy to operate, it is easily achieved, meets the international carbon footprint advocated and life Cycle Theory now, there is good economic benefit and social benefit.

Description

Rich-titanium material and comprehensive utilization are prepared using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method
Technical field
The invention belongs to new material technology fields, are specifically related to a kind of utilization chloride process titanium dioxide abraum salt Acid leaching ilmenite The method for preparing rich-titanium material and comprehensive utilization.
Background technique
Titanium deposit can be divided into rock mine and two kinds of placer, and rock mine is primary ore, and placer is secondary ore, belong to sedimentary rock mineral deposit. The main titanium-containing iron ore of rock mine, rutile content is low, and FeO content is high, general FeO:Fe2O3In 2.9-5.8.Impurity in rock mine SiO2And Al2O3Content is higher, while being mingled with the oxides such as vanadium, chromium, copper, cobalt, and mineral phase structure is fine and close, separates TiO2With other at Divide difficulty, the Panzhihua mineral deposit in China just belongs to Yan Kuang, and the content of calcium and magnesium is higher.
Placer contains the mineral such as ilmenite and rutile, general TiO2Grade it is high, aoxidize serious placer, the oxidation of iron Object is lost after weathering, TiO2It is free to form rutile ore, FeO can further weathering, formation Fe2O3, Fe2O3Content it is high, reach To FeO:Fe2O3The content of < 1, the impurity MnO being mingled in placer are higher, also association monazite, zircon etc. in placer.Due to Most of placer is by weathering, and mineral structure is loose, TiO2Enrichment be easy, through the resulting rutile of ore dressing and ferrotianium The TiO of mine2Grade it is high, mineral grain is bigger.
Currently, titanium white production technology is divided into chloridising and sulfuric acid process, the chloridising production production capacity whole world accounts for about 56%, China Titanium white production based on sulfuric acid process, Titanium Dioxide Produced by Chloride Procedure production capacity accounts for about 6.5% or so of domestic titanium dioxide aggregated capacity.But For sulfuric acid process, chloridising has process short, the advantages that superior product quality, three waste discharge is less, therefore, chloridising titanium White powder production technology is the state-run Development Technology technique of current country.But the external Titanium Dioxide Produced by Chloride Procedure production technology to China It is constantly in confidential state.The integrality and technical advance of domestic chlorination law technology are more external, and there are also very big distances.Chloridising The decomposition media used in production process is chlorine, this part chlorine a part recycles in system, and another part can only It is discharged with the pattern of hydrochloric acid, this part waste hydrochloric acid of discharge, current main processing mode is to neutralize, and after neutralization, is generated a large amount of Abraum salt, can not utilize, limit chloridising develop and there are environmental risk because chloridising removes the only a fews such as silver Ion is that precipitating is outer, and all soluble matter of other ions, storage is unstable, leads to not the drawbacks such as stockpiling.How to comprehensively utilize This part of waste hydrochloric acid, turns waste into wealth, and comprehensive utilization, is the break-through point in Titanium Dioxide Produced by Chloride Procedure production technology future.
Furthermore it mainly prepares high titanium slag using electric furnace smelting process in generating at present, artificial gold is prepared by Reductive leaching Red stone.Electric furnace smelting process prepares high titanium slag using generation technique is smelted, and simple and easy, equipment enlarging, the three wastes are few, easy to process The advantages that recycling, occupies leading position.But the production technology is limited to the removal ability of calcium and magnesium;Reductive leaching is Australia Leah CSIR O greatly studies a kind of successfully high-grade ilmenite of suitable weathering, and strong reduction requires temperature height, technical difficulty big.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of utilization chloride process titanium dioxide abraum salt Acid leaching ferrotianium The method that mine prepares rich-titanium material and comprehensive utilization.This method preferably utilizes chloride process titanium dioxide waste hydrochloric acid, carries out the life of rich-titanium material It produces, and by remaining waste hydrochloric acid and the chloride comprehensive reutilization that is mingled with.
The method of the present invention for preparing rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite, Leaching and filtering including ilmenite, the drying calcining preparation rich-titanium material of filter cake, washing lotion recycle, mother liquor concentrations preparation oxidation Iron oxide red and ammonium chloride.
Wherein:
The leaching of ilmenite is specifically with filtering: by ilmenite and chloride process titanium dioxide waste hydrochloric acid according to certain quality volume Than being mixed, abraum salt Acid leaching is carried out under stirring condition, after leaching, is filtered while hot.
The mass concentration of chloride process titanium dioxide waste hydrochloric acid is 20~25%, mass volume ratio GTiO2:VHCl=1:2~5, stirring Speed control is in 30~60r/min, and at 5~9 hours, whipping temp was controlled in the range of 30~80 DEG C for mixing time control.
The drying calcining preparation rich-titanium material of filter cake is specifically: the filtrate after cake filtration is by Ca2+、Mg2+Ion removes general labourer After sequence, obtained FeCl3And FeCl2Enter iron oxide red and ammonium chloride preparation section as mother liquor;Filter cake after filters pressing is used first Originally after water washing 2~3 times, then filter cake is placed in Muffle furnace and carries out drying calcining, the washing lotion after washing recycles.
The temperature of drying calcining is in 350~450 DEG C, and drying time is 2~4 hours.
Washing lotion recycles specifically: cleaning solution being returned to the leaching operation of ilmenite, waste hydrochloric acid is configured with it, makes to give up The mass concentration of hydrochloric acid controls in the range of 20~25%, uses as leaching liquid.
Mother liquor concentrations prepare iron oxide red with ammonium chloride: will pass through Ca2+、Mg2+It is obtained after ion removal of impurities process FeCl3And FeCl2Further steam is used to be concentrated as mother liquor, after carrying out air oxidation, ammonium bicarbonate soln is added, instead Should be until pink ferric carbonate occur, after static 30~60min, precipitating is placed in Muffle furnace and dries by filtration washing precipitating Dry calcining, is made iron oxide red;By the solution after filtration washing in the range of 80~95 DEG C, it is concentrated into crystal appearance, then It is down to room temperature, crystallizes and ammonium chloride product is made.
It is concentrated using steam, makes full Fe concentration control in the range of 80~160g/L, carry out 30~60min of air oxidation Afterwards, according to V (FeCI3)/V(NH4HCO3Ammonium bicarbonate soln is added in the volume ratio of)=1:2.6~3.8, ammonium bicarbonate soln Concentration is 100~180g/L.
Until calcination temperature is increased to 650 DEG C from room temperature, after 650 DEG C of 30~50min of heat preservation, it is cooled to room temperature naturally, It grinds and iron oxide red is made.
The present invention mainly utilizes the waste hydrochloric acid generated in Titanium Dioxide Produced by Chloride Procedure production process, is comprehensively utilized, system Standby rich-titanium material, then remaining waste hydrochloric acid and the chloride recovery being mingled with are utilized.
The method of the present invention for preparing rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite, Cardinal principle is that primary step is exactly the iron and other impurities removed in ilmenite, to improve the product of titanium dioxide as far as possible Position.The phenomenon that there are high pulverization rates due to hydrochloric acid method causes product fineness partially thin, therefore how production filtering high expensive drops High pulverization rate during less salt Ore Leaching becomes the most important thing of research, and hydrochloric acid method leaching process leads to serious dusting occur The reason of phenomenon, mainly exists due to hydrolysis, and the particle for hydrolyzing titanium dioxide generated is too thin, large specific surface area, table Face free energy is high, and absorption is serious between particle, forms spherical particle.
The hydrochloric acid leaching of ilmenite is a complicated heterogeneous reaction, and reaction product is a variety of complexings containing chlorine root Object.
FeTiO3+6H+→Fe2++Ti4++3H2O
2FeO·TiO2+ 6HCl==2FeCl2+TiO2+TiOCl2+3H2O
2MgO·TiO2+ 6HCl==2MgCl2+TiO2+TiOCl2+3H2O
2CaO·TiO2+ 6HCl==2CaCl2+TiO2+TiOCl2+3H2O
2Fe2O3·TiO2+ 14HCl==4FeCl3+TiO2+TiOCl2+7H2O
There is partial-titanium dissolution then to hydrolyze again in dilute hydrochloric acid leaching process, hydrolysis are as follows:
TiOCl2+(X+1)H2O==TiO2·xH2O+2HCl
The present invention directly leaches ilmenite by using hydrochloric acid, removes FeO, CaO, MgO, Fe in ilmenite2O3Deng stabilization Property difference trapped oxide, to improve the grade of titanium dioxide.
The leaching condition in hydrochloric acid method leaching process is explored, the generation of hydrolysis is reduced, so that high pulverization rate is reduced, at To improve TiO2The method of quality.By creative exploration, ilmenite is leached using normal pressure leaching technology, chloridising The mass concentration of titanium white waste hydrochloric acid is 20~25%, mass volume ratio GTiO2:VHCl=1:2~5, reaction time control 5~9 Hour, reaction temperature control is at 30~80 DEG C, the TiO of preparation2Content is in 80~90% ranges.
The group branch of leaching initial stage iron and titanium enters solution with the dissolution of identical speed, and after reacting a period of time, iron continues Dissolution, titanium occur hydrolytic precipitation, cause the concentration of the titanium in solution to decline, an equilibrium level is finally reached, by leaching The selection of condition reduces and reaches the balance time used, thus the phenomenon that the pulverization rate occurred during reducing hydrochloric acid leaching is high, Make the TiO of preparation2Mass content is in 80~90% ranges.
The property and Leaching way of mineral surface are affected to the generation of rich-titanium material, can by the ilmenite slightly restored To change the property of mineral surface, the generation of rich-titanium material is improved.
After filters pressing obtains filter cake, filtrate removes Ca by aerating oxidation2+、Mg2+Plasma impurity.
Compared with the prior art, the present invention has the following beneficial effects:
(1) side of the present invention that rich-titanium material and comprehensive utilization are prepared using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, the TiO using chloride process titanium dioxide waste hydrochloric acid as leaching reagent, after leaching2Content reach 80~90%, obtained after filters pressing Filter cake be further processed the rich titanium ore of preparation or synthetic rutile, filtrate prepares iron oxide red and ammonium chloride after removal of impurities, Fe in iron oxide red2O3Mass content > 90%, the mass content > 97% of ammonium chloride in ammonia chloride crystal.
(2) this method by using Titanium Dioxide Produced by Chloride Procedure produce in the waste hydrochloric acid that discharges, comprehensively utilized, reduce ring Border pollution and control expense realize the new method using waste hydrochloric acid preparation rich-titanium material and by-product iron oxide red and ammonium chloride, The existing irretrievable problem of Titanium Dioxide Produced by Chloride Procedure waste hydrochloric acid can be eradicated, the recycling of waste, process flow and behaviour are realized Make simple, it is easy to accomplish, meet the international carbon footprint advocated and life Cycle Theory now, there is good economic benefit and society Benefit.
Detailed description of the invention
Fig. 1 is to utilize chloride process titanium dioxide abraum salt Acid leaching ilmenite preparation rich-titanium material and material Comprehensive recycle technology stream Cheng Tu.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
A method of rich-titanium material and comprehensive utilization, including ferrotianium are prepared using chloride process titanium dioxide abraum salt Acid leaching ilmenite The leaching and filtering of mine, the drying calcining preparation rich-titanium material of filter cake, washing lotion recycle, and mother liquor concentrations prepare iron oxide red and chlorine Change ammonium.
(1) Titanium Dioxide Produced by Chloride Procedure waste hydrochloric acid mass concentration is controlled 20%, by itself and ilmenite according to mass volume ratio In GTiO2:VHClIt is mixed, is stirred in the range of=1:2, in 30r/min, mixing time control is small 5 for mixing speed control When, temperature controls in the range of 30 DEG C, carries out abraum salt Acid leaching, and leaching is finished, filtered while hot.
(2) the drying calcining preparation rich-titanium material of filter cake: the filtrate after cake filtration passes through Ca2+、Mg2+Ion removal of impurities process The FeCl obtained afterwards3And FeCl2Mother liquor enters iron oxide red and ammonium chloride preparation section.Filtered filter cake uses tap water again After washing 2 times, the washing lotion after washing is recycled.Filter cake is placed in Muffle furnace and dries calcining, temperature controls in 350 DEG C, Drying time is 4 hours.
(3) cleaning solution is returned into leaching operation, configures waste hydrochloric acid with it, make the control of its concentration in the range of 20%, It is used as leaching liquid.
(4) Ca mother liquor concentrations preparation iron oxide red and ammonium chloride: will be passed through2+、Mg2+It is obtained after ion removal of impurities process FeCl3And FeCl2Mother liquor further steam is used to be concentrated, make its full Fe concentration control in the range of 80g/L, carry out After air oxidation 30min, ammonium bicarbonate soln concentration is controlled in the range of 100g/L, according to V (FeCl3)/V(NH4HCO3)= Ammonium bicarbonate soln is added in 1/2.6 volume ratio, guarantees that ammonium bicarbonate soln is excessive, is reacted to pink ferric carbonate and is Only, after static 30min, filtration washing precipitating will be deposited in Muffle furnace and dry calcining, and calcination temperature is increased to 650 from room temperature It until DEG C, after 650 DEG C of heat preservation 30min, is cooled to room temperature naturally, grinds and iron oxide red is made.
By the solution after filtration washing in the range of 80 DEG C, it is concentrated into crystal appearance, then slow cooling, crystallization is made Ammonium chloride product.
Embodiment 2
A method of rich-titanium material and comprehensive utilization, including ferrotianium are prepared using chloride process titanium dioxide abraum salt Acid leaching ilmenite The leaching and filtering of mine, the drying calcining preparation rich-titanium material of filter cake, washing lotion recycle, and mother liquor concentrations prepare iron oxide red and chlorine Change ammonium.
(1) Titanium Dioxide Produced by Chloride Procedure waste hydrochloric acid mass concentration is controlled 25%, by itself and ilmenite according to mass volume ratio In GTiO2:VHClIt is mixed, is stirred in the range of=1:5, in 60r/min, mixing time control is small 9 for mixing speed control When, temperature controls in the range of 80 DEG C, carries out abraum salt Acid leaching, and leaching is finished, filtered while hot.
(2) the drying calcining preparation rich-titanium material of filter cake: the filtrate after cake filtration passes through Ca2+、Mg2+Ion removal of impurities process The FeCl obtained afterwards3And FeCl2Mother liquor enters iron oxide red and ammonium chloride preparation section.Filtered filter cake uses tap water again After washing 3 times, the washing lotion after washing is recycled.Filter cake is placed in Muffle furnace and dries calcining, temperature controls in 450 DEG C, Drying time is 2 hours.
(3) cleaning solution is returned into leaching operation, configures waste hydrochloric acid with it, make the control of its concentration in the range of 25%, It is used as leaching liquid.
(4) Ca mother liquor concentrations preparation iron oxide red and ammonium chloride: will be passed through2+、Mg2+It is obtained after ion removal of impurities process FeCl3And FeCl2Mother liquor further steam is used to be concentrated, make its full Fe concentration control in the range of 160g/L, carry out After air oxidation 60min, ammonium bicarbonate soln concentration is controlled in the range of 180g/L, according to V (FeCI3)/V(NH4HCO3)= Ammonium bicarbonate soln is added in 1/3.8 volume ratio, guarantees that ammonium bicarbonate soln is excessive, is reacted to pink ferric carbonate and is Only, after static 60min, filtration washing precipitating will be deposited in Muffle furnace and dry calcining, and calcination temperature is increased to 650 from room temperature It until DEG C, after 650 DEG C of heat preservation 50min, is cooled to room temperature naturally, grinds and iron oxide red is made.
By the solution after filtration washing in the range of 95 DEG C, concentration value crystal occurs, then slow cooling, and crystallization is made Ammonium chloride product.
Embodiment 3
A method of rich-titanium material and comprehensive utilization, including ferrotianium are prepared using chloride process titanium dioxide abraum salt Acid leaching ilmenite The leaching and filtering of mine, the drying calcining preparation rich-titanium material of filter cake, washing lotion recycle, and mother liquor concentrations prepare iron oxide red and chlorine Change ammonium.
(1) by the control of Titanium Dioxide Produced by Chloride Procedure waste hydrochloric acid mass concentration in the range of 22%, by itself and ilmenite concentrate according to matter Volume ratio is measured in GTiO2:VHClIt is mixed, is stirred in the range of=1:3, mixing speed is controlled in 40r/min, mixing time control At 6 hours, temperature controlled in the range of 50 DEG C system, carried out abraum salt Acid leaching, leaching is finished, filtered while hot.
(2) the drying calcining preparation rich-titanium material of filter cake: the filtrate after cake filtration passes through Ca2+、Mg2+Ion removal of impurities process The FeCl obtained afterwards3And FeCl2Mother liquor enters iron oxide red and ammonium chloride preparation section;Filtered filter cake uses tap water again After washing 2 times, the washing lotion after washing is recycled.Filter cake is placed in Muffle furnace and dries calcining, temperature controls in 400 DEG C, Drying time is 3 hours.
(3) cleaning solution is returned into leaching operation, configures waste hydrochloric acid with it, make the control of its concentration in the range of 22%, It is used as leaching liquid.
(4) Ca mother liquor concentrations preparation iron oxide red and ammonium chloride: will be passed through2+、Mg2+It is obtained after ion removal of impurities process FeCl3And FeCl2Mother liquor further steam is used to be concentrated, make its full Fe concentration control in the range of 100g/L, carry out After air oxidation 40min, excessive ammonium bicarbonate soln is added, ammonium bicarbonate soln concentration is controlled in the range of 120g/L, pressed According to V (FeCl3)/V(NH4HCO3Ammonium bicarbonate soln is added in the volume ratio of)=1/3.0, is reacted to pink ferric carbonate and occurs Until, after static 50min, filtration washing precipitating will be deposited in Muffle furnace and dry calcining, and calcination temperature is increased to from room temperature It until 650 DEG C, after 650 DEG C of heat preservation 40min, is cooled to room temperature naturally, grinds and iron oxide red is made.
By the solution after filtration washing in the range of 90 DEG C, concentration value crystal occurs, then slow cooling, and crystallization is made Ammonium chloride product.
Content detection analysis is carried out to the product of raw material ilmenite and synthetical recovery, wherein for recovery product (rich-titanium material, Iron oxide red, ammonium chloride) mass content analysis, each embodiment carries out 4 measurements, is averaged, to reduce detection error.
1 embodiment 1-3 ilmenite constituent analysis table of table
Project TiO2% Tfe% FeO% Fe2O3%
Embodiment 1 46.72 33 36.78 6.29
Embodiment 2 46.84 34.43 37.72 7.29
Embodiment 3 47.81 34.42 38.01 6.95
The rich-titanium material quality analytical table of 2 embodiment 1-3 of table preparation
The iron oxide red quality analysis table of 3 embodiment 1-3 of table preparation
The ammonium chloride quality analysis table of 4 embodiment 1-3 of table preparation

Claims (9)

1. a kind of method for preparing rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite, feature exist In: leaching and filtering including ilmenite, the drying calcining preparation rich-titanium material of filter cake, washing lotion recycle, mother liquor concentrations preparation Iron oxide red and ammonium chloride.
2. according to claim 1 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: the leaching of ilmenite is specifically with filtering: by ilmenite and chloride process titanium dioxide waste hydrochloric acid according to certain Mass volume ratio is mixed, and abraum salt Acid leaching is carried out under stirring condition, after leaching, is filtered while hot.
3. according to claim 2 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: the mass concentration of chloride process titanium dioxide waste hydrochloric acid is 20~25%, mass volume ratio GTiO2:VHCl=1:2 ~5, mixing speed control is in 30~60r/min, and at 5~9 hours, whipping temp was controlled at 30~80 DEG C for mixing time control In range.
4. according to claim 1 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: the drying calcining preparation rich-titanium material of filter cake is specifically: the filtrate after cake filtration is by Ca2+、Mg2+From Son cleans after process, obtained FeCl3And FeCl2Enter iron oxide red and ammonium chloride preparation section as mother liquor;Filter after filters pressing Cake is used first originally after water washing 2~3 times, then filter cake is placed in Muffle furnace and carries out drying calcining, the washing lotion circulation after washing It utilizes.
5. according to claim 4 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: the temperature for drying calcining is in 350~450 DEG C, and drying time is 2~4 hours.
6. according to claim 1 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: washing lotion recycles the leaching operation that cleaning solution is specifically returned to ilmenite, configures abraum salt with it Acid controls the mass concentration of waste hydrochloric acid in the range of 20~25%, uses as leaching liquid.
7. according to claim 1 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: mother liquor concentrations prepare iron oxide red with ammonium chloride and are specifically: will pass through Ca2+、Mg2+After the process that cleans The FeCl arrived3And FeCl2Further steam is used to be concentrated as mother liquor, after carrying out air oxidation, it is molten that ammonium hydrogen carbonate is added Liquid, until being reacted to pink ferric carbonate appearance, after static 30~60min, precipitating is placed in Muffle furnace by filtration washing precipitating Middle drying calcining, is made iron oxide red;By the solution after filtration washing in the range of 80~95 DEG C, it is concentrated into crystal appearance, Then it is down to room temperature, crystallizes and ammonium chloride product is made.
8. according to claim 7 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: be concentrated using steam, make full Fe concentration control in the range of 80~160g/L, carry out air oxidation After 30~60min, according to V (FeCI3)/V(NH4HCO3Ammonium bicarbonate soln, bicarbonate is added in the volume ratio of)=1:2.6~3.8 The concentration of ammonium salt solution is 100~180g/L.
9. according to claim 7 prepare rich-titanium material and comprehensive utilization using chloride process titanium dioxide abraum salt Acid leaching ilmenite Method, it is characterised in that: until calcination temperature is increased to 650 DEG C from room temperature, after 650 DEG C of 30~50min of heat preservation, be down to naturally After room temperature, grinds and iron oxide red is made.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110713213A (en) * 2019-11-27 2020-01-21 宜宾天原海丰和泰有限公司 Method for preparing nano iron oxide red by using chlorination waste residues
CN114671462A (en) * 2022-03-30 2022-06-28 河南佰利联新材料有限公司 Method for recycling chlorination process acidic wastewater and application
CN115974140A (en) * 2021-11-27 2023-04-18 四川省有色矿冶科技有限公司 Method for producing titanium oxychloride by acidolysis of ilmenite with hydrochloric acid acidolysis solution
CN115974145A (en) * 2021-11-27 2023-04-18 四川省有色矿冶科技有限公司 Production process for continuously preparing titanium dioxide and titanium-rich material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1710122A (en) * 2005-06-16 2005-12-21 昆明理工大学 Method for preparing rutile type titanium-rich material from primary titanium-rich material
CN105621495A (en) * 2014-10-31 2016-06-01 陕西启源科技发展有限责任公司 Method for preparing high purity iron oxide red from picking waste liquid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1710122A (en) * 2005-06-16 2005-12-21 昆明理工大学 Method for preparing rutile type titanium-rich material from primary titanium-rich material
CN105621495A (en) * 2014-10-31 2016-06-01 陕西启源科技发展有限责任公司 Method for preparing high purity iron oxide red from picking waste liquid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
余家华等: "国内外钛矿和富钛料生产现状及发展趋势", 《世界有色金属》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110713213A (en) * 2019-11-27 2020-01-21 宜宾天原海丰和泰有限公司 Method for preparing nano iron oxide red by using chlorination waste residues
CN115974140A (en) * 2021-11-27 2023-04-18 四川省有色矿冶科技有限公司 Method for producing titanium oxychloride by acidolysis of ilmenite with hydrochloric acid acidolysis solution
CN115974145A (en) * 2021-11-27 2023-04-18 四川省有色矿冶科技有限公司 Production process for continuously preparing titanium dioxide and titanium-rich material
CN115974145B (en) * 2021-11-27 2024-04-19 官长平 Production process for continuously preparing titanium pigment and titanium-rich material
CN114671462A (en) * 2022-03-30 2022-06-28 河南佰利联新材料有限公司 Method for recycling chlorination process acidic wastewater and application

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