CN107460345A - A kind of method for producing high titanium slag - Google Patents
A kind of method for producing high titanium slag Download PDFInfo
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- CN107460345A CN107460345A CN201610384795.XA CN201610384795A CN107460345A CN 107460345 A CN107460345 A CN 107460345A CN 201610384795 A CN201610384795 A CN 201610384795A CN 107460345 A CN107460345 A CN 107460345A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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Abstract
The invention discloses a kind of method for producing high titanium slag, this method can obtain TiO using electro-titanium slag as raw material after mechanical activation, high-temperature roasting, washing, hot acid removal of impurities, washing, calcination2Content is more than 96% high titanium slag.First, ball mill grinding is added after titanium slag and activator being mixed;The additive that material mixes after to activation mixes, and is contained with graphite crucible, is put into high-temperature roasting in roaster;Washed after roasting material is ground with ionized water, solid-liquor separation is carried out after the completion of washing, liquid phase is concentrated by evaporation recovery additive, deionized water washing process is used after solid-phase material pickling;Calcined after obtained solid material is dried and high titanium slag is just made.Low-grade titanium slag can be changed into rich-titanium material by this method, and also greatly reduce the yield of accessory substance green vitriol.Full-flow process is simple, high income, concentration ratio are high, environmentally friendly, cost is low, and industrial applications prospect is good.
Description
Technical field
The invention belongs to field of metallurgy, is related to a kind of method for producing high titanium slag.
Background technology
High titanium slag is by physics production process and the titanium ore enriched substance that is formed is commonly called as, and fusing titanium ore is heated by electric furnace,
Make the enriched substance of the titanium dioxide high content that titanium dioxide and iron fusing obtain after separating in titanium ore.High titanium slag neither waste residue,
Nor accessory substance, but produce the quality raw materials of titanium tetrachloride, titanium dioxide and titanium sponge.
China's titanium dioxide and titanium sponge industry development are rapid, and because high titanium slag Ti content is high, " three wastes " produce(Processing)Amount
Few, the utilization rate of resource and the energy is high, and can help product quality raising, and the demand of China's high titanium slag increases rapidly.Although
The yield of domestic high titanium slag is constantly expanding, but still can not meet domestic powerful demand, and it is a large amount of that China is also required to import every year
High titanium slag make breach supplement.High titanium slag industry in China's still shows the situation of supply deficiency at present, in a few years from now on China
High titanium slag stills need a large amount of imports.
Within significant period of time from now on, titanium dioxide, metal sponge titanium products using high titanium slag as raw material still belong to country
The key project of development is encouraged in industry restructuring.Primary mineral products of the high titanium slag as shortage, market prospects are very wide.
Some domestic more strong enterprises have started to the high titanium slag of independent research high-quality, some leading enterprise's inputs
The advanced technology and large scale equipment of huge capital Introduced From Abroad production high titanium slag.Strengthen research and development capabilities, utilize its technology
Advantage production high-quality, high yield product and intratype competition, seize market, by as maximum competing in high titanium slag industry development
Strive trend.
The titanium slag that some grades are 60% or so can be produced during traditional smelting titanium slag with electric stove, this kind of titanium slag is because grade
The relatively low production that cannot be directly used to Titanium Dioxide Produced by Chloride Procedure and titanium sponge.If but these titanium slags are not used and will result in
The significant wastage of resource.If directly this kind of titanium slag is enriched into more than 90% using electric furnace needs high cost again.If directly
This kind of titanium slag using sulfuric acid to leach, it can not obtain being adapted to chloridising production titanium dioxide and the high-grade produced needed for titanium sponge rich
Titanium material.So improving this kind of titanium slag grade using prior art means has very important realistic meaning.
The rich-titanium material that traditional electro-smelting ilmenite prepares typically contains TiO265%~75%, content of calcium and magnesium is up to 5%
~7%.And chloridising production titanium white requires the TiO in raw material2Content is more than 90%, and CaO+MgO content is less than 1.5%.
CN 200310110821 discloses a kind of raising titanium slag TiO2The method of grade, the invention are given birth to using Panxi Diqu
The titanium slag of production, through fluosolids roasting, gas reduction and high pressure acidleach, obtain TiO2Content be 89.8% synthetic rutile, the work
Skill fluidization requires higher with high-tension apparatus, and obtained synthetic rutile grade is relatively low.
CN 100455683C disclose a kind of method that rich-titanium material is produced with electro-titanium slag, and this method is with Yunnan somewhere titanium
Slag is raw material, proposes soda acid joint lixiviation process, obtains TiO2>90% rich-titanium material, the technique use high-tension apparatus, cost of investment
Higher, technical operation difficulty is big, and obtained rich-titanium material quality is relatively low.
United States Patent (USP) " the Upgrading sorelslag for production of of Patent No. 4038363
Synthetic rutile " disclose a kind of method that grade for improving Sorel slag prepares synthetic rutile, by oxidizing roasting
Titanium slag afterwards obtains high-grade dioxy through being calcined at wet-milling, washing, dilute sulfuric acid two-stage leaching, filtering, washing, 850 DEG C~950 DEG C
Change the synthetic rutile of titanium.
United States Patent (USP) " the Method of preparing a synthetic rutile from of Patent No. 5389355
A titaniferous slag containing alkaline earth metals " are disclosed from the titanium containing alkaline-earth metal
The method that synthetic rutile is extracted in slag, by the titanium slag after oxidation at more than 0.1 MPa and not less than 190 DEG C with excessive 20%
Hydrochloric acid solution acidolysis obtain synthetic rutile, the step of this synthetic rutile can also be leached by caustic soda, continues to reduce
The content of the impurity such as Si and Ca therein.
United States Patent (USP) " the Method to upgrade titania slag and of Patent No. 5830420
Resulting product " disclose the method for improving titanium slag grade, and the titanium slag after oxidizing roasting and reduction roasting is existed
Not less than inorganic acid acidleach is used under 125 DEG C, 0.35MPa~0.48MPa, acidleach product is scrubbed or washs, after alkali leaching, 600
DEG C~800 DEG C of calcination obtain high-grade titanium dioxide titanium slag.
The content of the invention
For problem above, it is an object of the invention to provide a kind of method for producing high titanium slag, this method:With electric furnace titanium
Slag is raw material, and TiO is can obtain after mechanical activation, high-temperature roasting, hot acid removal of impurities, washing, calcination2Grade is more than 96%
High titanium slag.This method flow is simple, concentration ratio is high, environmentally friendly, cost is low, and industrialization prospect is good.
The technical solution adopted by the present invention is:A kind of method for producing high titanium slag, it is characterised in that carry out according to the following steps:
(1)Ball mill grinding is added after titanium slag and activator are mixed by a certain percentage to less than 0.074 μm;
(2)Material mixes a certain amount of modifying agent and mixed after to activation, is contained with graphite crucible, is put into roaster and carries out high temperature
Roasting;
(3)Roasting material mill is dissipated, by certain liquid-solid ratio, washed with hot water, wash water is by being concentrated by evaporation recovery additive;
(4)By the dilute hydrochloric acid solution dissolved impurity of the product after washing, separation of solid and liquid after the completion of reaction, hydrochloric acid circular regeneration;
(5)Solid phase hot water washing process after hot acid removal of impurities, the liquid phase after processing can do slurry;
(6)Solid material drying, calcining after washing process, are made high titanium slag.
Step(1)Described activator is NaOH, Na2CO3、NaHCO3, one or more in CaO, titanium slag and activator
Mixing quality ratio be 1:0.5~1:3, soak time is 1~3 hour, and Task-size Controlling is in 100 mesh~300 after mechanical activation
Mesh.Step(2)The additive added during described high-temperature roasting is phosphate, borate, sulfate, one kind in carbonate or
It is several, graphite crucible is selected during roasting, at 800 DEG C~1000 DEG C, roasting time control is small 1.5~2.5 for sintering temperature control
When.Step(3)70 DEG C~90 DEG C of hot water of described roasting material, by liquid-solid ratio 3:1~5:1 10~40 points of washing
Clock, washing evaporation concentration recovery additive.Step(4)After described washing material with 10%~30% dilute hydrochloric acid solution at 75 DEG C
At a temperature of~100 DEG C, by liquid-solid ratio 3:1~5:1 hot acid cleans 30~60 minutes, and liquid phase reclaims hydrochloric acid after removal of impurities.Step(5)
50 DEG C~80 DEG C of hot water of solid-phase material after described hot acid removal of impurities, by liquid-solid ratio 3:1~5:1 washing process, after processing
Liquid phase can do water scouring water.Step(6)Solid-phase material after described washing after drying, at 600 DEG C~800 DEG C, calcines 1
~2 hours, high titanium slag is just made.
Advantages of the present invention essentially consists in:
(1)Meet the requirement of chloridising production titanium white using high titanium slag obtained by the inventive method, there is extensive adaptability.
(2)Crystal structure through mechanical activation raw material is destroyed, and is provided the foundation condition for subsequent treatment.
(3)Anosovite structure in Ti-enriched slag can be destroyed after adding additive high-temperature roasting, fundamentally solves anosovite knot
Structure is difficult to the problem of direct acidleach removal of impurities, and water-soluble or sour compound is generated after high-temperature roasting, effectively can be reduced in titanium slag
Calcium magnesium element content.
(4)Filtrate is Low acid solution after hot acid removal of impurities, recycles simplicity, so as to which sour consumption be greatly reduced, reduces environment
Pollution.
(5) present invention process flow is short, equipment investment is few, energy consumption is low, and accessory substance is less, and environmental pollution is small, meets energy-conservation
Emission reduction and the requirement of clean metallurgical.
Brief description of the drawings
Fig. 1 is a kind of process chart for the method for producing high titanium slag.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, one is entered to the present invention below in conjunction with instantiation
Step is described in detail:
Embodiment 1
Referring to accompanying drawing 1, condition:Take Ti02The % of content 71.63 electro-titanium slag 100g, add the ball mill fine grinding of 50g activators
To 96% less than 0.074mm;Then with additive in mass ratio 10:1 mixes, and the roasting time at 900 DEG C of sintering temperature
2h;Roasting material presses liquid-solid ratio 5 with 85 DEG C of deionized waters:1 washing lh;Solid-liquor separation is carried out after washing, liquid phase passes through steaming
Concentration and recovery additive is sent out, the hydrochloric acid solution that solid phase mass concentration is 15% presses liquid-solid ratio 4 under 105 DEG C, condition of normal pressure:1 acid
Wash 2h;The liquid phase that solid-liquid separation on ore pulp comes out after pickling reclaims hydrochloric acid through evaporation, and the solid phase after pickling is pressed with 90 DEG C of deionized waters
Liquid-solid ratio 5:1 carries out washing process;Solid-liquor separation is carried out after the completion of washing, liquid phase can return to technique front end and do slurry, Gu
Mutually through drying, calcining, Ti0 is made2Content is 96.82% high titanium slag.
Embodiment 2
Referring to accompanying drawing 1, condition:Take Ti02The % of content 71.63 electro-titanium slag 100g, add the ball mill fine grinding of 25g activators
To 96% less than 0.074mm;Then with additive in mass ratio 15:1 mixes, and the roasting time at 900 DEG C of sintering temperature
2h;Roasting material presses liquid-solid ratio 5 with 85 DEG C of deionized waters:1 washing lh;Solid-liquor separation is carried out after washing, liquid phase passes through steaming
Concentration and recovery additive is sent out, the hydrochloric acid solution that solid phase mass concentration is 15% presses liquid-solid ratio 4 under 105 DEG C, condition of normal pressure:1 acid
Wash 2h;The liquid phase that solid-liquid separation on ore pulp comes out after pickling reclaims hydrochloric acid through evaporation, and the solid phase after pickling is pressed with 90 DEG C of deionized waters
Liquid-solid ratio 5:1 carries out washing process;Solid-liquor separation is carried out after the completion of washing, liquid phase can return to technique front end and do slurry, Gu
Mutually through drying, calcining, Ti0 is made2Content is 89.65% high titanium slag.
Embodiment 3
Referring to accompanying drawing 1, condition:Take Ti02The % of content 71.63 electro-titanium slag 100g, add the ball mill fine grinding of 100g activators
To 96% less than 0.074mm;Then with additive in mass ratio 5:1 mixes, and the roasting time at 900 DEG C of sintering temperature
2h;Roasting material presses liquid-solid ratio 5 with 85 DEG C of deionized waters:1 washing lh;Solid-liquor separation is carried out after washing, liquid phase passes through steaming
Concentration and recovery additive is sent out, the hydrochloric acid solution that solid phase mass concentration is 15% presses liquid-solid ratio 4 under 105 DEG C, condition of normal pressure:1 acid
Wash 2h;The liquid phase that solid-liquid separation on ore pulp comes out after pickling reclaims hydrochloric acid through evaporation, and the solid phase after pickling is pressed with 90 DEG C of deionized waters
Liquid-solid ratio 5:1 carries out washing process;Solid-liquor separation is carried out after the completion of washing, liquid phase can return to technique front end and do slurry, Gu
Mutually through drying, calcining, Ti0 is made2Content is 90.22% high titanium slag.
Embodiment 4
Referring to accompanying drawing 1, condition:Take Ti02The % of content 71.63 electro-titanium slag 100g, add the ball mill fine grinding of 50g activators
To 96% less than 0.074mm;Then with additive in mass ratio 10:1 mixes, and the roasting time at 800 DEG C of sintering temperature
2h;Roasting material presses liquid-solid ratio 5 with 85 DEG C of deionized waters:1 washing lh;Solid-liquor separation is carried out after washing, liquid phase passes through steaming
Concentration and recovery additive is sent out, the hydrochloric acid solution that solid phase mass concentration is 15% presses liquid-solid ratio 4 under 105 DEG C, condition of normal pressure:1 acid
Wash 2h;The liquid phase that solid-liquid separation on ore pulp comes out after pickling reclaims hydrochloric acid through evaporation, and the solid phase after pickling is pressed with 90 DEG C of deionized waters
Liquid-solid ratio 5:1 carries out washing process;Solid-liquor separation is carried out after the completion of washing, liquid phase can return to technique front end and do slurry, Gu
Mutually through drying, calcining, Ti0 is made2Content is 88.98% high titanium slag.
Embodiment 5
Referring to accompanying drawing 1, condition:Take Ti02The % of content 71.63 electro-titanium slag 100g, add the ball mill fine grinding of 50g activators
To 96% less than 0.074mm;Then with additive in mass ratio 10:1 mixes, and when being calcined at 1000 DEG C of sintering temperature
Between 2h;Roasting material presses liquid-solid ratio 5 with 85 DEG C of deionized waters:1 washing lh;Solid-liquor separation is carried out after washing, liquid phase passes through
Recovery additive is concentrated by evaporation, the hydrochloric acid solution that solid phase mass concentration is 15% presses liquid-solid ratio 4 under 105 DEG C, condition of normal pressure:1
Pickling 2h;The liquid phase that solid-liquid separation on ore pulp comes out after pickling reclaims hydrochloric acid through evaporation, 90 DEG C of deionized waters of the solid phase after pickling
By liquid-solid ratio 5:1 carries out washing process;Solid-liquor separation is carried out after the completion of washing, liquid phase can return to technique front end and do slurry,
Ti0 is made through drying, calcining in solid phase2Content is 92.91% high titanium slag.
Embodiment 6
Referring to accompanying drawing 1, condition:Take Ti02The % of content 71.63 electro-titanium slag 100g, add the ball mill fine grinding of 50g activators
To 96% less than 0.074mm;Then with additive in mass ratio 10:1 mixes, and the roasting time at 900 DEG C of sintering temperature
2h;Roasting material presses liquid-solid ratio 5 with 85 DEG C of deionized waters:1 washing lh;Solid-liquor separation is carried out after washing, liquid phase passes through steaming
Concentration and recovery additive is sent out, the hydrochloric acid solution that solid phase mass concentration is 15% presses liquid-solid ratio 4 under 95 DEG C, condition of normal pressure:1 acid
Wash 2h;The liquid phase that solid-liquid separation on ore pulp comes out after pickling reclaims hydrochloric acid through evaporation, and the solid phase after pickling is pressed with 90 DEG C of deionized waters
Liquid-solid ratio 5:1 carries out washing process;Solid-liquor separation is carried out after the completion of washing, liquid phase can return to technique front end and do slurry, Gu
Mutually through drying, calcining, Ti0 is made2Content is 86.39% high titanium slag.
Claims (7)
- A kind of 1. method for producing high titanium slag, it is characterised in that carry out according to the following steps::(1)Ball mill grinding is added after titanium slag and activator are mixed by a certain percentage to less than 0.074 μm;(2)Material mixes a certain amount of additive and mixed after to activation, is contained with graphite crucible, is put into roaster and carries out high temperature Roasting;(3)Roasting material is ground, by certain liquid-solid ratio, washed with hot water, wash water is by being concentrated by evaporation recovery additive;(4)By the dilute hydrochloric acid solution dissolved impurity of the product after washing, separation of solid and liquid after the completion of reaction, hydrochloric acid circular regeneration;(5)Solid phase hot water washing process after hot acid removal of impurities, the liquid phase after processing can do slurry;(6)Solid material drying, calcining after washing process, are made high titanium slag.
- 2. the method for production high titanium slag according to claim 1, it is characterised in that activator NaOH, Na2CO3、 NaHCO3, one or more in CaO, the mixing quality ratio of titanium slag and activator is 1:0.5~1:3, soak time is 1~3 Hour, Task-size Controlling is in the mesh of 100 mesh~300 after mechanical activation.
- 3. the method for production high titanium slag according to claim 1, it is characterised in that the additive added during high-temperature roasting is One or more in phosphate, borate, sulfate, carbonate, graphite crucible is selected during roasting, and sintering temperature control exists 800 DEG C~1000 DEG C, roasting time was controlled at 1.5~2.5 hours.
- 4. the method for production high titanium slag according to claim 1, it is characterised in that roasting material is with 70 DEG C~90 DEG C Hot water, by liquid-solid ratio 3:1~5:1 washing 10~40 minutes, washing evaporation concentration recovery additive.
- 5. it is according to claim 1 production high titanium slag method, it is characterised in that after washing material with 10%~30% it is dilute Hydrochloric acid solution is at a temperature of 75 DEG C~100 DEG C, by liquid-solid ratio 3:1~5:1 hot acid is cleaned 30~60 minutes, and liquid phase is returned after removal of impurities Receive hydrochloric acid.
- 6. the method for production high titanium slag according to claim 1, it is characterised in that the solid-phase material after hot acid removal of impurities is with 50 DEG C~80 DEG C of hot water, by liquid-solid ratio 3:1~5:1 washing process, the liquid phase after processing can do water scouring water.
- 7. it is according to claim 1 production high titanium slag method, it is characterised in that the solid-phase material after washing after drying, At 600 DEG C~800 DEG C, calcine 1~2 hour, high titanium slag is just made.
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CN108774692A (en) * | 2018-06-13 | 2018-11-09 | 长江师范学院 | A kind of rich-titanium material for the method and its preparation preparing rich-titanium material using high calcium picrocrichtonite |
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CN111705226A (en) * | 2020-06-22 | 2020-09-25 | 眉山顺应动力电池材料有限公司 | Method for removing impurities from high-titanium slag |
CN112265987A (en) * | 2020-09-24 | 2021-01-26 | 中南大学 | Combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon slag |
CN114477276A (en) * | 2022-02-21 | 2022-05-13 | 四川顺应动力电池材料有限公司 | Method for preparing titanium tetrachloride |
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CN111705226B (en) * | 2020-06-22 | 2022-05-31 | 四川顺应动力电池材料有限公司 | Method for removing impurities from high-titanium slag |
CN112265987A (en) * | 2020-09-24 | 2021-01-26 | 中南大学 | Combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon slag |
CN114477276A (en) * | 2022-02-21 | 2022-05-13 | 四川顺应动力电池材料有限公司 | Method for preparing titanium tetrachloride |
CN114477276B (en) * | 2022-02-21 | 2024-01-09 | 四川顺应动力电池材料有限公司 | Method for preparing titanium tetrachloride |
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