CN103834798B - By low-grade TiO 2slag prepares the method for rich titanium material - Google Patents
By low-grade TiO 2slag prepares the method for rich titanium material Download PDFInfo
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- CN103834798B CN103834798B CN201210483809.5A CN201210483809A CN103834798B CN 103834798 B CN103834798 B CN 103834798B CN 201210483809 A CN201210483809 A CN 201210483809A CN 103834798 B CN103834798 B CN 103834798B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention is open a kind of by low-grade TiO
2slag prepares the method for rich titanium material, it is characterized in that: melt point slag for raw material with vanadium titano-magnetite through the titaniferous that retailoring-electric furnace drastic reduction obtains, its TiO
2content is about 35%-45%, and carry out crushing and screening to-200 orders, drying preheating, carries out sulfation preroasting, and alkali first through one section of normal pressure alkaline leaching, then through two sections of high pressure alkaline leachings, is finally soaked slag diluted acid normal pressure leaching by fired slags, and leached mud obtains TiO through washing drying
2the rich titanium material of content 60%-80%, can be widely used in the production of sulfate process titanium dioxide; The molten point slag of electric furnace of titanium is rich in enrichment process in this approach, and can make full use of the titanium resource in the vanadium titano-magnetite of China, and production cost is lower, environmental pollution is less, has good industrial application value.
Description
Technical field
The present invention relates to and melt by the electric furnace being rich in titanium a kind of method that point slag prepares rich titanium material.
Background technology
China's wide geographic area is all rich in a large amount of vanadium titano-magnetites, and when titanium resource situation is increasingly severe, how rationally, this part v-ti magnetite ore resources of efficiency utilization seems most important.For the vanadium titano-magnetite of different areas, the technical process of its processing mode and Commercial cultivation is entered and is also not quite similar." molten point of rotary hearth furnace coal-based direct reduction-electric furnace " new technological process of current domestic proposition, the target that the Comprehensive that can realize the elements such as iron in vanadium titano-magnetite, vanadium, titanium and chromium utilizes, compared with " blast furnace-converter " technique, demonstrate its superiority highlightedly.The molten point slag of the electric furnace that new technological process obtains, is rich in a large amount of titanium elements, can be recycled, and in non-new technological process technique in the past, the blast furnace slag being rich in titanium obtained or electric furnace slag, be not all able to Comprehensive and utilize.For rationally effectively extracting the titanium elements in China's vanadium titano-magnetite, enrichment process is carried out to the molten point slag of electric furnace, obtain the rich titanium material that can be used for sulfate process titanium dioxide and produce, thus improve the efficiency of the titanium ore utilization of resources, widen the comprehensive utilization scope of China's vanadium titano-magnetite, be of great practical significance.
Summary of the invention
the technical problem to be solved in the present invention: propose a kind of molten point slag of electric furnace being rich in titanium by enrichment process, the technological method of obtained rich titanium material.
technical scheme of the present invention
A kind of by low-grade TiO
2prepare the technological method of rich titanium material, melt point slag for raw material with vanadium titano-magnetite through the titaniferous that retailoring-electric furnace drastic reduction obtains, its TiO
2content is about 35%-45%, and carry out crushing and screening to-200 orders, drying preheating, carries out sulfation preroasting, and alkali first through one section of normal pressure alkaline leaching, then through two sections of high pressure alkaline leachings, is finally soaked slag diluted acid normal pressure leaching by fired slags, and leached mud obtains TiO through washing drying
2the rich titanium material of content 60%-80%.
Sulfuric acid concentration 80%-98% is chosen in the molten point slag sulfation preroasting of electric furnace after described drying and preheating.
The molten point slag sulfation pre-calcination temperature 150-450 DEG C of electric furnace after described drying and preheating.
Acid sludge mass ratio: 0.5:1-1.5:1 in the molten point slag sulfation preroasting of electric furnace after described drying and preheating.
The NaOH concentration range of one section of described normal pressure alkaline leaching is 1-3mol/L.
The temperature range of two sections of described high pressure alkaline leachings is 160-220 DEG C.
The NaOH concentration range of two sections of described high pressure alkaline leachings is 1.5-4mol/L.
The dilute hydrochloric acid concentration 1.5-3.0mol/L of described alkali leaching slag diluted acid normal pressure leaching.
The temperature 60-90 DEG C of described alkali leaching slag diluted acid normal pressure leaching.
beneficial effect of the present invention:
1, the molten point slag of the electric furnace obtained through retailoring-electric furnace drastic reduction with the vanadium titano-magnetite of China is for raw material, and the chemical constitution of this raw material, phase structure, mineral characteristic and electro-titanium slag, ilmenite concentrate have bigger difference;
2, the method for sulfation High Temperature Pre roasting is utilized to make fine and close mineral structure obtain corrosion, destroy the complicated embedding mode for cloth of mineral structure, under the high temperature conditions, part composite salt and vitriol oil generation chemical reaction, complicated combination is made to be able to separation and war in various degree or decomposition, for effective removal of impurities of next stage creates conditions;
3, High Temperature Pre fired slags is through crushing and screening, carries out one section of alkaline leaching, and the remnants acid on the one hand and in fired slags, removes free state silicon, the aluminium element in fired slags on the other hand; Because a molten point of slag derives from twice retailoring, its mineral structure is extremely complicated, and institute thinks the silicon, the aluminium element that remove in composition silicate, aluminate, and the method adopting two sections of high pressure base to soak removes silicon, aluminium element, and effect is ideal;
4, the method for normal pressure acidic leaching is utilized to remove the composite salt that in molten point slag, a large amount of impurity elements such as calcium, magnesium and part can react with acid solution.
The present invention also has certain suitability to being prepared rich titanium material by electro-titanium slag and ilmenite concentrate.
accompanying drawing explanation:
Fig. 1 process flow sheet of the present invention.
Embodiment
Embodiment 1:
The molten point slag 1000g of power taking stove, carry out abrasive dust, be milled to-200 orders, get molten point ground-slag 500g, dry 10h under 80 DEG C of conditions in loft drier, get dried molten point ground-slag 400g, the sulfuric acid being 98% with concentration mixes to mix thoroughly and carries out roasting, makes a molten point slag be pelletizing shape, gets maturing temperature 400 DEG C, sulfuric acid is 1:1, roasting time 3h with the mass ratio of molten point slag; Crushing and screening after the cooling of sulfation prebake slag, gets-200 order sulfation prebake slag 300g and carries out normal pressure alkaline leaching, choose NaOH concentration 2mol/L, extraction temperature 80 DEG C, extraction time 4h, and normal pressure alkali leaching slag is dried through washing and filtering; Get normal pressure alkali leaching slag 150g and carry out high pressure alkaline leaching under 200 DEG C of conditions, choosing NaOH concentration is 2.5mol/L, and extraction time is 3h, and oxygen pressure is 1.0MPa, and high pressure base leaching slag is dried through washing and filtering; Finally get high pressure base leaching slag 100g, mix with dilute hydrochloric acid solution and put into water-bath and react, the temperature of diluted acid leaching 80 DEG C, gets dilute hydrochloric acid concentration 2mol/L, extraction time 6h, liquid-solid ratio 3:1, and after acid leaching residue washs after filtration, under 80 DEG C of conditions, dry 10h, obtains TiO
2content is the rich titanium material of 78.2%.
Embodiment 2:
The molten point slag 1000g of power taking stove, carry out abrasive dust, be milled to-200 orders, get molten point ground-slag 500g, dry 10h under 80 DEG C of conditions in loft drier, get dried molten point ground-slag 400g, the sulfuric acid being 95% with concentration mixes to mix thoroughly and carries out roasting, makes a molten point slag be pelletizing shape, gets maturing temperature 350 DEG C, sulfuric acid is 1:1.2, roasting time 3h with the mass ratio of molten point slag; Crushing and screening after the cooling of sulfation prebake slag, gets-200 order sulfation prebake slag 300g and carries out normal pressure alkaline leaching, choose NaOH concentration 2.5mol/L, extraction temperature 70 DEG C, extraction time 3h, and normal pressure alkali leaching slag is dried through washing and filtering; Get normal pressure alkali leaching slag 150g and carry out high pressure alkaline leaching under 180 DEG C of conditions, choosing NaOH concentration is 3mol/L, and extraction time is 3h, and oxygen pressure is 1.2MPa, and high pressure base leaching slag is dried through washing and filtering; Finally get high pressure base leaching slag 100g, mix with dilute hydrochloric acid solution and put into water-bath and react, the temperature of diluted acid leaching 90 DEG C, get dilute hydrochloric acid concentration 2.5mol/L, extraction time 5h, liquid-solid ratio 3:1, after acid leaching residue washs after filtration, under 80 DEG C of conditions, dry 10h, obtains TiO
2content is the rich titanium material of 79.4%.
Embodiment 3:
The molten point slag 1000g of power taking stove, carry out abrasive dust, be milled to-200 orders, get molten point ground-slag 500g, dry 10h under 80 DEG C of conditions in loft drier, get dried molten point ground-slag 400g, the sulfuric acid being 98% with concentration mixes to mix thoroughly and carries out roasting, makes a molten point slag be pelletizing shape, gets maturing temperature 420 DEG C, sulfuric acid is 1:1.5, roasting time 2h with the mass ratio of molten point slag; Crushing and screening after the cooling of sulfation prebake slag, gets-200 order sulfation prebake slag 300g and carries out normal pressure alkaline leaching, choose NaOH concentration 2.5mol/L, extraction temperature 85 DEG C, extraction time 3h, and normal pressure alkali leaching slag is dried through washing and filtering; Get normal pressure alkali leaching slag 150g and carry out high pressure alkaline leaching under 200 DEG C of conditions, choosing NaOH concentration is 2.0mol/L, and extraction time is 3h, and oxygen pressure is 1.2MPa, and high pressure base leaching slag is dried through washing and filtering; Finally get high pressure base leaching slag 100g, mix with dilute hydrochloric acid solution and put into water-bath and react, the temperature of diluted acid leaching 85 DEG C, get dilute hydrochloric acid concentration 1.5mol/L, extraction time 4h, liquid-solid ratio 4:1, after acid leaching residue washs after filtration, under 80 DEG C of conditions, dry 10h, obtains TiO
2content is the rich titanium material of 80.2%.
The present invention also has certain suitability to being prepared rich titanium material by electro-titanium slag and ilmenite concentrate, but is particularly useful for extracting and reclaims vanadium titano-magnetite electric furnace and melt titanium in point slag.
Claims (2)
1. one kind by low-grade TiO
2slag prepares the method for rich titanium material, it is characterized in that: melt point slag for raw material with vanadium titano-magnetite through the titaniferous that retailoring-electric furnace drastic reduction obtains, its TiO
2content 35%-45%, carry out crushing and screening to-200 orders, drying preheating, carries out sulfation preroasting, and alkali first through one section of normal pressure alkaline leaching, then through two sections of high pressure alkaline leachings, is finally soaked slag diluted acid normal pressure leaching by fired slags, and leached mud obtains TiO through washing drying
2the rich titanium material of content 60%-80%;
Sulfuric acid concentration 80%-98% is chosen in the molten point slag sulfation preroasting of electric furnace after drying and preheating;
The molten point slag sulfation pre-calcination temperature 150-450 DEG C of electric furnace after drying and preheating;
The NaOH concentration range of one section of normal pressure alkaline leaching is 1-3mol/L;
The temperature range of two sections of high pressure alkaline leachings is 160-220 DEG C;
The NaOH concentration range of two sections of high pressure alkaline leachings is 1.5-4mol/L;
The dilute hydrochloric acid concentration 1.5-3.0mol/L of alkali leaching slag diluted acid normal pressure leaching;
The temperature 60-90 DEG C of alkali leaching slag diluted acid normal pressure leaching.
2. one according to claim 1 is by low-grade TiO
2slag prepares the method for rich titanium material, it is characterized in that: acid sludge mass ratio: 0.5:1-1.5:1 in the molten point slag sulfation preroasting of the electric furnace after drying and preheating.
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| CN201210483809.5A CN103834798B (en) | 2012-11-26 | 2012-11-26 | By low-grade TiO 2slag prepares the method for rich titanium material |
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| CN201210483809.5A CN103834798B (en) | 2012-11-26 | 2012-11-26 | By low-grade TiO 2slag prepares the method for rich titanium material |
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| CN103834798A CN103834798A (en) | 2014-06-04 |
| CN103834798B true CN103834798B (en) | 2015-11-18 |
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| CN111705227B (en) * | 2020-06-29 | 2022-03-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for smelting titanium slag by two-step method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134730A (en) * | 1993-09-07 | 1996-10-30 | 技术资源有限公司 | Upgrading titaniferous materials |
| CN102787194A (en) * | 2012-08-27 | 2012-11-21 | 攀枝花学院 | Method for preparing titanium-rich material by directly reducing molten slag from vanadium-titanium-ferrum concentrate |
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- 2012-11-26 CN CN201210483809.5A patent/CN103834798B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134730A (en) * | 1993-09-07 | 1996-10-30 | 技术资源有限公司 | Upgrading titaniferous materials |
| CN102787194A (en) * | 2012-08-27 | 2012-11-21 | 攀枝花学院 | Method for preparing titanium-rich material by directly reducing molten slag from vanadium-titanium-ferrum concentrate |
Non-Patent Citations (2)
| Title |
|---|
| 电炉钛渣碱浸除硅、铝与碱浸渣的预氧化焙烧动力学;路辉等;《过程工程学报》;20100630;第10卷(第3期);第513-521页 * |
| 电炉钛渣碱浸除硅、铝机理研究;路辉等;《轻金属》;20101231(第7期);第53-57页 * |
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