CN101638719A - Method for producing synthetic rutile by wet process - Google Patents
Method for producing synthetic rutile by wet process Download PDFInfo
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- CN101638719A CN101638719A CN200910169506A CN200910169506A CN101638719A CN 101638719 A CN101638719 A CN 101638719A CN 200910169506 A CN200910169506 A CN 200910169506A CN 200910169506 A CN200910169506 A CN 200910169506A CN 101638719 A CN101638719 A CN 101638719A
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- hydrochloric acid
- leaching
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- ilmenite concentrate
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Abstract
A method for producing artificial rutile by a wet method relates to a method for preparing the artificial rutile by using titanium concentrate as a raw material and leaching in a hydrochloric acid medium. The method is characterized by comprising the following steps: (1) finely grinding the titanium concentrate to be less than 0.15mm, wherein more than 70% of the titanium concentrate is less than 0.074 mm; (2) under the condition of normal pressure, performing multistage countercurrent leaching by using a hydrochloric acid solution with the mass concentration of 15-25%, wherein the dosage of hydrochloric acid is that the volume ratio of the hydrochloric acid solution to the titanium concentrate is 1: 1-8: 1, the leaching temperature is 70-105 ℃, and the leaching time of each stage is 0.5-4 h; (3) and filtering and washing the last-stage leached ore pulp, drying and calcining a filter cake to obtain the artificial rutile powder. The method of the invention uses hydrochloric acid with strong impurity removal capacity as a leaching agent, and iron, calcium, magnesium and other impurities enter a solution in the form of chloride through multi-stage countercurrent leaching, thereby achieving the purpose of mixing with TiO2And separating to prepare high-grade synthetic rutile. Titanium ore suitable for use in the present invention includes titanium concentrates of the type of rock ore and placer ore. The method has simple process and equipment, high removal rate of non-iron impurities such as calcium, magnesium and the like, low concentration of leached initial hydrochloric acid and contribution to linking of a hydrochloric acid regeneration system and recycling of regenerated acid.
Description
Technical field
The method of method for producing synthetic rutile by wet, relating to a kind of is raw material with the ilmenite concentrate, leaches the method for preparing artificial rutile in hydrochloric acid medium.
Background technology
Along with the natural rutile resource is petered out, titanium resource will rely on ilmenite concentrate more.Ilmenite concentrate (FeTiO
3) being divided into rock ore deposit and placer two classes, the theory of ilmenite concentrate contains TiO
2Amount is 52.63%.The ilmenite concentrate TiO that from placer, selects
2Content is generally 50-64%, and the ilmenite concentrate TiO that from the rock ore deposit, selects
2Content is generally 42-48%.Because the ilmenite concentrate grade is low, contains a large amount of iron, when being directly used in Producing Titanium Dioxide, " three wastes " amount is big, production cost is high, by producing 1t titanium white, FeSO
4Be 3-4t, dilute sulphuric acid is 8-10t, and environmental protection pressure is big.Thereby usually need the impurity in the concentrated ilmenite is removed by chemical method further the separation, to obtain TiO
2Higher " the rich titanium material " of content is as the raw material of titanium industry.
People's titanium material package of getting rich is drawn together titanium slag and artificial rutile, and conventional at present rich titanium material production method is that electrosmelting is produced titanium slag.There is abundant titanium resource in China's Flos Bombacis Malabarici-area, Xichang, belongs to the ilmenite concentrate of the high ore type of calcium-magnesium content, and the ilmenite concentrate grade that obtains after ore dressing is low, calcium magnesium addition content height, and MgO and CaO total content reach 5-7%, even higher.Utilize the melting of this kind ilmenite concentrate, be difficult to remove detrimental impurity such as calcium, magnesium, aluminium, can only obtain low-grade titanium slag, titanium slag titanium oxide content TiO
2Content only about 80%, calcic magnesium about 5%, iron about 6% can not can only be used for sulfate process titanium dioxide production at present as the raw materials for production of titanium white chloride and titanium sponge, and product is lacked competitiveness.
Method for producing synthetic rutile by wet is the rich titanium material production technology of new development.Reduction bubble method, direct sulfuric acid leaching can be removed the iron contamination in the ilmenite concentrate, but be difficult to remove non-iron contaminations such as calcium, magnesium.And the ability of salt acid leaching process removal impurity is strong, but the high-grade artificial rutile of output, and directly hydrochloric acid divides normal pressure to leach and the pressurization leaching.The equipment corrosion that the hydrochloric acid pressurization is leached is serious, and directly the leaching of normal pressure hydrochloric acid requires to adopt concentrated hydrochloric acid could obtain high-quality rutile, the hydrochloric acid normal pressure directly leaches the Panxi Diqu ilmenite concentrate and prepares artificial rutile " (" non-ferrous metal " 2007 the 59th the 4th phase of volume; 108-111 page or leaf) point out; and the optimum acidity that one section normal pressure leaches is 30% hydrochloric acid; and the regenerating acid concentration of regeneration of hydrochloric acid technology only can reach about 20%; therefore, the reprocessing cycle of hydrochloric acid becomes the difficult problem of normal pressure extract technology.
Summary of the invention
Purpose of the present invention is exactly in order to overcome the deficiency that above-mentioned prior art exists, and providing a kind of is raw material with the ilmenite concentrate, and technology and equipment are simple, and non-iron contaminations such as calcium magnesium are removed the rate height, the TiO of artificial rutile
2The content height, it is lower to leach concentration of hydrochloric acid, is convenient to and being connected and the method for the method for producing synthetic rutile by wet of the recycle of regenerating acid of regeneration of hydrochloric acid system.
The present invention seeks to be achieved through the following technical solutions.
The method of method for producing synthetic rutile by wet is characterized in that the step of its process comprises:
(1) ilmenite concentrate is finely ground to below the 0.15mm, wherein more than 70% less than 0.074mm;
(2) under condition of normal pressure, be that the hydrochloric acid soln of 15%-25% carries out multi-stage countercurrent and leaches with mass concentration, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 1: 1-8: 1, extraction temperature 70-105 ℃, every grade of extraction time 0.5-4h;
(3) with the leaching slurry filtration washing of last one-level, filtration cakes torrefaction, calcining obtain the artificial rutile powder.
The method of method for producing synthetic rutile by wet of the present invention is characterized in that ilmenite concentrate is finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm.
The method of method for producing synthetic rutile by wet of the present invention is characterized in that with mass concentration being that the hydrochloric acid soln of 18%-22% carries out multi-stage countercurrent and leaches.
The method of method for producing synthetic rutile by wet of the present invention, it is characterized in that carrying out the leaching progression that multi-stage countercurrent leaches is the 2-4 level.
The method of method for producing synthetic rutile by wet of the present invention is characterized in that the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 3: 1-6: 1.
The method of method for producing synthetic rutile by wet of the present invention is characterized in that extraction temperature is 85-95 ℃.
The method of method for producing synthetic rutile by wet of the present invention is characterized in that every grade of extraction time 0.5-2h.
The method of method for producing synthetic rutile by wet of the present invention is characterized in that hydrochloric acid soln is a regeneration hydrochloric acid, can also be to be disposed by technical hydrochloric acid.
Method of the present invention utilizes hydrochloric acid to strong characteristics of non-ferrous metal impurity stripping capacity such as iron and calcium magnesium, ilmenite concentrate is carried out normal pressure leach removing the foreign metal in the ilmenite concentrate, thereby obtain high-grade artificial rutile.In theory, concentration of hydrochloric acid is high more, its ability of removing metallic impurity is strong more, but the regeneration of hydrochloric acid technology of industrial application is subjected to the restriction of hydrochloric acid azeotropic point at present, the concentration of regeneration hydrochloric acid generally is no more than 22%, therefore ilmenite concentrate leaches when producing artificial rutile, should adopt the hydrochloric acid soln of low concentration to leach as far as possible, is beneficial to regeneration of hydrochloric acid and circulation.
Method of the present invention adopts multi-stage countercurrent to leach mode to reduce the requirement of leaching concentration of hydrochloric acid solution, is implemented under the condition of normal pressure, and the hydrochloric acid of employing low concentration leaches produces artificial rutile, and technology is simple, and leaching plant and material solve easily, and product TiO
2The content height is beneficial to the regeneration and the circulation of hydrochloric acid.
Description of drawings
Fig. 1 is the principle process flow sheet (leaching with three stage countercurrents is example) of the method for the invention.
Embodiment
The method of method for producing synthetic rutile by wet is finely ground to ilmenite concentrate below the 0.15mm, wherein more than 70% less than 0.074mm; Ilmenite concentrate mass concentration after the fine grinding is that the hydrochloric acid soln of 15%-25% is under condition of normal pressure, carrying out multi-stage countercurrent leaches, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 1: 1-8: 1, and extraction temperature 70-105 ℃, every grade of extraction time 0.5-4h; Every grade of ore pulp that comes out carries out solid-liquid separation by dense or filtration, and the solution of separating is as the leach liquor of upper level, and slag is as the leaching raw material of next stage.The solution that comes out from first step leaching solid-liquid separation on ore pulp is the spent acid of iron content, calcium, magnesium etc., through regeneration of hydrochloric acid technology regeneration hydrochloric acid, regeneration hydrochloric acid is used for the leaching agent of last step, thereby realize the regeneration and the circulation of hydrochloric acid, consider the hydrochloric acid cyclic utilization rate, replenish some technical hydrochloric acids in right amount according to the consumption situation when in the end one-level leaches.Leach the slag that solid-liquid separation on ore pulp is come out from last step,, make the artificial rutile powder through washing, dry, calcining.
With following indefiniteness embodiment method of the present invention is further described, helping understanding content of the present invention and advantage thereof, and as the qualification to protection domain of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
Get TiO
2The ore type ilmenite concentrate 100g of content 47.74%, be finely ground to below the 0.15mm, wherein more than 70% less than 0.074mm, adopt the hydrochloric acid soln of mass concentration 18% to carry out the leaching of three stage countercurrents, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 6: 1,95 ℃ of temperature, every grade of extraction time 0.5h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 92.15%.
Embodiment 2
Get TiO
2The ore type ilmenite concentrate 100g of content 47.74%, be finely ground to below the 0.15mm, wherein more than 70% less than 0.074mm, adopt the hydrochloric acid soln of mass concentration 15% to carry out the leaching of three stage countercurrents, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 1: 1,90 ℃ of temperature, every grade of extraction time 4h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 85.78%.
Embodiment 3
Get TiO
2The ore type ilmenite concentrate 100g of content 47.74%, be finely ground to below the 0.15mm, wherein more than 70% less than 0.074mm, adopt the hydrochloric acid soln of mass concentration 18% to carry out the leaching of three stage countercurrents, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 8: 1,95 ℃ of temperature, every grade of extraction time 2h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 94.25%.
Embodiment 4
Get TiO
2The ore type ilmenite concentrate 100g of content 47.74%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 20% to carry out the four-stage counter-current leaching, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 3: 1,95 ℃ of temperature, every grade of extraction time 1h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 95.20%.
Embodiment 5
Get TiO
2The ore type ilmenite concentrate 100g of content 47.74%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 25% to carry out the four-stage counter-current leaching, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 3: 1,85 ℃ of temperature, every grade of extraction time 1h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 95.75%.
Embodiment 6
Get TiO
2The placer type ilmenite concentrate 100g of content 49.89%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 20% to carry out the leaching of three stage countercurrents, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 4: 1,90 ℃ of temperature, every grade of extraction time 1h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 94.80%.
Embodiment 7
Get TiO
2The placer type ilmenite concentrate 100g of content 49.89%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 18% to carry out the two-stage countercurrent leaching, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 4: 1,95 ℃ of temperature, every grade of extraction time 1h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 93.52%.
Embodiment 8
Get TiO
2The placer type ilmenite concentrate 100g of content 49.89%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 18% to carry out the two-stage countercurrent leaching, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 4: 1,70 ℃ of temperature, every grade of extraction time 1h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 91.52%.
Embodiment 9
Get TiO
2The placer type ilmenite concentrate 100g of content 49.89%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 22% to carry out the two-stage countercurrent leaching, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 4: 1,105 ℃ of temperature, every grade of extraction time 1h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 95.40%.
Embodiment 10
Get TiO
2The ore type ilmenite concentrate 100g of content 47.74%, be finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm, adopt the hydrochloric acid soln of mass concentration 18% to carry out the leaching of three stage countercurrents, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 6: 1,95 ℃ of temperature, every grade of extraction time 0.5h, leach slurry filtration, filter cake obtains artificial rutile powder, the TiO of artificial rutile powder through washing, drying, calcining
2Content 93.20%.
Claims (8)
1, the method for method for producing synthetic rutile by wet is characterized in that the step of its process comprises:
(1) ilmenite concentrate is finely ground to below the 0.15mm, wherein more than 70% less than 0.074mm;
(2) under condition of normal pressure, be that the hydrochloric acid soln of 15%-25% carries out multi-stage countercurrent and leaches with mass concentration, the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 1: 1-8: 1, extraction temperature 70-105 ℃, every grade of extraction time 0.5-4h;
(3) with the leaching slurry filtration washing of last one-level, filtration cakes torrefaction, calcining obtain the artificial rutile powder.
2, the method for method for producing synthetic rutile by wet according to claim 1 is characterized in that it being that ilmenite concentrate is finely ground to below the 0.1mm, wherein more than 90% less than 0.05mm.
3, the method for method for producing synthetic rutile by wet according to claim 1 is characterized in that being is that the hydrochloric acid soln of 18-22% carries out multi-stage countercurrent and leaches with mass concentration.
4, the method for method for producing synthetic rutile by wet according to claim 1, it is characterized in that carrying out the leaching progression that multi-stage countercurrent leaches is the 2-4 level.
5, the method for method for producing synthetic rutile by wet according to claim 1 is characterized in that the hydrochloric acid consumption is that hydrochloric acid soln volume and ilmenite concentrate mass ratio are 3: 1-6: 1.
6, the method for method for producing synthetic rutile by wet according to claim 1 is characterized in that extraction temperature is 85-95 ℃.
7, the method for method for producing synthetic rutile by wet according to claim 1 is characterized in that every grade of extraction time 0.5-2h.
8, the method for method for producing synthetic rutile by wet according to claim 1 is characterized in that hydrochloric acid soln is a regeneration hydrochloric acid, or the technical hydrochloric acid configuration.
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| CN200910169506A CN101638719A (en) | 2009-09-08 | 2009-09-08 | Method for producing synthetic rutile by wet process |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103276204A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院过程工程研究所 | Method for preparing titanium slag by wet-processing on vanadium-titanium magnetite concentrates |
| CN103352129A (en) * | 2013-06-17 | 2013-10-16 | 中国船舶重工集团公司第七二五研究所 | Method for improving quality of titanium concentrate |
| CN104451166A (en) * | 2014-12-31 | 2015-03-25 | 北京清大国华环保科技有限公司 | Method and device for recovering zinc and chrome in heavy metal sludge |
| CN106882839A (en) * | 2015-12-15 | 2017-06-23 | 北京矿冶研究总院 | Method for comprehensively utilizing titanium white waste acid |
| CN106882838A (en) * | 2015-12-15 | 2017-06-23 | 重钢西昌矿业有限公司 | Method for producing titanium dioxide by using waste acid self-circulation non-blast furnace titanium slag sulfuric acid method |
| EP3114244A4 (en) * | 2014-03-05 | 2017-11-08 | Kamaleddine, Fouad F. | The production of high-grade synthetic rutile from low-grade titanium-bearing ores |
| CN111979413A (en) * | 2019-05-22 | 2020-11-24 | 攀枝花驰瑞矿冶科技有限公司 | Production method of titanium-rich material |
| CN113604671A (en) * | 2021-07-30 | 2021-11-05 | 四川顺应动力电池材料有限公司 | Method for preparing high-purity titanium slag from high-calcium-magnesium titanium concentrate |
| CN113716604A (en) * | 2021-08-09 | 2021-11-30 | 武汉工程大学 | Artificial rutile and preparation method thereof |
| CN114426305A (en) * | 2020-10-29 | 2022-05-03 | 中国科学院过程工程研究所 | Method for preparing artificial rutile by modifying and leaching titanium concentrate containing calcium and magnesium |
-
2009
- 2009-09-08 CN CN200910169506A patent/CN101638719A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103276204B (en) * | 2013-05-17 | 2015-04-01 | 中国科学院过程工程研究所 | Method for preparing titanium slag by wet-processing on vanadium-titanium magnetite concentrates |
| CN103276204A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院过程工程研究所 | Method for preparing titanium slag by wet-processing on vanadium-titanium magnetite concentrates |
| CN103352129A (en) * | 2013-06-17 | 2013-10-16 | 中国船舶重工集团公司第七二五研究所 | Method for improving quality of titanium concentrate |
| EP3114244A4 (en) * | 2014-03-05 | 2017-11-08 | Kamaleddine, Fouad F. | The production of high-grade synthetic rutile from low-grade titanium-bearing ores |
| CN104451166A (en) * | 2014-12-31 | 2015-03-25 | 北京清大国华环保科技有限公司 | Method and device for recovering zinc and chrome in heavy metal sludge |
| CN106882839A (en) * | 2015-12-15 | 2017-06-23 | 北京矿冶研究总院 | Method for comprehensively utilizing titanium white waste acid |
| CN106882838A (en) * | 2015-12-15 | 2017-06-23 | 重钢西昌矿业有限公司 | Method for producing titanium dioxide by using waste acid self-circulation non-blast furnace titanium slag sulfuric acid method |
| CN106882839B (en) * | 2015-12-15 | 2018-08-14 | 北京矿冶研究总院 | Method for comprehensively utilizing titanium white waste acid |
| CN106882838B (en) * | 2015-12-15 | 2018-12-14 | 重钢西昌矿业有限公司 | Method for producing titanium dioxide by using waste acid self-circulation non-blast furnace titanium slag sulfuric acid method |
| CN111979413A (en) * | 2019-05-22 | 2020-11-24 | 攀枝花驰瑞矿冶科技有限公司 | Production method of titanium-rich material |
| CN114426305A (en) * | 2020-10-29 | 2022-05-03 | 中国科学院过程工程研究所 | Method for preparing artificial rutile by modifying and leaching titanium concentrate containing calcium and magnesium |
| CN113604671A (en) * | 2021-07-30 | 2021-11-05 | 四川顺应动力电池材料有限公司 | Method for preparing high-purity titanium slag from high-calcium-magnesium titanium concentrate |
| CN113716604A (en) * | 2021-08-09 | 2021-11-30 | 武汉工程大学 | Artificial rutile and preparation method thereof |
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