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A process for preparing artificial rutile by leaching ilmenite with hydrochloric acid

An artificial rutile and hydrochloric acid leaching technology, which is applied in the field of metallurgy, can solve problems such as complex process, lower product quality, and complicated side processes, and achieve the effects of fast leaching speed, reduced powder generation, and strong impurity removal ability

Active Publication Date: 2017-07-21
KUNMING METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among them, the reduction corrosion method is a method of selective iron removal. First, the iron oxide in the ilmenite is reduced to metallic iron in a solid state, and then the iron in the reduced ilmenite is rusted and separated by an aqueous electrolyte solution, so that TiO 2 Enrichment into artificial rutile, this method has the characteristics of uniform particle size, stable color, and easy treatment of "three wastes", but it is only suitable for processing high-grade ilmenite placer; the sulfuric acid method is mainly for reduction roasting of high-grade oxidized placer, after Concentration of 22-23% titanium white waste acid pressure leaching iron and other impurities in the dissolved ore, and then filter washing and calcination process, so that TiO 2 Enrichment, this method can not only remove iron in the ore, but also partially remove soluble impurities such as calcium, magnesium, aluminum and manganese, and can also use waste sulfuric acid from the sulfuric acid titanium dioxide production plant to reduce costs, but this method is only suitable for It is suitable for processing high-quality ilmenite concentrate. If the grade of ilmenite concentrate is low, the process will be complicated and the quality of the product will be reduced. At the same time, the amount of three wastes is large and the by-process is complicated.
The hydrochloric acid method uses hydrochloric acid pressure leaching, the leaching speed is fast, the impurity removal ability is strong, it can remove iron, calcium, magnesium, aluminum and manganese and other impurities, and can obtain high-grade artificial rutile. There is still no precedent for large-scale successful industrial application of artificial rutile prepared by leaching in my country. One of the main reasons is the problem of a large amount of pulverization of materials during the leaching process.

Method used

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  • A process for preparing artificial rutile by leaching ilmenite with hydrochloric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Such as figure 1 As shown, take 200 g of ilmenite, add 20 g of calcined petroleum coke as a reducing agent according to 10% by mass, mix well and add into a graphite crucible, and the graphite crucible is roasted in a closed atmosphere furnace at 900 ° C for 60 min; 150g of ilmenite was leached under pressure, the concentration of hydrochloric acid was 20%, the leaching temperature was 140°C, the liquid-solid ratio was 8:1, the stirring speed was 400r / min, and the leaching time was 6h. After leaching, it was filtered, and the filtrate was sampled and analyzed. HCl 138.7g / L, Fe in the filtrate T 37.14g / L, Fe 2+30.7g / L. After filtration, the filter residue was washed with dilute hydrochloric acid with a mass concentration of 1.8% until the filtrate was colorless, then dried at 78°C for 11 hours, and then calcined at 1000°C for 2 hours. 2 The content is 91.37%.

Embodiment 2

[0043] Such as figure 1 As shown, take 200 g of ilmenite, add 20 g of calcined petroleum coke as a reducing agent according to 10% by mass, mix well and add into a graphite crucible, and the graphite crucible is roasted at 900 ° C for 120 min in a closed atmosphere furnace; 150g of ilmenite was leached under pressure, the concentration of hydrochloric acid was 20%, the leaching temperature was 140°C, the liquid-solid ratio was 9:1, the leaching time was 8h, the stirring speed was 400r / min, after the leaching was completed, it was filtered, and the filtrate was sampled and analyzed. HCl 144.08g / L, Fe in the filtrate T 35.29g / L, Fe 2+ 28.72g / L. After filtration, the filter residue was washed with dilute hydrochloric acid with a mass concentration of 1.3% until the filtrate was colorless, then dried at 82°C for 10 hours, and then calcined at 1000°C for 2 hours. 2 The content is 93.24%.

Embodiment 3

[0045] Such as figure 1 As shown, take 200 g of ilmenite, add 20 g of calcined petroleum coke as a reducing agent according to 10% by mass, mix well and add into a graphite crucible, and the graphite crucible is roasted at 900 ° C for 120 min in a closed atmosphere furnace; 150g of ilmenite was leached under pressure, the concentration of hydrochloric acid was 24%, the leaching temperature was 140°C, the liquid-solid ratio was 9:1, the leaching time was 8 hours, the stirring speed was 400r / min, after the leaching was completed, it was filtered, and the filtrate was sampled and analyzed. HCl 165.71g / L, Fe in the filtrate T 36.72g / L, Fe 2+ 18.22g / L. After filtration, the filter residue was first dried at 85°C for 10h, and then calcined at 1000°C for 2h, the TiO in the obtained rutile 2 The content is 91.47%.

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Abstract

The invention relates to a process for making artificial rutile by leaching of mohsite hydrochloric acid and belongs to the technical field of metallurgy. The process includes using mohsite graded at 45-52% as raw materials, and distributing carbonaceous reducing agent for reducing roasting, pressure leaching, filtering, roasting, and regenerating of hydrochloric acid, so that impurity removal of mohsite and recycling of hydrochloric acid are effectively realized and artificial rutile is made. The process is characterized in that mohsite and carbonaceous reducing agent are uniformly mixed for reducing roasting, and leaching rate of impurities like silicon, iron, calcium and magnesium is increased; hydrochloric acid is regenerated by distilling leaching mother liquor and can be reused in leaching; filter slag can be roasted after pressurized leaching and filtering so as to obtain artificial rutile. The process has the advantages of high leaching speed, high impurity removal efficiency, high grade and recyclability of hydrochloric acid. In addition, the process is applicable to industrial production in the aspects of technique, equipment, economy and environment protection.

Description

technical field [0001] The invention belongs to the technical field of metallurgy, and in particular relates to a process for preparing artificial rutile by leaching ilmenite with hydrochloric acid. Background technique [0002] Rutile has excellent properties such as high temperature resistance, corrosion resistance, high strength and small specific gravity, and is widely used in aviation, aerospace, machinery, chemical industry, seawater desalination and other industries. At present, the annual production of rutile in my country is only tens of thousands of tons, while the demand has reached more than one million tons, and the supply is seriously in short supply. Therefore, most of the rutile raw materials depend on foreign imports, and the price is very expensive, which leads to domestic related enterprises in the international competition. at a disadvantage. With the depletion of natural rutile production, the available supply of high-grade natural rutile has declined sh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
Inventor 崔涛袁野和晓才彭建蓉谢刚李小英赖浚谢天鉴施辉献田林徐庆鑫许娜魏可柯浪徐俊毅
Owner KUNMING METALLURGY INST
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