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Method for preparing high-grade artificial rutile from high-calcium and high-magnesium rock-mineral ilmenite

A technology of artificial rutile and ilmenite, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of equipment corrosion, difficult removal of calcium and magnesium, high energy consumption, and achieve the effect of mild reaction conditions

Inactive Publication Date: 2016-02-03
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain TiO 2 Artificial rutile with a content greater than 99.5%, but the obtained hydrolysis waste liquid contains a large amount of free sulfuric acid, sulfate of iron and magnesium, etc., which is difficult to handle
[0004] To sum up, at present, with Panxi ilmenite as raw material in my country, calcium and magnesium are difficult to remove no matter whether it is a single smelting method, corrosion method, or stone original method, and only low-grade titanium-rich materials or artificial rutile can be obtained. , while the hydrochloric acid method has high energy consumption and serious corrosion to equipment

Method used

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  • Method for preparing high-grade artificial rutile from high-calcium and high-magnesium rock-mineral ilmenite
  • Method for preparing high-grade artificial rutile from high-calcium and high-magnesium rock-mineral ilmenite

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Finely ground ilmenite concentrate below 50 μm with ammonium sulfate ((NH 4 ) 2 SO 4 ) are uniformly mixed, and the mass ratio of ilmenite concentrate and ammonium sulfate is controlled to be 1:14.

[0032] (2), put the mixture obtained in step (1) into the tube furnace, ° C / min heating up to 250 ° C and keep warm for 240min. After the reaction finished, continue to feed the material with 10 ° C / min rises to 430°C with the furnace and keeps the temperature for 240min. After the reaction was over, the material was taken out and cooled to room temperature naturally to obtain a massive solid.

[0033] (3), leaching the massive solid obtained in step (2) with water, and controlling the leaching temperature to 90 ° C The reaction time is 10 minutes, and the liquid-solid mass ratio is 3:1. After the reaction, the solution was cooled to room temperature and filtered to obtain a filter residue.

[0034] (4), the filter residue obtained in the step (3), is leached w...

Embodiment 2

[0037] (1) Finely ground ilmenite concentrate below 50 μm with ammonium sulfate ((NH 4 ) 2 SO 4 ) are uniformly mixed, and the mass ratio of ilmenite concentrate and ammonium sulfate is controlled to be 1:5.

[0038] (2), put the mixture obtained in step (1) into the tube furnace, ° C / min heat up to 360 ° C and keep warm for 120min. After the reaction finished, continue to feed the material with 10 ° C / min rises with the furnace to 560°C and keeps it warm for 120min. After the reaction was over, the material was taken out and cooled to room temperature naturally to obtain a massive solid.

[0039] (3), leaching the massive solid obtained in step (2) with water, controlling the leaching temperature to be 40 ° C The reaction time is 90 minutes, and the liquid-solid mass ratio is 15:1. After the reaction, the solution was cooled to room temperature and filtered to obtain a filter residue.

[0040] (4), leaching the filter residue obtained in step (3) with a mass fraction...

Embodiment 3

[0043] (1) Finely ground ilmenite concentrate below 50 μm with ammonium sulfate ((NH 4 ) 2 SO 4 ) are uniformly mixed, and the mass ratio of ilmenite concentrate and ammonium sulfate is controlled to be 1:20.

[0044] (2), put the mixture obtained in step (1) into the tube furnace, ° C / min heat up to 420 ° C and keep warm for 60min. After the reaction finished, continue to feed the material with 10 ° C / min rises with the furnace to 650°C and keeps it warm for 60 minutes. After the reaction was over, the material was taken out and cooled to room temperature naturally to obtain a massive solid.

[0045] (3), leaching the massive solid obtained in step (2) with water, controlling the leaching temperature to be 40 ° C The reaction time is 50 minutes, and the liquid-solid mass ratio is 10:1. After the reaction, the solution was cooled to room temperature and filtered to obtain a filter residue.

[0046] (4), leaching the filter residue obtained in step (3) with a mass frac...

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Abstract

The invention discloses a method for preparing high-grade artificial rutile from high-calcium and high-magnesium rock-mineral ilmenite. The method comprises the following steps: step 1, sulfating and decomposing ilmenite at low temperature and converting titanium, iron, calcium, magnesium and other metal components into corresponding sulfates; step 2, selectively decomposing solid products obtained in the step 1 at moderate temperature to enable TiOSO4 to be resolved into water-insoluble TiO2, (NH4)2Fe(SO4)2 to be resolved into soluble FeSO4 and Fe2(SO4)3 and CaSO4, MgSO4, FeSO4, Fe2(SO4)3 and the like to be not resolved or almost not resolved; step 3, immersing a roasted product obtained in the step 2 with water to enable sulfates of soluble iron, calcium and magnesium to be dissolved so as to effectively separate TiO2 from other metal components to obtain titanium slag; step 4, adopting diluted hydrochloric acid to leach titanium slag in the step III so as to remove insoluble iron oxides generated by decomposition of a small quantity of FeSO2 and Fe2(SO4)3 in the moderate-temperature roasting process; step 5, performing alkaline treatment on the titanium slag obtained in the step 4 to remove acid-insoluble SiO2 in titanium slag; step 6, calcining and transforming the titanium slag obtained in the step 5 to obtain rutile titanium dioxide slag (artificial rutile).

Description

technical field [0001] The invention belongs to the technical field of chemical metallurgy, and mainly relates to a method for preparing artificial rutile from ilmenite, in particular to a method for preparing high-grade artificial rutile from rock ore-type ilmenite with high calcium and magnesium content. Background technique [0002] At present, the production methods of titanium dioxide are mainly sulfuric acid method and chlorination method. The sulfuric acid method can use low-grade ilmenite as raw material, but the process is long, the production process is discontinuous, the equipment is huge, and the amount of "three wastes" is large, which has caused serious environmental problems. At present, about 60% of titanium dioxide in the world is produced by the chlorination process. The chlorination process has the advantages of short process, low cost, and high product quality, but the chlorination process requires high-grade rutile as raw material. The global natural ru...

Claims

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Application Information

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IPC IPC(8): C01G23/053
Inventor 李春刘维燥梁斌
Owner SICHUAN UNIV
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