Method for preparing lithium carbonate through two-stage conversion of lithium ore

A lithium ore and lithium carbonate technology, applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of low lithium leaching rate, difficult decomposition of lithium ore, and low recovery rate

Inactive Publication Date: 2017-08-25
BEIJING GENERAL RES INST OF MINING & METALLURGY
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the difficulties in lithium ore decomposition, low lithium leaching rate, and complex purification process and low recovery rate of lithium solution due to the high content of impurities such as aluminum and iron in the leaching solution in the existing lithium ore extraction lithium technology. , to provide a method for producing lithium carbonate from lithium ore by adopting two-stage conversion methods of low-temperature sulfate roasting and medium-temperature reduction roasting, that is, first mixing concentrated sulfuric acid with lithium ore powder and then performing sulfuric acid aging reaction at 150-400 °C, Convert the lithium in the lithium ore into lithium sulfate with good water solubility, and at the same time convert the fluorine into hydrogen fluoride gas to remove, and complete the first stage of conversion; , aluminum and other sulfates are converted into water-insoluble alumina and iron oxide, and the sulfur-containing roasting flue gas is used to make acid to complete the second stage of conversion; the reduced calcined sand is leached with water to extract lithium, while impurities such as aluminum, iron, and calcium are removed Leave it in the leaching slag, and filter it with water leaching pulp to directly obtain a relatively pure lithium sulfate solution, which not only realizes the separation of lithium, aluminum, and iron during the leaching process, but also reduces the flue gas obtained by roasting to sulfur dioxide flue gas, which is convenient for acid production. Sulfuric acid regeneration cycle reduces the consumption of chemicals such as sulfuric acid and neutralization alkali

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  • Method for preparing lithium carbonate through two-stage conversion of lithium ore

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Experimental program
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Effect test

Embodiment 1

[0033] Mix 100g of mixed lithium concentrate powder with 95% concentrated sulfuric acid to obtain a mixture. The amount of concentrated sulfuric acid added is 1.5 times the theoretical amount of sulfuric acid required. The mixture is aged and roasted at 300°C for 2 hours, and the obtained clinker is crushed. Mix it with coal powder, and then reduce and roast at 900°C for 30 minutes. The amount of coal powder added is twice the amount of theoretical coal powder required for the complete reduction and decomposition of aluminum sulfate and iron sulfate in the clinker; The amount is added according to the leaching solid-liquid mass ratio of 1:3, the leaching temperature is 50°C, and the leaching time is 30 minutes, then filtered to obtain a lithium-containing leaching solution, the pH value of the leaching solution is adjusted to 11 with sodium hydroxide, and filtering is obtained. The obtained filtrate is precipitated with sodium carbonate to obtain lithium carbonate.

Embodiment 2

[0035]Take 100g lepidolite ore powder and mix with 90% concentrated sulfuric acid to obtain a mixture. The amount of concentrated sulfuric acid added is twice the theoretical amount of sulfuric acid required. The mixture is matured and roasted at 250°C for 2 hours. The obtained matured material is crushed and mixed with Coal powder is mixed, and then reduced and roasted at 600°C for 1 hour. The amount of coal powder added is twice the amount of theoretical coal powder required for the complete reduction and decomposition of aluminum sulfate and ferric sulfate in the clinker; Add according to the leaching solid-liquid mass ratio of 1:2, the leaching temperature is 90°C, the leaching time is 30min, and then filter to obtain the lithium-containing leaching solution; adjust the pH value of the leaching solution to 11 with sodium hydroxide, filter, and the obtained filtrate is precipitated with sodium carbonate to obtain carbonic acid lithium.

Embodiment 3

[0037] Mix 100g of spodumene concentrate powder with 95% concentrated sulfuric acid to obtain a mixture. The amount of concentrated sulfuric acid added is twice the theoretical amount of sulfuric acid required. The mixture is matured and roasted at 250°C for 2 hours, and the obtained matured material is crushed After that, it is mixed with coal powder, and then reduced and roasted at 600°C for 1 hour. The amount of coal powder added is twice the amount of theoretical coal powder required for the complete reduction and decomposition of aluminum sulfate and iron sulfate in the clinker; The amount to be added is added according to the leaching solid-to-liquid mass ratio of 1:3, the leaching temperature is 50°C, and the leaching time is 30 minutes, and then filtered to obtain a lithium-containing leaching solution; the pH value of the leaching solution is adjusted to 11 with sodium hydroxide, and filtered, and the obtained filtrate is precipitated with sodium carbonate Lithium carb...

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Abstract

The invention discloses a method for preparing lithium carbonate through two-stage conversion of lithium ore and belongs to the technical field of lithium metallurgy. The method comprises the steps: mixing lithium ore powder and concentrated sulfuric acid, performing low-temperature sulfation calcination under condition of 150 to 400 DEG C to convert lithium in the lithium ore into lithium sulfate with good water solubility and meanwhile converting fluorine into hydrogen fluoride gas to be removed to finish first-stage conversion; then performing medium-temperature reduction calcinations on a clinker under 550 to 900 DEG C to convert sulfate of iron, aluminum and the like into aluminum oxide and ferric oxide, which are difficult to dissolve in water, in the clinker to finish second-stage conversion, wherein generated sulfur dioxide flue gas can be used for preparing acid; soaking reduced calcine with water to extract lithium, leaving impurities of iron, aluminum and the like in leaching residues and filtering water-soaked ore pulp to directly obtain a purer lithium sulfate solution. The method not only achieves separation of the lithium from the aluminum and the iron in a leaching process, but also achieves regeneration cycle of sulfuric acid, reduces consumption of chemicals of sulfuric acid, neutralizing alkali and the like and has high lithium recovery rate.

Description

technical field [0001] The invention belongs to the field of lithium metallurgy, and relates to a method for extracting lithium from ore, in particular to a method for preparing lithium carbonate from lithium ore through two-stage conversion of low-temperature sulfation roasting and medium-temperature reduction roasting. Background technique [0002] Lithium is mainly used in industrial fields such as atomic reactors, light alloys and batteries, especially for the development of new energy industries such as lithium batteries and nuclear power. Lithium extraction raw materials mainly include lithium ore and salt lake brine. Due to the simple process of extracting lithium from salt lake brine, low energy consumption and low cost, salt lake brine has become the main raw material for lithium salt production abroad. Although my country is rich in salt lake resources, because most of the domestic salt lake brine has the characteristics of high magnesium-lithium ratio, it is diff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
CPCC01D15/08
Inventor 蒋训雄冯林永范艳青汪胜东靳冉公蒋伟张登高
Owner BEIJING GENERAL RES INST OF MINING & METALLURGY
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