Method for producing lithium carbonate by leaching spodumene with nitric acid

A technology of lithium carbonate and nitric acid, applied in the direction of lithium carbonate;/acid carbonate, process efficiency improvement, etc., can solve the problems of low comprehensive utilization rate of auxiliary materials, low lithium recovery rate, and inability to recycle, etc. To achieve the effect of increasing the comprehensive utilization rate, being environmentally friendly and improving the complex process

Pending Publication Date: 2022-08-05
四川顺应锂材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of this method is that the recovery rate of lithium is not high and other rare metals cannot be recovered, and the auxiliary materials for leaching spodumene cannot be recycled, the comprehensive utilization rate of auxiliary materials is low, the production cost is high, and the amount of slag produced is very large

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  • Method for producing lithium carbonate by leaching spodumene with nitric acid
  • Method for producing lithium carbonate by leaching spodumene with nitric acid

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Experimental program
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Effect test

Embodiment 1

[0049] like figure 1 Shown, is the process flow diagram of the method for producing lithium carbonate by leaching spodumene nitric acid of the present invention; the detailed steps of the method for producing lithium carbonate by leaching spodumene nitric acid of the present invention are as follows:

[0050] A method for producing lithium carbonate by leaching spodumene (containing raw ore) with nitric acid specifically comprises the following steps:

[0051] Step 1: calcining spodumene (containing raw ore) at 1000° C. for 3 hours, and ball-milling the spodumene (containing raw ore) after calcination, and the average particle size of spodumene (containing raw ore) after ball milling is less than 48 μm.

[0052] Step 2: Slurry the pretreated spodumene (containing raw ore) in step 1 and water at a liquid-solid mass ratio of 2.5:1, and the slurry is subjected to secondary reverse leaching of nitric acid. 120wt%, the amount of nitric acid used in the secondary leaching of nitric a...

Embodiment 2

[0059] A method of leaching spodumene (containing raw ore) with nitric acid to produce lithium carbonate is implemented by the method described in Example 1, and the difference is:

[0060] In the step 1, the calcination temperature is 1050°C, and the calcination time is 2h.

[0061] Step 2: Slurry the pretreated spodumene (containing raw ore) in step 1 and water at a liquid-solid mass ratio of 3:1, and the slurry is subjected to secondary reverse leaching of nitric acid, wherein the amount of nitric acid in the primary leaching of nitric acid is the theoretical amount. 150wt%, the amount of nitric acid in the secondary leaching of nitric acid is 30wt% of the theoretical amount, the reaction temperature of the primary leaching and the reaction temperature of the secondary leaching are 150 ℃, and the reaction time of the primary leaching and the secondary leaching are 3h respectively.

[0062] In the described step 4, the extractant used is 4-tert-butyl-2-(α-methylbenzyl)phenol...

Embodiment 3

[0067] A method of leaching spodumene (containing raw ore) with nitric acid to produce lithium carbonate is implemented by the method described in Example 1, and the difference is:

[0068] In the step 1, the calcination temperature is 1100°C, and the calcination time is 1.5h.

[0069] Step 2: Slurry the pretreated spodumene (containing raw ore) in step 1 and water at a liquid-solid mass ratio of 3:1, and the slurry is subjected to secondary reverse leaching of nitric acid, wherein the amount of nitric acid in the primary leaching of nitric acid is the theoretical amount. 145%, the amount of nitric acid in the secondary leaching of nitric acid is 40% of the theoretical amount, the reaction temperature of the primary leaching and the reaction temperature of the secondary leaching are 170 °C, and the reaction time of the primary leaching and the secondary leaching are 2.5h respectively.

[0070] In the step 5, the crystallization temperature is 30°C.

[0071] The Li finally pre...

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Abstract

The invention discloses a method for producing lithium carbonate by leaching lepidolite with nitric acid. The method comprises the following steps: calcining and ball-milling spodumene; water is added for pulping, nitric acid is added into the pulp for nitric acid secondary reverse leaching, and leaching liquid and leaching residues are obtained; adjusting the pH value of the leachate; monovalent ionic liquid and non-monovalent element compound precipitates are obtained; extracting rubidium and cesium salts and a solution after the rubidium and cesium salts are extracted from the monovalent ionic liquid by adopting an extracting agent and a diluting agent; crystallizing and separating the solution from which the rubidium salt and the cesium salt are extracted, and performing membrane treatment on the crystallized solution to obtain a mixture of HNO3, LiOH and NaOH; and crystallizing the LiOH and NaOH mixture to separate out a LiOH product, carbonizing the crystallized mother liquor 1 to generate a Li2CO3 product, and recycling the carbonized mother liquor 2. According to the method, potassium, rubidium, cesium, sodium and leaching residues are recycled while lithium is extracted, the comprehensive utilization rate of lithium ore is increased, complexity of a traditional production process is simplified, the process production cost is reduced, the added value of products is increased, and maximum resource utilization is achieved.

Description

technical field [0001] The invention belongs to the technical field of battery-grade lithium carbonate preparation, and relates to a method for producing lithium carbonate by leaching spodumene with nitric acid. Background technique [0002] As the lightest and least dense metal, lithium has unique physical and chemical properties, known as "industrial monosodium glutamate", and has its presence in various traditional industrial fields. With the development of the new energy industry, the demand for lithium batteries is huge, and lithium is also known as the "energy metal" of the 21st century. Lithium resources are widely used in glass and ceramic manufacturing, alloy and primary aluminum production, lithium battery production, pharmaceuticals and optical materials and other industries. In addition, they are also used in military and nuclear industries. As an important supporting mineral for the development of strategic emerging industries, lithium is regarded as a new econ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/06C22B3/26C22B3/44C22B26/10C22B26/12C01D15/08
CPCC22B3/065C22B26/10C22B26/12C22B3/44C22B3/262C01D15/08C01P2006/80Y02P10/20
Inventor 赵林何永但勇赵澎刘芸秀宋世杰袁利梅
Owner 四川顺应锂材料科技有限公司
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