Method for converting rubdium and cesium in spodumene lithium-extracted slag into soluble salt

A spodumene, lithium slag technology, applied in chemical instruments and methods, rubidium/cesium/francium compounds, inorganic chemistry, etc. Loss of waste and other problems, to achieve the effect of low resource content, low acid and alkali consumption, and large processing capacity

Active Publication Date: 2016-01-27
天齐锂业(江苏)有限公司 +2
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  • Application Information

AI Technical Summary

Problems solved by technology

Spodumene slag is usually treated as cheap building slag, resulting in the loss and waste of precious rubidium and cesium resources
[0010] The inventor of the present invention has tried many methods to convert the rubidium and cesium in the waste residue after lithium extraction into soluble salts, such as directly soaking the slag with high-concentration sulfuric acid (55%) for 8 hours, and the leaching rate of rubidium and cesium is low 40%; in the spodumene conversion roasting process, the temperature is appropriately raised or lowered, and the conversion rate of rubidium and cesium in a certain temperature range decreases with the increase of temperature, but the highest conversion rate is still lower than 40%; the slag or Roasting material adopts sodium sulfate pressure cooking method and adds additives, the conversion rate of rubidium and cesium is lower than 15%; the slag is mixed with sodium sulfate and roasted, the conversion rate of rubidium and cesium is lower than 20%; the slag is added with concentrated sulfuric acid for repeated acidification at 300°C , the conversion rate of rubidium and cesium is lower than 10%; the slag is mixed with sodium hydroxide and roasted, and the conversion rate of rubidium and cesium can reach 70%, but the roasted product is in the form of molten salt, which is difficult for large-scale production
[0011] The method for further extracting rubidium and cesium from the slag after extracting lithium from spodumene has not been reported yet.

Method used

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  • Method for converting rubdium and cesium in spodumene lithium-extracted slag into soluble salt
  • Method for converting rubdium and cesium in spodumene lithium-extracted slag into soluble salt
  • Method for converting rubdium and cesium in spodumene lithium-extracted slag into soluble salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Weigh 2000g of slag after lithium extraction, add 300g of sodium chloride, 700g of calcium chloride, and 100g of calcium oxide and mix well.

[0057] The slag data is as follows (the same below):

[0058] Table 1

[0059] Li 2 o

Rb

Cs

K

Na

Ca

0.31％

0.11％

0.035％

0.44％

0.1％

2.31％

[0060] (2) Place the mixed material obtained in step (1) in a small-sized rotary kiln at a temperature of 800° C. and a roasting time of 60 minutes. After cooling, take it out to obtain a roasted material.

[0061] (3) Transfer the calcined material obtained in step (2) to a beaker, add 2480 mL of water, and stir at room temperature for 30 minutes to obtain a slurry.

[0062] (4) Pass the slurry obtained in step (3) through a plate frame for solid-liquid separation, and wash with water 3 times. The solid residue was dried at 105°C. The filtrate and washing water are stored separately, the filtrate enters the next step, and...

Embodiment 2

[0069] (1) Weigh 2000g of slag after lithium extraction, add 700g of sodium chloride, 1300g of calcium chloride, and 100g of calcium oxide, and mix well.

[0070] (2) Put the mixed material obtained in step (1) in a small-sized rotary kiln, bake at 950° C. for 60 minutes, take it out after cooling, and obtain the roasted material.

[0071] (3) Transfer the calcined material obtained in step (2) to a beaker, add 4920 mL of water, and stir at room temperature for 30 minutes to obtain a slurry.

[0072] (4) Pass the slurry obtained in step (3) through a plate frame for solid-liquid separation, and wash with water 3 times. The solid residue was dried at 105°C. The filtrate and washing water are stored separately, the filtrate enters the next step, and the washing water returns to step (3) for use as leaching water. Gained solid slag and filtrate data are as follows:

[0073] table 3

[0074]

[0075] (5) Adjust the pH value of the solution obtained in step (4) to 11-14 with...

Embodiment 3

[0079] (1) Weigh 5000g of slag after lithium extraction, add 3000g of calcium chloride and 200g of calcium oxide, and mix well.

[0080] (2) Put the mixed material obtained in step (1) in a small-sized rotary kiln, bake at 800° C. for 60 minutes, take it out after cooling, and obtain the roasted material.

[0081] (3) Transfer the calcined material obtained in step (2) to a container, add 8200 mL of water, and stir at room temperature for 60 minutes to obtain a slurry.

[0082] (4) Pass the slurry obtained in step (3) through a plate frame for solid-liquid separation, and wash with water 3 times. The solid residue was dried at 105°C. The filtrate and washing water are stored separately, the filtrate enters the next step, and the washing water returns to step (3) for use as leaching water. Gained solid slag and filtrate data are as follows:

[0083] Table 4

[0084]

[0085] (5) Adjust the pH value of the solution obtained in step (4) to 11-14 with NaOH, filter out the s...

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Abstract

The invention relates to a process for extracting rubdium and cesium from spodumene lithium-extracted slag and belongs to the technical field of rubdium and cesium extraction. The process specifically comprises the following steps of (1) adding a converting auxiliary material into slag generated after lithium is extracted from the spodumene, uniformly mixing the materials, and roasting the materials for 30 to 180 minutes at the temperature of 800 to 950 DEG C, wherein the converting auxiliary material is one of or a mixture of more of calcium chloride, sodium chloride, calcium oxide, sodium sulfate and potassium sulfate; (2) cooling the roasted materials obtained in the step (1), and leaching the roasted materials by taking water as an extracting agent; (3) performing solid and liquid separation on the mixed slurry formed after the leaching in the step (2), wherein the liquid phase of soluble rubdium and cesium salts can be subsequently gathered and separated. According to the method for extracting the rubdium and cesium from a rubidium, cesium and silicon aluminate skeleton structure provided by the invention, the rubdium and cesium can be extracted from high-grade ore, and the rubdium and cesium can also be extracted from low-grade ore and slag. The extraction rate of the rubidium can reach up to 98 percent, and the extraction rate of the cesium can reach up to 99 percent.

Description

technical field [0001] The invention relates to a process for extracting rubidium and cesium from spodumene lithium extraction slag, which is suitable for extracting rubidium and cesium from spodumene lithium extraction slag, and also suitable for extracting rubidium and cesium from minerals with aluminosilicate skeleton molecular structure rubidium cesium. Background technique [0002] Rubidium and cesium have a unique photoelectric effect. Among all metal elements, the photoelectric valve is the largest, and the work function of electrons is the smallest. From visible light to infrared spectral lines and ultraviolet spectral lines, ionization and emission of electrons can be effectively observed. The excellent photoelectric properties and chemical activity of rubidium and cesium have applications that cannot be replaced by other metal elements in various technical fields. [0003] Recently, the industrial applications of rubidium and cesium in the world are mainly in high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D17/00
Inventor 邓红云严新星涂明江曹乃珍高洁姚丽陶帅李仕红
Owner 天齐锂业(江苏)有限公司
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