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Method for removing calcium ions in sulfuric acid rare earth extraction separation process

A separation process, technology of rare earth sulfate, applied in the direction of improving process efficiency, etc., to achieve good calcium reduction effect, reduce calcium sulfate crystallization, and slow down the effect of calcium sulfate crystallization

Active Publication Date: 2020-07-14
甘肃稀土新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a method for removing calcium ions in the extraction and separation process of rare earth sulfate, so as to solve the problem that it is difficult to effectively prevent and remove calcium sulfate crystallization in the prior art

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  • Method for removing calcium ions in sulfuric acid rare earth extraction separation process
  • Method for removing calcium ions in sulfuric acid rare earth extraction separation process
  • Method for removing calcium ions in sulfuric acid rare earth extraction separation process

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Effect test

Embodiment 1

[0039] like figure 1 Be the technical process schematic diagram of the present invention, comprise the following steps:

[0040] Step 1: lead the aqueous phase of the high-calcium sulfate rare earth sulfate solution with a calcium content of 1.89 g / L at the highest concentration point of the extraction production line to the oil separation tank for oil separation. After the oil separation, the petroleum content of the high-calcium water phase is less than 30 ppm;

[0041] Step 2: Introduce people 100m into the decalcification tank 3 Add 5000kg of calcium sulfate active seed crystals to the high calcium sulfate rare earth solution after oil separation, start stirring, and react for 60 minutes;

[0042] Step 3: Introduce the slurry in the decalcification tank into a thickener and age for 60 minutes, and analyze the calcium content in the isolated rare earth sulfate solution, and the calcium content is 1.23g / L.

[0043] Step 4: The slurry at the bottom of the thickener is intro...

Embodiment 2

[0047] Influence of the amount of calcium sulfate active seed crystals on the calcium-lowering effect of lanthanum-cerium sulfate solution

[0048] Among them, the lanthanum cerium sulfate solution is produced on-site by the Gansu rare earth production line, the rare earth concentration is 8-10g / L, and the calcium ion concentration is 2-3g / L; the calcium sulfate seed is prepared by the reaction of concentrated sulfuric acid and calcium hydroxide slurry to ensure the pH of the reaction process The value is 6-7.

[0049] Take 500mL of lanthanum cerium sulfate solution and place it in a 1000mL beaker, weigh calcium sulfate seeds in different proportions and add them to the beaker, stir for 1h, let stand for 1h, analyze the supernatant calcium ion concentration (calcium oxide meter), see the experimental results figure 2 ,from figure 2 It can be seen that when calcium sulfate active seeds are added, regardless of the amount added, the concentration of calcium ions in the lantha...

Embodiment 3

[0051] Effect of Stirring Reaction Time on Calcium Removal Efficiency of Lanthanum-Cerium Sulfate Solution

[0052] Get 500mL of lanthanum cerium sulfate solution and place it in a 1000mL beaker, take by weighing 25g of calcium sulfate seed crystals by solid-to-liquid ratio 5%, add in the beaker, stir for different times, leave standstill for 1h, analyze the supernatant calcium ion concentration (calcium oxide meter), For specific data, see image 3 ,from image 3 It can be seen from the figure that when calcium sulfate seeds are added, the concentration of calcium ions in the lanthanum cerium sulfate solution decreases rapidly (within 1 h) to a certain extent, and remains almost unchanged with the prolongation of stirring time. At the beginning of crystallization, because the system has a large degree of supersaturation, it provides a strong driving force for crystallization, which makes the initial crystallization proceed explosively, as observed in the experiment. decreas...

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Abstract

The invention discloses a method for removing calcium ions in a sulfuric acid rare earth extraction separation process, and belongs to the field of hydrometallurgy. According to the method, a method for reducing calcium ions in rare earth feed liquid by utilizing calcium sulfate seed crystal to induce crystallization is adopted, oil separation treatment is carried out on an extraction production line high-calcium sulfuric acid rare earth solution, calcium sulfate active seed crystals are added according to a solid-to-liquid ratio (wt.%) of 3%-20%, reacting is carried out for 0.5-2.0 hours, aging is carried out for 0.5-2.0 hours, solid-liquid separation is realized, filter residues are removed, external calcium reduction is realized, after the calcium is reduced, the water phase of the sulfuric acid rare earth solution is added into low-calcium waste water, and further diluting is carried out until the calcium ion saturation solubility is lower than the calcium ion saturation solubility, thereby effectively reducing the crystallization of an extraction production line.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy, and in particular relates to a method for removing calcium ions in the extraction and separation process of rare earth sulfate. Background technique [0002] Calcium sulfate crystallization hazards are serious in the hydrometallurgical process. For the Baotou mixed rare earth mine with the largest reserves in the world, the common separation process is the third-generation sulfuric acid method patented technology smelting independently developed by Beijing Nonferrous Metals Research Institute. Baotou rare earth After the concentrated ore is roasted with concentrated sulfuric acid, soaked in water, and neutralized, the calcium element is mainly precipitated into the waste residue in the form of calcium sulfate, and a small part of the calcium element is dissolved in the rare earth sulfate solution in the form of calcium sulfate, and is in a supersaturated state. In the transformation process of rare...

Claims

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Application Information

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IPC IPC(8): C22B3/22C22B3/44C22B59/00
CPCC22B3/22C22B3/44C22B59/00Y02P10/20
Inventor 李虎平韩满璇王斌田斌胡广寿
Owner 甘肃稀土新材料股份有限公司
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