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Method for preparing high pure scandium oxide from hydrochloric acid mother liquid for producing zirconium oxychloride

A technology for producing zirconium oxychloride and scandium trioxide, which is applied in the field of preparation of high-purity scandium trioxide, can solve the problems of unqualified product quality, low total recovery rate of scandium, and large loss of organic phase, etc. It is easy to achieve process indicators The effect of control, easy equipment and small investment

Inactive Publication Date: 2014-12-24
ZIBO GUANGTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the long-term static phase separation is adopted, it is still difficult to complete the phase separation, and the entrainment is serious, resulting in a large loss of the organic phase and the product quality cannot meet the standard. Although the product is purified many times, it is still difficult to reach the standard. The main elements exceeding the standard are zirconium, hafnium, titanium, and thorium. , rare earth, etc.
During the purification process of scandium, the loss of scandium is serious, although the extraction rate is high, the total recovery rate of scandium is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The chemical composition of zirconium oxychloride hydrochloride mother liquor is shown in Table 1. We only tested the elements with relatively high content, and did not detect other trace elements, such as W and Se.

[0034] Table 1 Zirconium oxychloride hydrochloride mother liquor chemical composition

[0035] Element

[0036] Gd

[0037] (1) Extraction: the mother liquor of zirconium oxychloride hydrochloride is used in a mixing tank The baffleless self-flowing extraction tank is used for three-stage countercurrent extraction, and the extract is a mixture of 20% P204, 5% tributyl phosphate and 75% sulfonated kerosene by volume. The mixed extraction time is 10 minutes, the phase separation time is 50 minutes, compared with A / O=1:2, the raffinate is discharged, and the organic phase enters the next step. The organic phase is centrifuged at a speed of 2400r / min by a L350 centrifugal extractor to separate the aqueous phase and undergo demulsificatio...

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Abstract

The invention belongs to the field of wet metallurgy, and particularly relates to a method for preparing high pure scandium oxide from a hydrochloric acid mother liquid for producing zirconium oxychloride. The method comprises the following steps of (1) extracting the hydrochloric acid mother liquid, separating by centrifugation to remove water phase from an organic phase and for demulsification and washing with acid; (2) subjecting an organic phase loaded in the acid solution to reverse extraction and filtration, discharging the filtrate, dissolving filter residues with acid and extracting; (3) subjecting the organic phase to reverse extraction and filtration, discharging the filtrate, and dissolving the filter residues with acid; (4) regulating a pH value of the acid solution, adding oxalic acid to precipitate scandium, filtering, roasting the filter residues, then dissolving the roasted residues with acid and filtering; (5) regulating a pH value of the filtrate, adding oxalic acid to precipitate scandium again, filtering, roasting the filter residues again, boiling the roasted residues in an acid water, regulating the pH, filtering, washing with water, roasting and drying to obtain a product. The method is used for preparing the high pure scandium oxide from an acid liquid solution with complex components, and changes wastes into valuables. A separation technology employing a baffle-free type self-flow extraction tank, a variable frequency technique and a centrifugal extractor is used to solve technical problems of difficult phase separation and serious emulsification in the extraction technology, and conditions for recovering valuable metals from the complex material liquid are provided.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy, in particular to a method for preparing high-purity scandium trioxide from hydrochloric acid mother liquor for producing zirconium oxychloride. Background technique [0002] Adding sodium hydroxide to alkali-fused zircon sand, washing with water to remove silicon, adding hydrochloric acid to filter, and concentrating and crystallizing the filtrate to produce zirconium oxychloride products will produce a large amount of mother liquor of zirconium oxychloride hydrochloride. The content of scandium is generally 800-1200ppm, which is several orders of magnitude higher than the content of scandium in the waste acid of the titanium dioxide industry, but other harmful elements are also extremely high. The elements that seriously affect the quality of scandium include zirconium, hafnium, titanium, rare earth, Thorium et al. [0003] When the material liquid is neutralized with alkali, the yield of dry res...

Claims

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Application Information

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IPC IPC(8): C22B59/00C22B3/26C22B3/46
CPCY02P10/20
Inventor 刘其永杨秋良毕明亮杨光耀刘策
Owner ZIBO GUANGTONG CHEM
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