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Process for separating zirconium and hafnium by solvent extracting method

An extraction method and process technology, which is applied in the field of separation of zirconium and hafnium by solvent extraction, can solve the problems that the extraction operation is difficult to perform normally, the extraction capacity is small, and the separation factor is high, so as to avoid the accumulation of a large amount of chloride ions, the extraction process is stable, and the separation factor high effect

Active Publication Date: 2017-07-07
BEIJING RESEARCH INSTITUTE OF CHEMICAL ENGINEERING AND METALLURGY
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Problems solved by technology

Among them, the MIBK-HCNS extraction method has low hafnium content in zirconium, large extraction capacity, basically closed process, and mature technology, but the consumption of chemicals is high, and it is easy to decompose to produce poisonous gas, and the solubility of MIBK in water is as high as 0.20%, so the loss is serious, and there is still sewage Emissions and other issues, so the law has gradually been phased out
The advantages of the TOA extraction method are small pollution, simple equipment, and low investment costs, but the extraction capacity of this method is small, the separation factor is not high, and it is difficult to obtain high-purity zirconium and atomic-level hafnium
Tributyl Phosphate (TBP-HCl-HNO 3 ) method has high separation factor, less reagent input, and large extraction capacity, but the extraction stock solution used in this method has high acidity and is a mixed acid, and the emulsification phenomenon is serious during the operation process, which makes the extraction operation difficult to carry out normally, and limits the popularization and application of this process.

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  • Process for separating zirconium and hafnium by solvent extracting method
  • Process for separating zirconium and hafnium by solvent extracting method
  • Process for separating zirconium and hafnium by solvent extracting method

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Embodiment Construction

[0052] The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0053] Such as figure 1 Shown, a kind of solvent extraction method of the present invention separates zirconium and hafnium technology to be raw material with the hafnium-containing zirconyl chloride industrial product, prepare zirconium nitrate (hafnium) acid solution through operations such as water-soluble, alkali precipitation, washing, nitric acid dissolution; Then Using the TBP kerosene solution added with n-octanol as the extraction agent, taking advantage of the characteristics of TBP to preferentially extract zirconium, through multi-stage countercurrent extraction, most of the zirconium and a very small amount of hafnium are extracted into the organic phase; the organic phase is loaded with a certain Washing with a concentrated nitric acid solution can further remove most of the hafnium in the organic phase; back-extract the loaded ...

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Abstract

The invention belongs to the field of wet metallurgy and the technical field of zirconium and hafnium separation, and in particular, relates to a process for separating zirconium and hafnium by a solvent extracting method. Industrial products containing hafnium zirconium chloride acetyl are used as raw materials for such procedures as water solution, alkali sinking, washing and nitric acid dissolving to prepare zirconium (hafnium) nitrate acetyl solution; TBP kerosene solution of adding phase modifying agent octanol is used as an extracting agent; most zirconium and less hafnium are extracted into an organic phase through multistage counter-current extraction by using the characteristic of TBP priority extraction of zirconium; the loaded organic phase is washed by nitric acid solution with a certain concentration to further remove most hafnium in the organic phase; the acid-washed loaded organic phase is reversely extracted by water to obtain zirconium nitrate acetyl solution; the solution is precipitated in ammonia, dried and calcined to obtain zirconium dioxide powder, and the mass of the zirconium dioxide powder accords with the atomic energy-level zirconium dioxide standard; less zirconium and most hafnium only remained in residual water phase of zirconium after reverse extraction are extracted; the content of zirconium in hafnium meets the requirements on impurity zirconium by atomic energy-level hafnium; and atomic energy-level hafnium can be directly prepared by enrichment.

Description

technical field [0001] The invention belongs to the technical field of separation of zirconium and hafnium in the field of hydrometallurgy, and in particular relates to a process for separating zirconium and hafnium by a solvent extraction method. Background technique [0002] Zirconium and hafnium are naturally symbiotic, and they belong to Group IVB elements in the periodic table of chemical elements. The atomic radii, ionic radii, and structures of the two are very similar, resulting in their chemical properties are also extremely similar, making them one of the most difficult to separate element pairs in the periodic table. At home and abroad, there are many studies on the separation methods of zirconium and hafnium, which are mainly divided into fire separation and wet separation. [0003] The fire separation successfully applied in industrial production is zirconium hafnium molten salt rectification method, which has the advantages of less consumption of chemical reag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/14C22B3/38C01G25/02
CPCC01G25/02C01P2006/80C22B34/14C22B3/3846Y02P10/20
Inventor 李大炳支梅峰赵凤岐舒祖骏周志全张永明
Owner BEIJING RESEARCH INSTITUTE OF CHEMICAL ENGINEERING AND METALLURGY
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