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Zirconium-hafnium separation method for preferentially extracting hafnium by utilizing organic acid

A separation method and organic acid technology, which is applied in the field of zirconium and hafnium separation, can solve the problems of poor separation effect of zirconium and hafnium, pollute the environment, and low efficiency, and achieve the effects of environmental protection, low acidity, and high efficiency

Active Publication Date: 2019-01-25
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention provides a zirconium and hafnium separation method using D2EHPA as the extraction agent in a hydrochloric acid system to preferentially extract hafnium with the help of organic acids. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The concentration of zirconium and hafnium ions in the preparation is 5×10 -4 mol·dm -3 , the organic acid concentration is 5×10 -3 mol·dm -3 , the concentration of hydrochloric acid is 0.06 mol·dm -3 solution as the aqueous phase. With 90% n-octane-10% n-octanol as diluent, prepare 5×10 -3 mol·dm -3 D2EHPA as the organic phase.

[0019] Mix the above-mentioned organic phase and aqueous phase at a volume ratio of 1:1, control the extraction temperature at 30°C, shake for one hour, use a centrifuge to separate the phases, dilute the aqueous phase by a certain number of times, and use ICP to measure the concentration of zirconium and hafnium ions, respectively Calculate the maximum separation factor. The organic phase was back-extracted with deionized water at 30°C, and the stripping rate was as high as 99%.

[0020] The specific process parameters and product properties are shown in Table 1.

Embodiment 2

[0022] The concentration of zirconium and hafnium ions in the preparation is 5×10 -4 mol·dm -3 , the organic acid concentration is 5×10 -3 mol·dm -3 , the concentration of hydrochloric acid is 0.1 mol·dm -3 solution as the aqueous phase. With 90% n-octane-10% n-octanol as diluent, prepare 5×10 -3 mol·dm -3 D2EHPA as the organic phase.

[0023] Mix the above-mentioned organic phase and aqueous phase at a volume ratio of 1:1, control the extraction temperature at 30°C, shake for one hour, use a centrifuge to separate the phases, dilute the aqueous phase by a certain number of times, and use ICP to measure the concentration of zirconium and hafnium ions, respectively Calculate the maximum separation factor. The organic phase was back-extracted with deionized water at 30°C, and the stripping rate was as high as 99%.

[0024] The specific process parameters and product properties are shown in Table 1.

Embodiment 3

[0026] The concentration of zirconium and hafnium ions in the preparation is 5×10 -4 mol·dm -3 , the organic acid concentration is 5×10 -3 mol·dm -3 , the concentration of hydrochloric acid is 0.14 mol·dm -3 solution as the aqueous phase. With 90% n-octane-10% n-octanol as diluent, prepare 5×10 -3 mol·dm -3 D2EHPA as the organic phase.

[0027] Mix the above-mentioned organic phase and aqueous phase at a volume ratio of 1:1, control the extraction temperature at 30°C, shake for one hour, use a centrifuge to separate the phases, dilute the aqueous phase by a certain number of times, and use ICP to measure the concentration of zirconium and hafnium ions, respectively Calculate the maximum separation factor. The organic phase was back-extracted with deionized water at 30°C, and the stripping rate was as high as 99%.

[0028] The specific process parameters and product properties are shown in Table 1.

[0029] Table 1

[0030] .

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PUM

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Abstract

The invention discloses a zirconium-hafnium separation method for preferentially extracting hafnium by utilizing organic acid. The method mainly solves the problems that the separation efficiency is low, the cost is high, the environment is polluted, and the oeration is complex. According to the method, D2EHPA is dissolved in 90% normal octane-10% n-caprylic alcohol and taken as an organic phase,zirconium-hafnium ions are dissolved in hydrochloric acid, tartaric acid, citric acid and glutamic acid are added, the mixture is taken as a water phase, the water phase and an organic phase are separated at the temperature of 30 DEG C after vibration, and the separation effect of preferentially extracting hafnium is achieved. The zirconium-hafnium ions are recovered through reverse extraction, the reverse extraction rate reaches 99% or above, and the organic phase can be recycled. The method is high in separation factor, low in pollution and cost and high in efficiency, and can be applied toindustrial production of zirconium-hafnium separation.

Description

technical field [0001] The invention relates to the technical field of separation of zirconium and hafnium. Background technique [0002] Metal zirconium and hafnium are located in subgroup IV of the periodic table of elements, and the arrangement of valence electrons outside the nucleus is similar (zirconium is 4d25s2, hafnium is 5d26s2), and is restricted by the "lanthanide contraction" effect, and the physical and chemical properties of zirconium and hafnium are also very Similarity, not easy to separate, has always been recognized as one of the most difficult elements to separate. In nature, zirconium and hafnium exist in the form of ores, and the content in the earth's crust is 0.025%, and hafnium accounts for about 2% of zirconium. [0003] Zirconium and hafnium play a vital role in the nuclear power industry. Zirconium has a small thermal neutron absorption cross section and is widely used in reactor cladding and structural materials. Hafnium has a large thermal ne...

Claims

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Application Information

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IPC IPC(8): C22B3/38C22B34/14
CPCC22B34/14C22B3/3846Y02P10/20
Inventor 崔玉赵嘉琳梁帅
Owner UNIV OF JINAN