Method for preparing zirconium by TBP extraction method

A technology of extraction and zirconia, applied in the field of hydrometallurgy, which can solve the problems of emulsification and high silicon content

Inactive Publication Date: 2020-07-07
林钢 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The traditional TBP extraction method separates zirconium and hafnium. TBP, tributyl phosphate is used as the extraction agent. Since the extracti

Method used

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  • Method for preparing zirconium by TBP extraction method

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Embodiment 1

[0032] Embodiment 1: technological process

[0033] Step 1: After adding ingredients into the zirconium oxychloride solution, carry out six-stage TBP extraction. The ingredients are a mixture of hydrochloric acid and nitric acid. The TBP organic phase used for extraction is made of 60% tributyl phosphate and 40% kerosene to obtain water Phase hafnium liquid and organic phase solution.

[0034] Step 2: the aqueous phase hafnium liquid obtained in step 1 is enriched and extracted with secondary diisooctyl phosphate (P204) to obtain an organic phase and raffinate waste acid, and the P204 organic phase is composed of 10% diisooctyl phosphate, 85% kerosene and 5% tributyl phosphate made.

[0035] Step 3: The organic phase obtained in step 2 is subjected to secondary ammonium bicarbonate back extraction to obtain an organic phase and an aqueous phase.

[0036] Step 4: The organic phase obtained in step 3 is acidified with secondary nitric acid to obtain an organic phase of diisooc...

Embodiment 2

[0044] Embodiment 2: operation process

[0045] The control and operating method of the equipment designed according to the technological process of embodiment 1 are as follows:

[0046] (1) Connection of the extraction tank: The extraction tank must first be cleaned and connected. Check that the switches (valves), flow meters, and pipelines of each inlet and outlet are smooth and normal. Check that upstream and downstream device settings are in place.

[0047] (2) Filling: according to the technical conditions - the ratio and the series are filled with each solution, and the empty tank does not move.

[0048] (3) Turn on the mixer, and measure the static and dynamic liquid level height difference of each extraction tank.

[0049] (4) Carry out normal operation according to the determined flow rate.

[0050] (5) Determination of acidity and ZrO in extraction grade 2 content.

[0051] (6) When the operation reaches equilibrium, directly determine whether the Hf liquid wat...

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Abstract

The invention discloses a preparation method of zirconium oxide. The preparation method comprises the following steps: 1, after ingredients is added into a zirconium oxychloride solution, TBP extraction is performed to obtain an aqueous phase hafnium solution and an organic phase solution; 2, the obtained organic phase solution carried out mixed acid washing to obtain a zirconium-containing organic phase and an acid washing solution; 3, the obtained zirconium-containing organic phase carried out reverse extraction to obtain water phase zirconium liquid and an organic phase; 4, the obtained aqueous phase zirconium liquid carried out ammonia precipitation, and the precipitate is calcined to obtain zirconium oxide; and 5, the obtained organic phase carried out alkali liquor treatment, water washing and nitric acid saturation treatment to obtain residual acid and an organic phase. The method has the advantages that the extraction capacity is large, the extraction equipment is small, the separation coefficient is high, the separation effect is good, the efficiency is high, the process is stable, the process is easy to control, the yield is high, and the recovery rate is high; and a closed system is adopted for extraction, so that environmental pollution is avoided. The Si/Zr ratio in the zirconium oxychloride solution is small, the production process does not produce emulsification,and meanwhile zirconia conforming to the atomic energy level is obtained.

Description

technical field [0001] The application relates to the technical field of hydrometallurgy, in particular to a method for preparing zirconium by a TBP extraction method. Background technique [0002] In order to realize an environment-friendly society, in the process of searching for new energy sources to replace fossil fuels, nuclear energy stands out due to its advantages of high efficiency and environmental protection. The use environment of nuclear energy makes its requirements for materials extremely strict. Zirconium and zirconium alloys are widely used in the nuclear industry due to their excellent nuclear properties. Atomic energy grade sponge zirconium material is an indispensable key material for reactor applications, and is used in nuclear fuel cladding, grids, end plugs and other core materials. [0003] The Krall method is currently the main production method for metal zirconium, which mainly includes the following steps: decomposition of zircon sand and preparat...

Claims

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Application Information

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IPC IPC(8): C22B3/38C22B3/44C22B34/14
CPCC22B3/44C22B34/14C22B3/3846Y02P10/20
Inventor 林钢陶勇
Owner 林钢
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