Zirconium and method for preparing zirconium

A zirconium oxide and metal heat technology, applied in the field of zirconium preparation, can solve the problems such as the difficulty of simple and efficient industrial production of zirconium, and achieve the effect of reducing oxygen content

Active Publication Date: 2014-12-10
HUNAN RARE EARTH METAL MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing zirconium and the obtained zirconium and the obtained zirconium, so as to solve the technical problem that zirconium with a purity higher than 99.9% is difficult to be simple and efficient and suitable for industrial production in the prior art

Method used

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  • Zirconium and method for preparing zirconium

Examples

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Comparison scheme
Effect test

Embodiment 1

[0040] The preparation of zirconium is carried out by this method. First, 180g of metal Ca, 200g of ZrO 2 (Zirconium oxide particle size is 20 mesh, hafnium content is 95ppm), 300g of anhydrous calcium chloride, mixed and reacted at 950°C for 3 hours, and the calcium chloride used is calcined at 500°C for 8 hours. The reduction reaction product is washed with water until no bubbles are generated to remove calcium oxide, so that unreacted metal Ca is converted into Ca(OH) 2 , Get the water-washed mixture. Then wash the water-washing mixture with 0.8mol / L acetic acid solution three times in sequence, and then wash with pure water until the pH of the solution is neutral, filter to remove the water, and then use absolute ethanol to suction filter twice, and finally in an argon atmosphere Medium and dry. Primary zirconium obtained after drying.

[0041] Add primary zirconium to 500gCaCl 2 And 10gCa molten salt, in an argon atmosphere, after holding at 950°C for 8 hours, the product i...

Embodiment 2

[0047] The preparation of zirconium is carried out by this method, and 200 g of metal Mg, 200 g of ZrO 2 (Its ZrO 2 The particle size is 50 mesh, and the hafnium content is 70ppm), 360g of sodium chloride, mixed and reacted at 1000°C for 2 hours. After the furnace is released, the metal thermal reduction reaction product is washed three times with 0.2mol / L HCl, and then pure water Wash the solution until the pH value of the solution is neutral, filter to remove the water, then use anhydrous ethanol to suction filter twice, and finally dry in an argon atmosphere to remove impurities. Primary zirconium obtained after drying.

[0048] Add primary zirconium to 500gCaCl 2 And 20gCa molten salt, in an argon atmosphere, after holding at 900°C for 8 hours, the product is washed with water to neutrality, filtered and dried to obtain secondary zirconium.

[0049] Put the secondary zirconium into a vacuum furnace when the vacuum degree is greater than 10 -5 Under the conditions, heat to 800°C...

Embodiment 3

[0055] This method is used to prepare zirconium, and 80g of metal CaH 2 , 200g of ZrO 2 (The particle size is 100 mesh, and the hafnium content is 55ppm), 160g of calcium chloride, mixed and reacted at 900°C for 3 hours. After the furnace is released, the metal thermal reduction reaction product is washed with water until no more bubbles are emitted to obtain a water-washed mixture , And then washed with 1mol / L acetic acid three times, then washed with pure water until the pH value of the solution is neutral, filtered to remove water, and then filtered twice with absolute ethanol, and finally dried in an argon atmosphere. Primary zirconium obtained after drying.

[0056] Add primary zirconium to 400gCaCl 2 And 10gCa molten salt, in an argon atmosphere, after holding at 1000°C for 5 hours, the product is washed with water to neutrality, filtered and dried to obtain secondary zirconium.

[0057] Put the secondary zirconium into a vacuum furnace when the vacuum degree is greater than ...

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Abstract

The invention provides zirconium and a method for preparing the zirconium. The method comprises the following steps: metallothermic reduction, namely promoting zirconium oxide and alkaline-earth metal or alkaline-earth metal hydride to perform a metallothermic reduction reaction, and removing impurities to obtain primary zirconium; molten salt refining, namely promoting the primary zirconium and mixed molten salt to perform a molten salt refining reaction so as to obtain secondary zirconium; vacuum distillation, namely performing vacuum distillation on the secondary zirconium so as to obtain tertiary zirconium; and combined melting, namely sequentially performing smelting in suspension and electron beam zone melting on the tertiary zirconium so as to obtain the product zirconium, wherein the mixed molten salt consists of CaCl2 and Ca. According to the method, the zirconium oxide is used as a raw material, metallothermic reduction, molten salt refining, vacuum distillation and combined melting methods are sequentially adopted, the primary zirconium obtained after the metallothermic reduction is subjected to molten salt refining, the oxygen content of the intermediate product zirconium can be effectively reduced, and the mixed molten salt used in the method can be easily removed by means of water washing, and the purity of zirconium cannot be influenced.

Description

Technical field [0001] The invention relates to the field of metal preparation, in particular, to a method for preparing zirconium and the obtained zirconium. Background technique [0002] Zr has a small thermal neutron capture cross-section and high strength, so it is widely used in nuclear reactor materials. In addition, Zr's excellent physical and chemical properties make it also used in reactors, valves and other components in the chemical industry, as well as additives for killed steel and non-ferrous alloys. With the advancement of science and technology, especially the rapid development of the nuclear industry in recent years, the purity requirements for Zr are getting higher and higher. The current methods for preparing zirconium with a purity greater than 99.9% mainly include the Kraul method, molten salt electrolysis method, halide thermal dissociation method, and metal thermal reduction ZrO 2 law. [0003] Kraul method: Since Kraul invented the method of reducing titani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/14C22B5/04C22B9/10C22B9/02
CPCY02P10/20
Inventor 黄美松贾帅广王志坚成维
Owner HUNAN RARE EARTH METAL MATERIAL RES INST
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