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Method for preparing zirconium

A technology of zirconia and chloride salt, which is applied in the field of zirconium preparation, can solve the problems of simplicity and high efficiency, and achieve the effect of reducing oxygen content

Active Publication Date: 2016-03-23
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, 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

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  • Method for preparing zirconium

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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, after mixing, react at 950°C for 3 hours, and the calcium chloride used is processed by calcination at 500°C for 8 hours. The reduction reaction product is washed with water until no bubbles are generated to remove calcium oxide and convert unreacted metal Ca into Ca(OH) 2 , to obtain a washing mixture. Then wash the water-washed mixture three times with 0.8mol / L acetic acid solution in sequence, then wash with pure water until the pH value of the solution is neutral, filter to remove water, and then use dehydrated ethanol to filter twice, finally in an argon atmosphere Medium dry. Primary zirconium obtained after drying.

[0041] Add primary zirconium to 500g CaCl 2 In molten salt with 10g Ca, under argon atmosphere, at 950°C for 8 hours, the product is washed wit...

Embodiment 2

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

[0048] Add primary zirconium to 500g CaCl 2 and 20g Ca molten salt, under argon atmosphere, at 900°C for 8 hours, after the product is washed to neutral, filtered and dried to obtain secondary zirconium.

[0049] Place the secondary zirconium into the vacuum furnace at a vacuum degree greater than 10 -5 Under the same conditions, it is heated to 800°C, k...

Embodiment 3

[0055] The preparation of zirconium was carried out by this method, and 80 g of metallic CaH 2 , 200g 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 being released from the furnace, the metallothermic reduction reaction product was washed with water until no bubbles emerged to obtain the water-washed mixture , and then washed three times with 1 mol / L acetic acid, and then washed with pure water until the pH value of the solution was 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 400g CaCl 2 In molten salt with 10g Ca, under argon atmosphere, at 1000°C for 5 hours, the product is washed with water until neutral, filtered and dried to obtain secondary zirconium.

[0057] Place the secondary zirconium into the vacuum furnace at a v...

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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. Background technique [0002] Zr is widely used in nuclear reactor materials because of its small thermal neutron capture cross-section and high strength. In addition, Zr's excellent physical and chemical properties make it also used in reactors, valves and other components in the chemical industry, 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 requirement for the purity of Zr is getting higher and higher. At present, the methods for preparing zirconium with a purity greater than 99.9% mainly include the Krall method, molten salt electrolysis, halide thermal dissociation, and metallothermic reduction of ZrO. 2 Law. [0003] Claure method: Since Claure invented the method of reducing titanium tetrachloride with ma...

Claims

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Application Information

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Patent Type & Authority Patents(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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