Method for preparing zirconia from solid waste zirconium

A zirconia and solid technology, applied in the field of resource utilization of solid waste, can solve the problems of low production cost, environmental pollution, etc., achieve the effects of low equipment requirements, broad market prospects, and avoid disposal problems

Inactive Publication Date: 2018-05-29
SHANDONG LEIBAO ZIRCONIUM SCI&TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention directly uses solid waste zirconium as a raw material to prepare zirconia, overcomes the "three wastes" environmental pollution problem existing in the traditional route of using zirconium oxychloride as a raw material to produce zirconia powder, and realizes the resource utilization of solid waste. The method for preparing zirconia powder of the present invention has low production cost, simple process and low equipment requirements

Method used

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  • Method for preparing zirconia from solid waste zirconium
  • Method for preparing zirconia from solid waste zirconium
  • Method for preparing zirconia from solid waste zirconium

Examples

Experimental program
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Effect test

Embodiment 1

[0059] A method for preparing zirconia with solid waste zirconium, comprising the following steps:

[0060] (1) The zirconia ceramic waste is pulverized and ground, and mixed with NaOH at a mass ratio of 1:1.1. After mixing, it is moved into a stainless steel pot and roasted at 800 ° C for 3 hours to obtain zirconium salt;

[0061] (2) washing the zirconium salt with deionized water, then adding it to hydrochloric acid with a concentration of 21 wt % and heating for 3 h to obtain a reaction product, and carrying out solid-liquid separation on the reaction product to obtain a transformation liquid, to the described Sulfuric acid is added in the transformation liquid to carry out the primary reaction to obtain basic zirconium sulfate as the first precipitate, the first precipitate is further reacted with sulfuric acid to obtain zirconium sulfate, and the zirconium sulfate is prepared as 0.25mol / L zirconium sulfate solution for backup;

[0062] (3) 0.25mol / L NaOH solution was dr...

Embodiment 2

[0067] A method for preparing zirconia with solid waste zirconium, comprising the following steps:

[0068] (1) The zirconia artificial gemstone processing and grinding slag is pulverized and ground, and mixed with NaOH at a mass ratio of 1:1.5. After mixing, it is moved into a stainless steel pot and roasted at 700 ° C for 3 hours to obtain zirconium salt;

[0069] (2) washing the zirconium salt with deionized water, then adding it to hydrochloric acid with a concentration of 23wt% and heating for 3h to obtain a reaction product, and carrying out solid-liquid separation on the reaction product to obtain a transformation liquid, and to the described Sulfuric acid is added in the transformation liquid to carry out the initial reaction, to obtain basic zirconium sulfate as the first precipitate, the first precipitate is further reacted with sulfuric acid to obtain zirconium sulfate, and the zirconium sulfate is prepared into 0.5 mol / L zirconium sulfate solution for backup;

[0...

Embodiment 3

[0075] A method for preparing zirconia with solid waste zirconium, comprising the following steps:

[0076] (1) The zirconia composite refractory waste processing and grinding slag is pulverized and ground, and mixed with NH 4 OH was mixed at a mass ratio of 1:1.3, and then moved into a stainless steel pot after mixing, and calcined at 1000 °C for 3 hours to obtain zirconium salt;

[0077] (2) washing the zirconium salt with deionized water, then adding it to hydrochloric acid with a concentration of 24 wt % and heating for 3 h to obtain a reaction product. The reaction product is subjected to solid-liquid separation to obtain a transformation liquid. Sulfuric acid is added in the transformation liquid to carry out the initial reaction, to obtain basic zirconium sulfate as the first precipitate, the first precipitate is further reacted with sulfuric acid to obtain zirconium sulfate, and the zirconium sulfate is prepared into 3.0 mol / L zirconium sulfate solution for backup;

...

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Abstract

The invention provides a method for preparing zirconia from solid waste zirconium. The method comprises the following steps: (1) performing alkalization: after solid waste zirconium are smashed and ground, alkali metal hydroxide is added for roasting, and zirconium salt is obtained; (2) performing extraction and concentration: the zirconium salt is washed with water for impurity removal, subjectedto acidic washing transformation and filtered to remove slag, a transformed solution is obtained and subjected to primary reaction with sulfuric acid, a first precipitate is obtained and subjected tosecondary reaction with sulfuric acid for crystallization and separation of zirconium sulfate, and a zirconium sulfate solution being 0.25-3 mol/L is prepared from zirconium sulfate for standby application; (3) adding dropwise a precipitant to the zirconium sulfate solution for reaction to obtain a second precipitate; (4) washing, drying and calcining the second precipitate to obtain zirconia. The method has the advantages of low equipment requirement, simple process and high powder quality, and recycling of solid waste zirconium is realized.

Description

technical field [0001] The invention relates to the technical field of solid waste resource utilization. More specifically, it relates to a method for preparing high-quality zirconia from solid waste zirconium. Background technique [0002] China currently uses 30-40wt / year of zirconium ore, becoming the world's largest consumer of zirconium ore resources. However, due to the limitation of China's zirconium resources, self-produced zirconium ore only accounts for 2 / 5 of the total consumption. According to the current GDP development rate and import ratio, if there is no new zirconium ore source, it can be used in China for about 40 years. With zero imports as the base estimate, the level of protection is only about 20 years. China's current demand for zircon ore resources relies heavily on foreign countries, and the price of imported zircon sand has risen from about 3,000 yuan / t in the early 1990s to a peak of 10,000 yuan / t in 2005. As zirconium is an important strategic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02C04B35/626C04B35/622C04B35/48C01F17/00
CPCC01G25/02C04B35/48C04B35/62204C04B35/62685C01P2004/82C01P2004/62C01P2004/64C04B2235/5454C04B2235/5445C04B2235/3225C01F17/206
Inventor 王光强周有福陈彩云刘学燕
Owner SHANDONG LEIBAO ZIRCONIUM SCI&TECH
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