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The preparation method of nanoscale zrO2 powder

A nano-scale, powder technology, applied in the field of preparation of nano-scale ZrO2 powder, can solve the problems of high production cost, high production equipment cost, and numerous production process steps, and achieve the effect of low production cost and simplified production process steps

Active Publication Date: 2015-09-16
贵州万方铝化科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, the solid phase synthesis method and the high temperature spray pyrolysis method have many process steps; the normal temperature hydrolysis method, the high temperature hydrolysis method and the metal organic compound hydrolysis method have high raw material costs; the spray induction coupled plasma pyrolysis method has high production equipment costs
Therefore, in related technologies, ZrO 2 There are many steps in the production process and the production cost is high

Method used

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  • The preparation method of nanoscale zrO2 powder
  • The preparation method of nanoscale zrO2 powder

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preparation example Construction

[0031] The embodiment of the present invention provides nano-scale ZrO 2 The preparation method of powder includes the following steps:

[0032] Step 101: Mix ZrO2-containing minerals or zirconium-containing minerals with fluoride to obtain a mixture;

[0033] Step 102: Make the mixture react, and finally obtain gaseous ZrF 4 ;

[0034] Step 103: To the gaseous ZrF 4 Into the water vapor, hydrolyze to obtain solid ZrO 2 Gas-solid mixture with gaseous HF;

[0035] Step 104: Quench the gas-solid mixture at 200°C~450°C for crystallization to obtain nano-scale ZrO 2 powder.

[0036] Nano-scale ZrO provided in the embodiment of the present invention 2 In the preparation method of powder, fluoride (AF z ) In the F element and minerals containing ZrO2 or zirconium-containing minerals (M x O y ·NZrO 2 ) The fluorine-philic element Zr reacts, and the reaction formula is:

[0037] M x O y ·NZrO 2 +AF z →M x O y +A 2 O z +ZrF4

[0038] ZrF 4 +2H 2 O→ZrO 2 +4HF

[0039] Through the above reaction, gas...

preparation example 1

[0065] Preparation Example 1: Using ZrO 2 Waste and NH 4 F is the raw material to prepare nano-scale ZrO 2 powder

[0066] ZrO 2 Coarse particles of ZrO in waste 2 And NH 4 F mix evenly to obtain the mixture, coarse particles of ZrO 2 With NH 4 The particle size of F is 3 mm or less. NH in the mixture 4 The mass percentage of F is 30%. The mixture is calcined at 910°C for 3 hours to generate NH 3 , H 2 O and ZrF 4 . ZrF 4 It is gaseous at high temperature and escapes. ZrF that will escape 4 After purification treatment (removal of NH 3 ) Introduce into another reactor and pass water vapor. The volume content of water vapor is 80%. After hydrolysis at 910℃, ZrO is generated 2 And HF gas. The high temperature mixed gas is quenched to 350℃ to obtain ZrO 2 For pellets, the cooling rate is 50°C / min. ZrO is obtained from the particles after agglomeration, separation, deacidification and other post-treatment processes 2 Powder (particle size is 50nm ~ 86nm). The reaction equation is...

preparation example 2

[0069] Preparation Example 2: Using oblique zircon and AlF 3 Preparation of nano-scale ZrO as raw material 2 powder

[0070] Combine oblique zircon with AlF 3 Mix evenly to get a mixture, oblique zircon and AlF 3 The particle diameters are all 3mm or less. AlF in mixture 3 The mass percentage is 40%. The mixture is calcined at 1000°C for 5 hours to generate Al 2 O 3 And ZrF 4 , Because this mineral contains silicon, there will be SiO 4 Gas is generated, so gaseous SiO needs to be removed 4 . For gaseous SiO 4 And gaseous ZrF 4 The composition of the mixed gas is cooled to below 600°C to obtain solid ZrF 4 And gaseous SiO 4 The gas-solid mixture is separated from the gas-solid mixture to obtain solid ZrF 4 . Then the solid ZrF 4 Raise the temperature to above 1000℃ for gasification to obtain gaseous ZrF 4 . ZrF 4 It is gaseous at high temperature and escapes from solids. ZrF that will escape 4 After purification treatment, it is introduced into another reactor, and water vapor ...

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Abstract

The invention relates to the field of preparation of chemical materials and particularly relates to a preparation method of nanoscale ZrO2 powder. The preparation method of the nanoscale ZrO2 powder comprises the following steps: mixing ZrO2-containing minerals or Zr-containing minerals and fluoride to obtain a mixture; enabling the mixture to react to finally obtain gaseous ZrF4; introducing water vapor to the gaseous ZrF4, and hydrolyzing to obtain a gas-solid mixture of solid ZrO2 and gaseous HF; carrying out shock cooling on the gas-solid mixture for crystalizing at 200-450 DEG C to obtain the nanoscale ZrO2 powder. According to the preparation method of the nanoscale ZrO2 powder, the preparation process can be finished by adopting a well-known reaction device in the field, and the production process and steps are simplified; in addition, cheap ZrO2-containing minerals or Zr-containing minerals, the fluoride and the water vapor are adopted as main raw materials, so that the production cost is low.

Description

Technical field [0001] The present invention relates to the field of chemical material preparation, in particular, to nanometer ZrO 2 Powder preparation method. Background technique [0002] ZrO 2 It is a white crystalline powder with high melting point, high boiling point, low thermal conductivity, large thermal expansion coefficient, low friction coefficient, good wear resistance, high chemical stability, and excellent corrosion resistance (especially good resistance to chemical erosion and microorganisms) Corrosion ability) and other characteristics, is very ideal high temperature refractory materials, abrasive materials and high temperature insulation materials. In many different fields, such as ceramic pigments, engineering ceramics, gem industry, piezoelectric components, ion exchangers and solid electrolytes, it has a wide range of uses. From a structural point of view, ZrO 2 Due to its acidic and basic surface centers, it is an ideal acid-based bifunctional catalytic mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82Y30/00B82Y40/00
Inventor 龚亚云刘瑞林乐洪章林李丹阳
Owner 贵州万方铝化科技开发有限公司