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Method for synthesizing nano zirconium oxide by rheological phase method

A nano-zirconia, rheological phase technology, applied in zirconia, nanotechnology, nanotechnology and other directions, can solve the problems of complex process, high equipment cost, difficult industrial production and other problems, and achieve simple process conditions, low cost and easy control. Effect

Inactive Publication Date: 2021-06-08
ANHUI JINGCHENG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for producing zirconia powder can be divided into three types: solid-phase synthesis, liquid-phase synthesis and gas-phase synthesis. The requirements for equipment are high, the cost is high, the process is complicated, and it is not easy for industrial production.

Method used

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  • Method for synthesizing nano zirconium oxide by rheological phase method
  • Method for synthesizing nano zirconium oxide by rheological phase method
  • Method for synthesizing nano zirconium oxide by rheological phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put 7.1g of solid zirconium sulfate and 5.1g of solid oxalic acid in a mortar, oxalic acid is organic acid citric acid, add surfactant, surfactant is anionic surfactant sodium dodecylbenzene sulfonate, surfactant The proportion of the amount to the total amount of reactants is 2%. Grind it into a powder, add 3ml of a mixed solution of alcohol and water with a ratio of 1:1, grind for 5min, grind to the rheological phase state, and transfer it to a polytetrafluoroethylene In the reaction kettle, the temperature of the reaction kettle is 80°C, and the temperature is kept constant for 10 hours. After the reaction is completed, the mixture is transferred to a centrifuge tube and centrifuged on a centrifuge. After the end, the supernatant is poured out, water is added, and the glass rod is used to stir for 2 minutes. Centrifuge again, repeat the centrifugation 3 times in this way, complete 4 times of water washing process, replace with ethanol and repeat the operation, complet...

Embodiment 2

[0033] Put 7.1g of solid zirconyl sulfate and 5.1g of solid oxalic acid in a mortar, oxalic acid is organic acid benzoic acid, add surfactant, surfactant is cationic surfactant cetyltrimethylammonium bromide, surface The amount of the active agent accounts for 3% of the total amount of the reactants. Grind it into a powder, add 5ml of a mixed solution of alcohol and water with a ratio of 1:2, and grind it for 10 minutes. In the reaction kettle of vinyl fluoride, the temperature of the reaction kettle is 90°C, and the temperature is kept constant for 14 hours. After the reaction is completed, the mixture is transferred to a centrifuge tube and centrifuged on a centrifuge. After the end, the supernatant is poured out, and water is added. Stir for 3 minutes, centrifuge again, repeat the centrifugation 4 times, complete the washing process 3 times, replace with ethanol and repeat the operation, complete 5 alcohol washings, and dry the centrifuge tube in an oven at 90°C after washin...

Embodiment 3

[0035] Put 7.1g of solid zirconyl sulfate and 5.1g of solid oxalic acid in a mortar, oxalic acid is organic acid benzoic acid, add surfactant, surfactant is nonionic surfactant PEG (polyethylene glycol)-10000, surface The amount of the active agent accounts for 5% of the total amount of the reactants. Grind it into a powder, add 7ml of a mixed solution of alcohol and water with a ratio of 2:1, and grind it for 15 minutes. In the reaction kettle of vinyl fluoride, the temperature of the reaction kettle is 100°C, and the temperature is kept constant for 16 hours. After the reaction is completed, transfer the mixture to a centrifuge tube and centrifuge on a centrifuge. After the end, pour off the supernatant, add water, and use a glass rod Stir for 4 minutes, centrifuge again, and repeat the centrifugation 5 times to complete the 5 times of water washing process, replace with ethanol and repeat the operation, complete 4 times of alcohol washing, after washing, dry the centrifuge t...

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Abstract

The invention discloses a method for synthesizing nano zirconium oxide by a rheological phase method. The method for synthesizing the nano zirconium oxide comprises the following steps: weighing and putting solid zirconium sulfate and solid oxalic acid into a ceramic mortar; adding different surfactants into a ceramic mortar, and grinding the surfactants into powder; adding an alcohol-water mixed solution into the solid mixture, and grinding obtained materials to a rheological phase state; transferring a reactant in the rheological phase state into a reaction kettle with a polytetrafluoroethylene lining; after the reaction is finished, performing centrifugal separating on a centrifugal machine, pouring out supernatant, adding water, performing stirring with a glass rod, performing centrifuging again, performing washing with water, and replacing with ethanol to repeat the operation; and after washing, putting a centrifugal tube into a drying box for constant-temperature drying to obtain zirconium oxide. According to the method for synthesizing the nano zirconium oxide, a novel synthesis method, namely a rheological phase method is adopted for synthesizing the nano oxide, the process conditions are simple, the cost is low, the requirement for equipment is low, the method is green and environmentally friendly, the yield of the zirconium dioxide powder is large, and the operation procedure is continuous and adjustable.

Description

technical field [0001] The invention relates to the field of inorganic nonmetals, in particular to a method for synthesizing nano zirconia by a rheological phase method. Background technique [0002] There are three crystal forms of zirconia, monoclinic crystal system at low temperature with a relative density of 5.65g / cm3; tetragonal crystal system with a relative density of 6.10g / cm3 at high temperature; cubic crystal system at a higher temperature with a relative density of 6.27 g / cm3. When heated to 1170°C, monoclinic zirconia transforms into tetragonal zirconia, which is very fast and accompanied by a volume shrinkage of 7% to 9%. However, during the cooling process, tetragonal zirconia often does not transform into monoclinic zirconia at 1170°C, but transforms at around 1000°C, which is a hysteresis transformation accompanied by volume expansion. In a ceramic matrix with a fixed composition, the phase transition temperature of zirconia decreases with the decrease of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y30/00
CPCC01G25/02B82Y30/00C01P2002/72C01P2004/03C01P2004/61
Inventor 侯帅帅杨景红吴月刘丙进王禹夏义文
Owner ANHUI JINGCHENG NEW MATERIAL CO LTD