Microwave preparation method of nano rare earth oxide

A nano-rare earth and oxide technology, applied in the field of rare earth, can solve the problems of low product purity and yield, low rare earth recovery rate, uncontrollable heating process, etc., and achieve the effects of uniform shape, uniform size and controllable heating process.

Pending Publication Date: 2020-09-08
GUANGXI ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the methods for preparing nano-rare earth oxides (praseodymium oxide, or neodymium oxide, or praseodymium neodymium oxide) mostly use precipitation, extraction and separation, and ion exchange methods. Among them, the precipitation method cannot be used due to low rare earth recovery rate, small output, and high cost. It is applied in industrial production, and due to the agglomeration of the particles due to the uneven heating inside and outside of the particles during the high temperature reaction, the prepared praseodymium oxide (or neodymium oxide, or praseodymium neodymium oxide) has a large particle size and different shapes. The heating process is uncontrollable; the extraction and separation method is widely used in industrial production, but it has the disadvantages of cumbersome process, high consumption of extractant and high cost; the ion exchange method has the disadvantages of long preparation process, troublesome operation, low recovery rate of rare earth, low product purity and Disadvantages such as low output

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A microwave preparation method for nano-praseodymium oxide, comprising the following steps,

[0029] (1) Surface treatment: take a praseodymium salt solution with a concentration of 0.1mol / L to adjust the pH to be alkaline, add stearic acid with 5% molar mass of the praseodymium salt solution, and obtain a surface-treated praseodymium-containing solution;

[0030] (2) Precipitation reaction: Add oxalic acid dropwise at a rate of 0.5 L / min while stirring in the surface-treated praseodymium-containing solution, age, filter, and wash to obtain a praseodymium-containing precipitate; the oxalic acid: praseodymium molar Ratio = 1:1;

[0031] (3) Microwave calcination: put the praseodymium-containing precipitate into a microwave reactor, and carry out microwave heating and calcination at a frequency of 915±50MHz, a power of 1kw, and a temperature of 800°C for 1h to obtain nano-praseodymium oxide powder; the microwave output method For continuous wave mode.

Embodiment 2

[0033] A microwave preparation method for nanometer neodymium oxide, comprising the steps of,

[0034] (1) Surface treatment: take a neodymium salt solution with a concentration of 2mol / L to adjust the pH to be alkaline, add polyacrylamide with a molar mass of 15% of the neodymium salt solution, and obtain a surface-treated neodymium-containing solution; the rare earth salt solution is;

[0035] (2) Precipitation reaction: Add ammonium bicarbonate dropwise at a speed of 3L / min while stirring in the surface-treated neodymium-containing solution, age, filter, and wash to obtain a neodymium-containing precipitate; the ammonium bicarbonate: The molar ratio of neodymium=3:1;

[0036] (3) Microwave calcination: put the neodymium-containing precipitate into a microwave reactor, and perform microwave heating and calcination for 5 hours at a frequency of 2450±50MHz, a power of 10kw, and a temperature of 1200°C to obtain nano-neodymium oxide powder; the microwave output method It is th...

Embodiment 3

[0038] A microwave preparation method of nanometer praseodymium neodymium oxide, comprising the following steps,

[0039] (1) Surface treatment: take the praseodymium neodymium salt solution with a concentration of 0.5mol / L to adjust the pH to be alkaline, add citric acid with 10% molar mass of the praseodymium neodymium salt solution, and obtain the surface-treated solution containing praseodymium neodymium;

[0040] (2) Precipitation reaction: Add a precipitant dropwise at a rate of 1.5 L / min while stirring in the surface-treated solution containing NdP, age, filter, and wash to obtain a NdPr precipitate; the precipitant is oxalic acid Root: carbonate group=1:0.2; Described precipitation agent: praseodymium neodymium molar ratio 2:1;

[0041](3) Microwave calcination: put the praseodymium and neodymium precipitate into a microwave reactor, and carry out microwave heating and calcination for 2 hours at a frequency of 2450±50MHz, a power of 8kw, and a temperature of 1000°C to ...

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PUM

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Abstract

The invention discloses a microwave preparation method of a nano rare earth oxide, wherein the microwave preparation method comprises the following steps: (1) surface treatment: taking a rare earth salt solution, regulating the pH value to be alkaline, and adding a surface assistant to obtain a surface-treated rare earth-containing solution; (2) precipitation reaction: dropwise adding a precipitant into the surface-treated rare earth-containing solution while stirring, and aging, filtering and washing to obtain corresponding rare earth precipitates; and (3) microwave calcination: putting the precipitate into a microwave reactor, and carrying out microwave heating calcination to obtain the nano rare earth oxide powder. According to the invention, the nano rare earth oxide with uniform granularity, consistent morphology and good dispersity is prepared by adopting a microwave heating calcining method and matching with a surface additive.

Description

technical field [0001] The invention relates to the field of rare earths, in particular to a microwave preparation method of nanometer rare earth oxides. Background technique [0002] Praseodymium oxide (Pr 6 o 11 ) is an inorganic compound, the English name is Praseodymium oxide, which can be used in glass, metallurgy, and as a phosphor additive, etc. Praseodymium oxide is one of the important products in light rare earth products. Because of its unique physical and chemical properties, it has been widely used in the fields of ceramics, glass, rare earth permanent magnets, rare earth cracking catalysts, rare earth polishing powders, abrasive materials and additives, and its prospects are still promising. Since the 1990s, my country's praseodymium oxide production technology and equipment have been greatly improved and perfected, and the products and output have increased rapidly. It can not only supply domestic applications and market requirements, but also export a cons...

Claims

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Application Information

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IPC IPC(8): C01F17/10C01F17/206C01F17/224C01F17/241
CPCC01F17/10C01F17/206C01F17/241C01F17/224
Inventor 黄志民黄慨顾传君冼学权黄绍权黄华林
Owner GUANGXI ACAD OF SCI
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