Method for preparing solid spherical rare earth oxide in one-step spraying thermal decomposition mode

A spray thermal decomposition, rare earth oxide technology, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as unbalanced decomposition, complex process control and equipment structure, and unavailability, and simplify the process. Parameter control and simplification of complex equipment structure, beneficial to industrial applications

Inactive Publication Date: 2013-09-25
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is worth noting that oxalic acid has certain toxicity, and it exists in wastewater, polluting the environment
At the same time, regardless of the oxalic acid precipitation method or the ammonium bicarbonate precipitation method, a large amount of carbon dioxide will be emitted during the burning rare earth precipitation process, which will increase the carbon emissions of the enterprise
In addition, the filtrate after precipitation by this method contains a large amount of chloride radicals, which cannot be utilized and will also cause environmental pollution.
[0005] Chinese patent application, application number 200410036484.1 discloses a method for preparing rare earth oxides, which solves the problems of high labor intensity, large equipment loss and serious pollution in the process of preparing rare earth oxides by oxalate precipitation method or ammonium bicarbonate precipitation method , unbalanced decomposition, poor consistency, and affecting product quality, etc., a technical scheme that can continuously burn and decompose rare earth carbonate or oxalate to prepare rare earth oxides was proposed, and the burning equipment was designed
Xu Huarui and others used the method of adding oxalate to cerium chloride solution to prepare solid spherical cerium oxide by thermal decomposition, but the method has the following problems. The first thermal decomposition process is divided into two stages, and the first stage is roasting. into cerium oxalate, and then carry out the second stage of roasting to decompose cerium oxalate to prepare cerium oxide, which leads to complex process control and equipment structure of this method, resulting in increased cost

Method used

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  • Method for preparing solid spherical rare earth oxide in one-step spraying thermal decomposition mode
  • Method for preparing solid spherical rare earth oxide in one-step spraying thermal decomposition mode
  • Method for preparing solid spherical rare earth oxide in one-step spraying thermal decomposition mode

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] First, the temperature of the roasting furnace is controlled at 400°C, and then a solution containing 350 g / L cerium chloride and 10 g / L oxalic acid is mixed with carrier compressed air at a flow rate of 800 liters / hour and sprayed into the roasting furnace. Roasting for 20 seconds, the slag is naturally cooled to obtain a solid spherical powder product with a cerium oxide content greater than 90wt%, and its scanning electron microscope picture is as follows: figure 1 shown, from figure 1 It can be seen that the particle size of spherical cerium oxide is uniform, and the average particle size is nanometer; its XRD pattern is as follows figure 2 shown, from figure 2 It can be seen that there are no miscellaneous peaks of other elements in the spectrum, and the purity of the powder is high.

Embodiment 2

[0041] First, the temperature of the roaster is controlled at 600°C, and then the solution containing 280g / L lanthanum chloride and 0.1g / L citric acid is mixed with the carrier compressed oxygen at a flow rate of 80 liters / hour and sprayed into the roaster Within 60 seconds of roasting, the slag is naturally cooled to obtain a solid spherical powder product with a lanthanum oxide content greater than 90wt%, and its XRD pattern is as follows Figure 4 shown, from Figure 4 It can be seen that there are no miscellaneous peaks of other elements in the spectrum, and the powder has high purity. It is a spherical substance with uniform particle size detected by scanning electron microscope.

Embodiment 3

[0043] First, the temperature of the roasting furnace is controlled at 700°C, and then the solution containing praseodymium chloride with a concentration of 80g / L and ammonium carbonate with a concentration of 0.1g / L is mixed with carrier compressed air at a flow rate of 180 liters / hour and sprayed into the roaster Within 4 seconds of roasting, the slag is naturally cooled to obtain a solid spherical powder product with a praseodymium oxide content greater than 90wt%, and its XRD pattern is as follows Figure 5 shown, from Figure 5 It can be seen that there are no miscellaneous peaks of other elements in the spectrum, and the powder has high purity. It is a spherical substance with uniform particle size detected by scanning electron microscope.

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Abstract

The invention belongs to the field of rare earth metallurgy, and in particular relates to a method for preparing a solid spherical rare earth oxide in a one-step spraying thermal decomposition mode. The method comprises the following steps of: firstly, controlling the temperature of a roasting furnace to 400-1700 DEG C, subsequently mixing a solution containing 10-350g/L rare earth oxide and 0.1-500g/L carboxylic acid additive with a carrier compressed gas with a flowing speed of 5-8,000L/h, subsequently spraying into the roasting furnace, roasting for 1-60 seconds, and naturally cooling down the roasting slag so as to obtain a solid spherical powder product of which the rare earth oxide content is greater than 90wt%. As a trivalent rare earth chloride solution is used as the raw material, ammonium bicarbonate and toxic oxalic acid are not used in the production process, carbon dioxide emitted in the roasting process in the conventional process is not generated, and the pollution on the environment is greatly reduced. Solid spherical powder can be prepared through one-step thermal decomposition.

Description

technical field [0001] The invention belongs to the field of rare earth metallurgy, and in particular relates to a method for preparing solid spherical rare earth oxides through one-step spray thermal decomposition. Background technique [0002] With the development of science and technology, rare earth oxides, as one of the basic materials for preparing new materials, have been more and more widely used. Rare earth oxides are the most common intermediate products in rare earth production, which can be further used to produce rare earth metals, alloys and functional materials, etc. At present, the preparation of rare earth oxides is developing in the direction of special physical and chemical properties, such as the preparation of rare earth oxides and rare earth composite powders with different particle sizes and specific surface areas. [0003] Rare earth oxides can be obtained by oxidizing rare earth metals in air, burning rare earth hydroxides and rare earth salts conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 吴文远边雪
Owner NORTHEASTERN UNIV
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