CN109399689B - Method for preparing rare earth oxide by microwave technology - Google Patents
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- CN109399689B CN109399689B CN201811540548.XA CN201811540548A CN109399689B CN 109399689 B CN109399689 B CN 109399689B CN 201811540548 A CN201811540548 A CN 201811540548A CN 109399689 B CN109399689 B CN 109399689B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
Hair brushThe method comprises the steps of microwave drying, microwave preheating, microwave ignition, air cooling and the like, wherein rare earth oxalate or rare earth carbonate is subjected to microwave radiation in microwave equipment, microwave drying is carried out at the temperature of 120 plus materials and 150 ℃ until the water content of the rare earth oxalate or rare earth carbonate is 3-5%, microwave preheating is carried out at the temperature of 300 plus materials and 500 ℃ until the water content of the rare earth oxalate or rare earth carbonate is 0, microwave ignition is carried out at the temperature of 700 plus materials and 1000 ℃ for 30-50 min, and finally air cooling and cooling are carried out to obtain the rare earth oxide. The microwave heating method of the invention has the advantages of uniform heating, easy control of the process, purity of the rare earth oxide product of more than or equal to 99.99 percent, grain diameter D50 of 0.5-2.0 mu m, particle size distribution (D90-D10)/(2D50) of less than or equal to 1, and specific surface area of 4-7m2/g。
Description
Technical Field
The invention belongs to the technical field of rare earth material preparation, and particularly relates to a method for preparing rare earth oxide by using a microwave technology.
Background
China is a big rare earth resource country, and the yield is the first in the world. The rare earth element has excellent physical, chemical, magnetic, optical and electrical properties due to its special material structure, and has a very wide application, which is called the strategic element of the 21 st century. With the continuous research and understanding of people on the performance and application of rare earth elements and the advantages of rich rare earth resources and low price in China, rare earth is increasingly and widely applied in the fields of domestic appliances, daily chemical industry, ferrous metallurgy, petrochemical industry, laser technology, superconducting materials, medical care, agriculture, forestry, environmental protection and the like in China.
The conventional rare earth oxide burning mode is that rare earth oxalate or rare earth carbonate is put into high-temperature equipment, the temperature is gradually increased to 950-1050 ℃, the rare earth oxalate or rare earth carbonate is continuously burned at the high temperature and the constant temperature for a period of time and then is converted into rare earth oxide, and waste gas generated in the burning process is mainly CO2And water vapor. And cooling the burned rare earth oxide to room temperature, sieving, mixing, packaging and transporting to a warehouse for sale. But the common burning mode has the following defects: firstly, the burning time is longer and the cost is high. According to the burning process, rare earth oxalate or rare earth carbonate is burned from normal temperature to high temperature for 4 hours, and the burning lasts for 24 hours, so that the production cost, particularly the power consumption cost is high. Secondly, the granularity is not uniform and the phenomenon of overburning exists. Because the rare earth oxalate or rare earth carbonate is heated unevenly in each firing process, the water vapor heat dissipation is insufficient, powder caking and uneven firing are easily causedEven over-burning occurs.
Therefore, a novel rare earth oxide processing mode is developed, and the problems of high energy consumption cost and uneven product quality are solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and obtains a method for preparing rare earth oxide by using a microwave technology by researching and optimizing conditions such as temperature, time, a heating mode, a cooling mode and the like of rare earth radiated by a microwave external field.
The invention is realized by the following modes:
a method for preparing rare earth oxide by using microwave technology comprises the following steps:
(1) microwave drying: putting rare earth oxalate or rare earth carbonate into microwave equipment, starting microwave radiation, heating to 120-150 ℃ at the heating rate of 25-30 ℃/min, and drying for 10-30 min by microwave until the water content of the rare earth oxalate or rare earth carbonate is 3-5%;
(2) microwave preheating: heating to 300-500 ℃ at the heating rate of 15-20 ℃/min, and preheating for 20-60 min by microwave until the water content of the rare earth oxalate or rare earth carbonate is 0;
(3) microwave firing: heating to 700-1000 ℃ at a heating rate of 5-10 ℃/min, and performing microwave ignition for 30-50 min;
(4) gradient air cooling: in the air cooling process, the cooling speed is 5-10 ℃/min for 0-20 min, 15-20 ℃/min for 21-40 min, 25-30 ℃/min for 41 min, and the air cooling is continued for 10-20 min after the temperature is reduced to normal temperature, so as to obtain the rare earth oxide.
Preferably, the frequency of the microwave drying is 915 MHz.
Preferably, the power of the microwave drying is 50-100 KW/m3。
Preferably, the frequency of the microwave preheating is 2.45 GHz.
Preferably, the power of the microwave preheating is 150-200 KW/m3。
Preferably, the temperature of the microwave preheating is 400 ℃.
Preferably, the frequency of the microwave burning is 5.80 GHz.
Preferably, the power of the microwave ignition is 250-300 KW/m3。
Preferably, the temperature of the microwave ignition is 950 ℃.
Preferably, the microwave burning time is 50 min.
The principle of the invention is as follows:
the invention adopts the process of gradually increasing the frequency and the power in the wave radiation process. The initial stage of rare earth oxalate or rare earth carbonate has large volume and high water content, and the microwave drying adopts 915 MHz frequency and 50-100 KW/m power3The penetration capacity and the water evaporation capacity of the microwave can be enhanced, and the water content is reduced to 3-5%; when the volume of the material is reduced and the water content is less, the microwave preheating adopts the frequency of 2.45 GHz and the power of 150-KW/m3The microwave penetration capacity is met, the oscillation frequency of water molecules is increased, the water evaporation capacity is further improved, and the water content is reduced to 0; at the moment, the rare earth material is a dry material, the volume is further reduced, and the microwave ignition adopts the frequency of 5.80 GHz and the power of 250-300 KW/m3The microwave can penetrate through the rare earth material, the high-frequency oscillation of material molecules can be guaranteed, the heat generation and heat transfer efficiency are accelerated, the rare earth material can be heated quickly, at high temperature and uniformly, the firing quality is improved, and the obtained rare earth oxide has small and uniform granularity and large specific surface area. The air cooling process is carried out in microwave equipment at the same time, the temperature is reduced in a gradient manner, the temperature reduction speed is 5-10 ℃/min after 0-20 min, the temperature reduction speed is 15-20 ℃/min after 21-40 min, the temperature reduction speed is 25-30 ℃/min after 41 min, air cooling is continued for 10-20 min after the temperature is reduced to the normal temperature, the temperature reduction process is controlled to be changed from slow to fast, the phenomenon that the product is agglomerated due to the fact that the temperature reduction speed is too fast at high temperature is avoided, air cooling is continued after the temperature is reduced to the normal temperature, the phenomenon that the product absorbs water and is affected with damp is avoided, and the product quality is guaranteed.
The invention has the beneficial effects that:
1. the microwave radiation method has the advantages of high temperature rise speed and uniform heating, and can avoid the phenomena of caking, uneven firing and overburning of the rare earth powder.
2. The microwave radiation method has strong penetrating power, the rare earth material is completely decomposed, and the recovery rate of the rare earth is more than or equal to 98 percent.
3. The microwave radiation method has short period and low energy consumption, and can improve the production efficiency and reduce the production cost.
4. The air cooling is carried out in the microwave equipment, so that the rare earth oxide powder is prevented from moisture regain and caking in the cooling process, and the product quality is ensured.
5. The rare earth oxide product has the purity of more than or equal to 99.99 percent, the grain diameter D50 of 0.5 to 2.0 mu m, the grain size distribution (D90-D10)/(2D50) of less than or equal to 1 and the specific surface area of 4 to 7m2Per g, the product quality is very good.
Detailed Description
The invention is further described with reference to specific examples, without limiting the scope of protection and the scope of application of the invention.
Example 1
A method for preparing rare earth oxide by using microwave technology comprises the following steps:
(1) microwave drying: placing rare earth oxalate into microwave equipment, starting microwave radiation with frequency of 915 MHz, heating to 130 deg.C at a heating rate of 25 deg.C/min, microwave drying for 20 min with power of 80 KW/m3Until the water content of rare earth oxalate is 3%;
(2) microwave preheating: starting microwave frequency of 2.45 GHz, heating to 400 deg.C at a rate of 15 deg.C/min, microwave preheating for 30 min, and power of 160 KW/m3Until the water content of the rare earth oxalate is 0;
(3) microwave firing: starting microwave frequency at 5.80 GHz, heating to 950 deg.C at a rate of 5 deg.C/min, microwave-burning for 50 min at a power of 280 KW/m3；
(4) Gradient air cooling: in the air cooling process, the cooling speed is 5 ℃/min for 0-20 min, 15 ℃/min for 21-40 min, and 25 ℃/min after 41 min, and the rare earth oxide is obtained after air cooling is continued for 15 min after the temperature is reduced to normal temperature.
Example 2
A method for preparing rare earth oxide by using microwave technology comprises the following steps:
(1) microwave drying: placing rare earth oxalate or rare earth carbonate into microwave equipment, starting microwave radiation with frequency of 915 MHz, heating to 150 deg.C at a temperature rise rate of 30 deg.C/min, microwave drying for 10 min with power of 100 KW/m3Until the water content of rare earth oxalate or rare earth carbonate is 3 percent;
(2) microwave preheating: starting microwave frequency of 2.45 GHz, heating to 500 deg.C at a rate of 20 deg.C/min, microwave preheating for 20 min, and power of 180 KW/m3Until the water content of the rare earth oxalate or rare earth carbonate is 0;
(3) microwave firing: starting microwave frequency at 5.80 GHz, heating to 1000 deg.C at a heating rate of 10 deg.C/min, microwave burning for 30 min at a power of 300 KW/m3；
(4) Gradient air cooling: in the air cooling process, the cooling speed is 10 ℃/min for 0-20 min, 20 ℃/min for 21-40 min, and 25 ℃/min after 41 min, and the rare earth oxide is obtained after air cooling is continued for 10 min after the temperature is reduced to normal temperature.
Example 3
A method for preparing rare earth oxide by using microwave technology comprises the following steps:
(1) microwave drying: placing rare earth oxalate or rare earth carbonate into microwave equipment, starting microwave radiation with frequency of 915 MHz, heating to 140 deg.C at a heating rate of 28 deg.C/min, microwave drying for 15 min with power of 70 KW/m3Until the water content of rare earth oxalate or rare earth carbonate is 5 percent;
(2) microwave preheating: starting microwave frequency of 2.45 GHz, heating to 300 deg.C at a heating rate of 18 deg.C/min, microwave preheating for 60 min, and power of 150 KW/m3Until the water content of the rare earth oxalate or rare earth carbonate is 0;
(3) microwave firing: starting microwave frequency at 5.80 GHz, heating to 700 deg.C at a heating rate of 8 deg.C/min, microwave burning for 40 min at a power of 250 KW/m3；
(4) Gradient air cooling: in the air cooling process, the cooling speed is 5 ℃/min for 0-20 min, 20 ℃/min for 21-40 min, and 25 ℃/min after 41 min, and the rare earth oxide is obtained after air cooling is continued for 10 min after the temperature is reduced to normal temperature.
Example 4
A method for preparing rare earth oxide by using microwave technology comprises the following steps:
(1) microwave drying: placing rare earth oxalate or rare earth carbonate into microwave equipment, starting microwave radiation with frequency of 915 MHz, heating to 130 deg.C at a heating rate of 26 deg.C/min, microwave drying for 25 min with power of 70 KW/m3Until the water content of rare earth oxalate or rare earth carbonate is 4 percent;
(2) microwave preheating: starting microwave frequency of 2.45 GHz, heating to 450 deg.C at a heating rate of 16 deg.C/min, preheating for 45 min with microwave, and power of 170 KW/m3Until the water content of the rare earth oxalate or rare earth carbonate is 0;
(3) microwave firing: starting the microwave frequency at 5.80 GHz, heating to 750 deg.C at a heating rate of 6 deg.C/min, microwave-burning for 35 min at a power of 250 KW/m3；
(4) Gradient air cooling: in the air cooling process, the cooling speed of 0-20 min is 8 ℃/min, the cooling speed of 21-40 min is 16 ℃/min, the cooling speed after 41 min is 28 ℃/min, and air cooling is continued for 20 min after the temperature is reduced to the normal temperature, so that the rare earth oxide is obtained.
Example 5
A method for preparing rare earth oxide by using microwave technology comprises the following steps:
(1) microwave drying: placing rare earth oxalate or rare earth carbonate into microwave equipment, starting microwave radiation with frequency of 915 MHz, heating to 135 deg.C at a heating rate of 26 deg.C/min, microwave drying for 25 min with power of 90 KW/m3Until the water content of rare earth oxalate or rare earth carbonate is 3 percent;
(2) microwave preheating: starting microwave frequency of 2.45 GHz, heating to 350 deg.C at a heating rate of 16 deg.C/min, microwave preheating for 40 min, and power of 160 KW/m3Until the water content of the rare earth oxalate or rare earth carbonate is 0;
(3) microwave firing: starting microwave frequency at 5.80 GHz, heating to 850 deg.C at a rate of 6 deg.C/min, microwave-burning for 45 minThe rate is 260 KW/m3；
(4) Gradient air cooling: in the air cooling process, the cooling speed of 0-20 min is 6 ℃/min, the cooling speed of 21-40 min is 16 ℃/min, the cooling speed after 41 min is 26 ℃/min, and the air cooling is continued for 10-20 min after the temperature is reduced to the normal temperature, so that the rare earth oxide is obtained.
The technical effects of examples 1 to 5 of the present invention are shown in table 1:
TABLE 1 Performance parameters of rare earth oxides prepared in examples 1-5
As shown in Table 1, the average grain diameter D50 of the rare earth oxide product of the invention is 0.5-2.0 μm, the grain size distribution (D90-D10)/(2D50) is less than or equal to 1, and the specific surface grain size is controlled to be 4-7m2Per g, the performance is very good. The overall performance of the rare earth oxide of example 2 is slightly better than that of example 1, and then the firing temperature of 1000 ℃ in example 2 is higher, which causes 1.2% of agglomeration phenomenon in the sample, and meanwhile, from the viewpoint of saving energy consumption, example 1 is a preferred scheme of the present invention. It should be noted that the embodiments 1 to 5 are not intended to limit the scope of the present invention, and other combinations of process parameters based on the schemes of the present invention are also within the scope of the present invention.
Claims (1)
1. A method for preparing rare earth oxide by using microwave technology is characterized by comprising the following steps:
(1) microwave drying: placing rare earth oxalate into microwave equipment, starting microwave radiation with frequency of 915 MHz, heating to 130 deg.C at a heating rate of 25 deg.C/min, microwave drying for 20 min with power of 80 KW/m3Until the water content of rare earth oxalate is 3%;
(2) microwave preheating: starting microwave frequency of 2.45 GHz, heating to 400 deg.C at a rate of 15 deg.C/min, microwave preheating for 30 min, and power of 160 KW/m3Until the water content of the rare earth oxalate is 0;
(3) microwave firing: starting microwave frequency at 5.80 GHz, heating to 950 deg.C at a rate of 5 deg.C/min, microwave-burning for 50 min at a power of 280 KW/m3；
(4) Gradient air cooling: in the air cooling process, the cooling speed is 5 ℃/min for 0-20 min, 15 ℃/min for 21-40 min, and 25 ℃/min after 41 min, and the rare earth oxide is obtained after air cooling is continued for 15 min after the temperature is reduced to normal temperature.
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| CN114180613B (en) | 2021-12-13 | 2024-04-12 | 包头稀土研究院 | Method for preparing rare earth oxide by recycling ammonia and carbon and application of rare earth oxide |
| CN115010163B (en) * | 2022-05-20 | 2024-04-09 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
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| CN101113010A (en) * | 2007-07-04 | 2008-01-30 | 北京化工大学 | Method for preparing cerium oxide nano particle by auxiliary microwave |
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Address after: 532200 Industrial Road East 8, Chongzuo City Industrial Zone, the Guangxi Zhuang Autonomous Region Patentee after: Guangxi Guosheng rare earth new material Co.,Ltd. Patentee after: CHINALCO GUANGXI NONFERROUS RARE EARTH DEVELOPMENT CO.,LTD. Address before: 532200 Industrial Road East 8, Chongzuo City Industrial Zone, the Guangxi Zhuang Autonomous Region Patentee before: CHINALCO GUANGXI GUOSHENG RARE EARTH DEVELOPMENT CO.,LTD. Patentee before: CHINALCO GUANGXI NONFERROUS RARE EARTH DEVELOPMENT CO.,LTD. |