JPS62132731A - Production of rare earth metal oxide - Google Patents
Production of rare earth metal oxideInfo
- Publication number
- JPS62132731A JPS62132731A JP60273033A JP27303385A JPS62132731A JP S62132731 A JPS62132731 A JP S62132731A JP 60273033 A JP60273033 A JP 60273033A JP 27303385 A JP27303385 A JP 27303385A JP S62132731 A JPS62132731 A JP S62132731A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- earth metal
- hydroxide
- metal oxide
- heating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 14
- -1 rare earth hydroxide Chemical class 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 230000001678 irradiating effect Effects 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 2
- 230000005855 radiation Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 9
- 230000008021 deposition Effects 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 150000004679 hydroxides Chemical class 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 241000252233 Cyprinus carpio Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明は、水酸化希土から容易に短時間で酸化希土を得
る方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for easily obtaining rare earth oxide from rare earth hydroxide in a short time.
希土類元素は、従来から金属、セラミックの改質材、ガ
ラス工業への利用など多くの産業分野に使用されている
が、特に最近では電子材料、磁性材料、光学材料などの
先端技術分野で急速に需要が増加しつつある。Rare earth elements have traditionally been used in many industrial fields, such as as modifiers for metals and ceramics, and in the glass industry, but recently they have been rapidly used in cutting-edge technology fields such as electronic materials, magnetic materials, and optical materials. Demand is increasing.
希土類元素は活性が非常に強いため、金属として凰m
+ /、?−シは田靴で一→舎蛍鮒1.イ&巧めイネ安
定であるので工業的にはその用途に応じて、水酸化物、
酸化物、塩化物、炭酸塩などの種々の中間化合物として
通常増り扱われる。その中でも酸化物は一定の組成の純
度の高いものが得られるために最も一般的な化合物とな
っている。Rare earth elements have very strong activity, so they are used as metals.
+/、? - Shi is Tasutode 1 → Sha Hotaru Carp 1. Because rice is stable, hydroxide,
It is commonly treated as a variety of intermediate compounds such as oxides, chlorides, and carbonates. Among these, oxides are the most common compounds because they can be obtained with a certain composition and high purity.
(従来の技術)
従来、希土類酸化物は希土類のシュウ酸塩、炭酸塩、水
酸化物を電気加熱炉やロータリーキルン等のガス加熱炉
で加熱焼成して製造している。そのうち、シュウ酸希土
は焼成温度が900℃以上と高いが高度に精製された酸
化希土が得られるため、高純度酸化希土の原料としてよ
く用いられている。一方、水酸化希土を原料とする場合
は不純物が入り易いという難点はあるが、比較的低い温
度で焼成できるため、希土類の中間化合物として製造の
種々の段階で有利に取り扱われる。(Prior Art) Conventionally, rare earth oxides have been produced by heating and baking rare earth oxalates, carbonates, and hydroxides in an electric heating furnace or a gas heating furnace such as a rotary kiln. Among these, oxalic acid rare earth has a high firing temperature of 900° C. or higher, but highly purified rare earth oxide can be obtained, so it is often used as a raw material for high purity rare earth oxide. On the other hand, when rare earth hydroxide is used as a raw material, it has the disadvantage that impurities easily enter, but because it can be fired at a relatively low temperature, it is advantageously used as a rare earth intermediate compound at various stages of production.
しかしながらどの原料を用いても、酸化希土類を得るた
めには、電気加熱またはガス加熱が必要で特にパッチ操
作で焼成を行なう場合、電気炉では、昇温、加熱に時間
がかかり、またガス加熱の場合も多少時間は短縮される
とはいえ操作に手間がかかり、エネルギー効率も悪く工
業的に有利な方法とは云えない。However, no matter which raw material is used, in order to obtain rare earth oxides, electric heating or gas heating is required. Particularly when firing is performed by patch operation, it takes time to raise the temperature and heat in an electric furnace, and gas heating is required. In this case, although the time is somewhat shortened, the operation is laborious and the energy efficiency is poor, so it cannot be said to be an industrially advantageous method.
(発明が解決しようとする問題点)
本発明は酸化着出を短時間に容易に効率よく得る方法に
関するものである。(Problems to be Solved by the Invention) The present invention relates to a method for easily and efficiently obtaining oxidation deposition in a short time.
本発明者等は、上記の目的を達成するため種々検討を加
えてきたが、特に原料として水酸化積土を用いた場合、
原料が乾燥状態、含水状態の何れの状態でもマイクロ波
を吸収し、短時間に高温状態になって酸化着出まで容易
に効率よく焼成できることを見出し本発明に到達した。The present inventors have made various studies to achieve the above objective, but in particular, when using hydroxide soil as a raw material,
The present invention was achieved by discovering that the raw material absorbs microwaves in both dry and hydrated states, reaches a high temperature in a short period of time, and can be fired easily and efficiently until oxidation deposition occurs.
(問題点を解決するための手段)
本発明の要旨は希土類水酸化物、特に含水状態の水酸化
物にマイクロ波を照射することにより、赤熱状態に加熱
し希土類酸化物を得る方法である。(Means for Solving the Problems) The gist of the present invention is a method of obtaining rare earth oxides by heating rare earth hydroxides, particularly hydroxides in a water-containing state, to a red-hot state by irradiating them with microwaves.
照射するマイクロ波の周波数は、300MHz 〜30
0GHz の範囲で実施可能であるが、一般に工業的に
使用が許可されている周波数2,450MHzのマイク
ロ波を使用するのが有利であり好ましい。The frequency of the microwave to irradiate is 300MHz to 30MHz.
Although it can be carried out in the range of 0 GHz, it is advantageous and preferred to use microwaves with a frequency of 2,450 MHz, which is generally allowed for industrial use.
原料の水酸化物にマイクロ波を照射すると700℃以上
、局部的にはi、ooo℃以上に加熱される。When the raw material hydroxide is irradiated with microwaves, it is heated to 700°C or higher, locally to i,ooo°C or higher.
照射時間は原料の含水量により多少の変動はあるが、通
常数十分保てば容易に酸化物が得られる。Although the irradiation time varies somewhat depending on the water content of the raw materials, oxides can be easily obtained if the irradiation time is kept for several tens of minutes.
原料の水酸化積土は通常水溶液からの沈殿物の形で得ら
れるため、含水状態で処理する場合が多く、この場合本
発明の方法は特に有利に実施できる。Since the raw material hydroxide pile is usually obtained in the form of a precipitate from an aqueous solution, it is often treated in a water-containing state, and in this case the method of the present invention can be carried out particularly advantageously.
本発明の方法を適用できる希土類としては、希土類元素
各単味の水酸化積土でもよく、またそれらの混合物でも
同様に処理できる。また製錬の工程で希土類元素の水酸
化物の中に他の金属の水酸化物が混合して来る場合があ
るが、この場合でも本発明の方法により上述の場合と同
様に、有利に実施でき次工程への中間原料として取り扱
うことができる。The rare earths to which the method of the present invention can be applied may be hydroxide piles of individual rare earth elements, or mixtures thereof can be treated in the same manner. In addition, in the smelting process, hydroxides of other metals may be mixed into the hydroxides of rare earth elements, but even in this case, the method of the present invention can be advantageously implemented in the same way as in the above case. It can be treated as an intermediate raw material for the next process.
本発明を実施する場合、バッチ式でも連続式でも実施可
能であるが、バッチ式の方が簡単な加熱装置を使用する
ことができるため有利である。次に本発明の実施態様を
よシ明確に示すため実施例をあげて説明する。The present invention can be carried out either batchwise or continuously, but the batchwise method is more advantageous because a simpler heating device can be used. Next, in order to more clearly illustrate the embodiments of the present invention, examples will be given and explained.
(実施例1)
アルミナ製容器に混合水酸化希±2.1Kg(酸化着出
として1.8 K9 ) を入れ、これを断熱材で覆
いマイクロ波加熱装置中にセットした。出力5KWで周
波数2,450MHz のマイクロ波を50分照射し、
得られた酸化物を冷却後、重量測定したところ1、8
K、、であり、はぼ定量的に酸化着出が得られた。(Example 1) Mixed diluted hydroxide ±2.1 kg (1.8 K9 as oxidation deposition) was placed in an alumina container, which was covered with a heat insulating material and set in a microwave heating device. Irradiate microwaves with an output of 5KW and a frequency of 2,450MHz for 50 minutes.
After cooling the obtained oxide, the weight was measured and it was found to be 1,8
K, and oxidation deposition was obtained almost quantitatively.
(実施例2)
アルミナ製容器に含水状態の混合水酸化希±2、0 K
g(酸化着出として1.1 K9 )を入れ、実施例1
と同様にして出力5Kll/、周波数4450MHz
のマイクロ波を70分照射し、得られた酸化物を冷却後
、重量測定したところ1.1 Kgでほぼ定量的に酸化
着出が得られた。(Example 2) Mixed hydroxide diluted in a water-containing state in an alumina container ±2,0 K
Example 1
Similarly, output 5Kll/, frequency 4450MHz
Microwave irradiation was performed for 70 minutes, and the resulting oxide was cooled and then weighed to find that the weight was 1.1 kg, indicating that oxidation deposition was almost quantitative.
(実施例3)
アルミナ製容器に含水状態の水酸化セリウム2、1 K
t (酸化セリウムとして1.2 KFりを入れ、実施
例1と同様に5KW、周波数2,450 MHz )
−rイクロ波を60分照射得られた酸化物を冷却後、重
量測定したところ1.2 K9で、はぼ定量的に酸化セ
リウムが得られた。(Example 3) Hydrated cerium hydroxide 2.1 K in an alumina container
t (Added 1.2 KF as cerium oxide, 5 KW as in Example 1, frequency 2,450 MHz)
-r Microwave was irradiated for 60 minutes. After cooling the obtained oxide, the weight was measured, and the weight was 1.2 K9, and cerium oxide was obtained almost quantitatively.
(発明の効果)
本発明の方法では加熱にマイクロ波を利用しており、昇
温、加熱が従来から用いられている電気加熱炉やガス加
熱炉等に比べて短時間で行なえるため、効率よく短時間
で希土類酸化物を得ることができる。(Effects of the Invention) The method of the present invention uses microwaves for heating, and can raise the temperature and heat in a shorter time than conventionally used electric heating furnaces, gas heating furnaces, etc., so it is efficient. Rare earth oxides can be obtained in a short time.
また前記の従来から用いられている加熱装置は容積が大
きく、広い据付面積を要するが、本発明の方法による装
置は小型でコンパクトであるため工業的実施が非常に容
易である。従って効率よく安価に酸化着出を提供するこ
とができるため、希土類を利用する種々の進歩に大いに
寄与することができる。In addition, the conventionally used heating device described above has a large volume and requires a large installation area, but the device according to the method of the present invention is small and compact, so it is very easy to implement industrially. Therefore, since oxidation deposition can be provided efficiently and inexpensively, it can greatly contribute to various advances in the use of rare earths.
Claims (2)
法において、マイクロ波加熱を行なうことを特徴とする
酸化希土の製造方法。(1) A method for producing rare earth oxide by heating and firing rare earth hydroxide, the method comprising performing microwave heating.
(1)項記載の方法。(2) The method according to claim (1), wherein the raw rare earth hydroxide is in a hydrated state.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60273033A JPS62132731A (en) | 1985-12-03 | 1985-12-03 | Production of rare earth metal oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60273033A JPS62132731A (en) | 1985-12-03 | 1985-12-03 | Production of rare earth metal oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62132731A true JPS62132731A (en) | 1987-06-16 |
Family
ID=17522231
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60273033A Pending JPS62132731A (en) | 1985-12-03 | 1985-12-03 | Production of rare earth metal oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62132731A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5362459A (en) * | 1993-05-17 | 1994-11-08 | Pure-Etch Co. | Neodymium recovery process |
| WO1996000698A1 (en) * | 1994-06-28 | 1996-01-11 | Pure Etch Co. | Rare earth recovery process |
| CN100339305C (en) * | 2005-12-23 | 2007-09-26 | 浙江大学 | Microwave synthesis preparation method for praseodymium hydroxide nanometer rod |
| JP2014227334A (en) * | 2013-05-27 | 2014-12-08 | マイクロ波化学株式会社 | Method for producing fine particles of rare earth oxide and fine particles of rare earth oxide |
| CN106241852A (en) * | 2016-06-22 | 2016-12-21 | 中山大学 | A kind of preparation method of Pr(OH)3 one-dimensional nanorod |
| CN114524451A (en) * | 2021-12-17 | 2022-05-24 | 中国北方稀土(集团)高科技股份有限公司 | Method for preparing large-particle-size rare earth oxide by one-step microwave at low temperature |
-
1985
- 1985-12-03 JP JP60273033A patent/JPS62132731A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5362459A (en) * | 1993-05-17 | 1994-11-08 | Pure-Etch Co. | Neodymium recovery process |
| WO1994026665A1 (en) * | 1993-05-17 | 1994-11-24 | Pure-Etch Co. | Neodymium recovery process |
| WO1996000698A1 (en) * | 1994-06-28 | 1996-01-11 | Pure Etch Co. | Rare earth recovery process |
| CN100339305C (en) * | 2005-12-23 | 2007-09-26 | 浙江大学 | Microwave synthesis preparation method for praseodymium hydroxide nanometer rod |
| JP2014227334A (en) * | 2013-05-27 | 2014-12-08 | マイクロ波化学株式会社 | Method for producing fine particles of rare earth oxide and fine particles of rare earth oxide |
| CN106241852A (en) * | 2016-06-22 | 2016-12-21 | 中山大学 | A kind of preparation method of Pr(OH)3 one-dimensional nanorod |
| CN114524451A (en) * | 2021-12-17 | 2022-05-24 | 中国北方稀土(集团)高科技股份有限公司 | Method for preparing large-particle-size rare earth oxide by one-step microwave at low temperature |
| CN114524451B (en) * | 2021-12-17 | 2024-02-20 | 中国北方稀土(集团)高科技股份有限公司 | Method for preparing large-granularity rare earth oxide by one-step microwave at low temperature |
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