JPH01201029A - Production of molybdenum dioxide from molybdate-containing aqueous solution - Google Patents
Production of molybdenum dioxide from molybdate-containing aqueous solutionInfo
- Publication number
- JPH01201029A JPH01201029A JP2488588A JP2488588A JPH01201029A JP H01201029 A JPH01201029 A JP H01201029A JP 2488588 A JP2488588 A JP 2488588A JP 2488588 A JP2488588 A JP 2488588A JP H01201029 A JPH01201029 A JP H01201029A
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- molybdate
- water
- molybdenum dioxide
- reaction
- 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.)
- Granted
Links
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 11
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 16
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 8
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、モリブデン酸塩含有水溶液から二酸化モリブ
デンを製造する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing molybdenum dioxide from an aqueous solution containing molybdate.
二酸化モリブデン（Ｍ ｏ Ｏｚ）の製造は、工業的に
はパラモリブデン酸アンモニウムや酸化モリブデンを水
素で還元する方法で一般に還元は２段階に行われる。第
１段階は、６００℃〜８００℃で次の反応が起こる
Ｍ ｏ ０３ ＋ Ｈｚ ”Ｍ ｏ Ｏｘ ＋ Ｈｚ
０第２段階は１，１００℃〜１ 、２００℃で次の反応
が起きる
ＭｏＯ□＋２ Ｈｚ Ｏ−Ｍｏ ＋ ２１１ｚ Ｏ〔発
明が解決しようとする問題点〕
従来の方法でＭｏｏｔの製造は水素雰囲気中で６００℃
〜８００℃の反応温度で８時間程度を要する。Molybdenum dioxide (M o Oz) is produced industrially by reducing ammonium paramolybdate or molybdenum oxide with hydrogen, and the reduction is generally carried out in two stages. In the first stage, the following reaction occurs at 600°C to 800°C.
0 In the second stage, the following reaction occurs at 1,100°C to 1,200°C. 600℃ inside
It takes about 8 hours at a reaction temperature of ~800°C.
また、加圧水素による方法も研究され報告されているが
、いずれも酸性側でアルカリ性溶液からは還元率が低い
、高純度への精製及び反応装置の腐蝕の点等から中性も
しくはアルカリ性での還元法が研究課題とされている。In addition, methods using pressurized hydrogen have been researched and reported, but both methods are acidic and have a low reduction rate from alkaline solutions, and from the viewpoint of purification to high purity and corrosion of the reaction equipment, reduction in neutral or alkaline conditions is recommended. law is considered a research topic.
本発明の方法によれば、密閉反応容器を用いてモリブデ
ン酸塩含有水溶液にヒドラジン又はアスコルビン酸を加
え、水と任意の割合で溶解する水溶性有機溶媒を添加し
、２３０℃〜２７０℃の蒸気圧下で、二酸化モリブデン
を製造する方法で、水素ガスを使用しないことを特徴と
する特
本発明で用いる水溶性有機溶媒としては、水と任意に混
ざり、水溶液中からモリブデンを沈澱させ得るものであ
ればよく、このようなものとしては、低級アルコールや
アセトン等が挙げられる。According to the method of the present invention, hydrazine or ascorbic acid is added to a molybdate-containing aqueous solution using a closed reaction vessel, a water-soluble organic solvent that dissolves in water in an arbitrary ratio is added, and steam at 230 ° C to 270 ° C. A method for producing molybdenum dioxide under pressure, characterized by not using hydrogen gas.The water-soluble organic solvent used in the present invention may be any solvent that can mix with water and precipitate molybdenum from an aqueous solution. Examples of such substances include lower alcohols and acetone.
この水溶性有機溶媒は、ヒドラジン又はアスコルビン酸
の添加前、添加後、あるいは同時に添加することができ
、このものの添加により、モリブデン酸塩含有水溶液か
ら、モリブデン酸塩が沈澱する。本発明では、このよう
なモリブデン酸塩をヒドラジン又はアスコルビン酸の存
在下で２３０℃〜２７０℃の蒸気圧下で反応させて二酸
化モリブデンに還元する。The water-soluble organic solvent can be added before, after, or simultaneously with the addition of hydrazine or ascorbic acid, and its addition precipitates molybdate from the molybdate-containing aqueous solution. In the present invention, such a molybdate is reduced to molybdenum dioxide by reacting it in the presence of hydrazine or ascorbic acid under a vapor pressure of 230°C to 270°C.
本発明によると反応温度ばエネルギーの消費が従来の６
００℃〜８００℃が、２５０℃程度の温度ですむこと、
反応時間も８時間程度要したのが、２時間〜３時間です
むこと、高価な水素ガスを全く使用せず、添加物が還元
を行うものであるから、経済的にも大きな効果がある。According to the present invention, the reaction temperature and energy consumption are lower than the conventional 6
00℃~800℃, the temperature should be around 250℃,
The reaction time, which used to take about 8 hours, is now only 2 to 3 hours, and since expensive hydrogen gas is not used at all and the additive performs the reduction, there is a great economic effect.
また本発明は高純度モリブデンの製造に好適である。Further, the present invention is suitable for producing high-purity molybdenum.
Ｍ Ｏ？Ｑ度］００ｇｚｌのモリブデン酸アンモニウム
溶？＆２５０＋ｍｆに「ヒドラジン水和物５％／を添加
して攪拌した場合」と「アスコルビン酸５ｇを添加して
撹拌した場合」についてメタノールを液比１ ： ２
（５００ｍｆ）を添加しモリブデン酸塩を析出させた
状態（ｐＨＢ）で密閉反応装置に装入し、反応温度２５
０℃、反応時間１５０分、７００ｒｐｍの条件で反応を
行い、反応溶液を固液分離し、析出物とる液を分析した
結果、析出物についてはＸ線回折の結果、ヒドラジン水
和物添加の場合と、アスコルビン酸添加の場合、いずれ
もＭｏｏｔの極めて強い回折線のみが表れＭｏＯ□に還
元されていた。ろ液（ｐＨ９，２）についても双方のＭ
Ｏは検出されず、モリブデン酸塩含有水ｔｇｆｉ中のＭ
ｏのすべてがＭｏｏｔに完全に還元されていることが明
らかとなった。MO? Q degree] 00gzl of ammonium molybdate solution? &250+mf with methanol in a liquid ratio of 1:2 for "when 5% hydrazine hydrate was added and stirred" and "when 5g of ascorbic acid was added and stirred"
(500mf) was added to precipitate molybdate (pHB), and the mixture was charged into a closed reactor, and the reaction temperature was 25°C.
The reaction was carried out at 0°C, reaction time 150 minutes, and 700 rpm, the reaction solution was separated into solid and liquid, and the precipitate was analyzed. In both cases, when ascorbic acid was added, only the extremely strong diffraction line of Moot appeared, indicating that it was reduced to MoO□. Regarding the filtrate (pH 9,2), both M
No O was detected, and M in molybdate-containing water tgfi
It became clear that all of o was completely reduced to Moot.
〔比 較 例〕 １
Ｍ ｏ ？Ｑ度１００ｇ／ｌのモリブデン酸アンモニウ
ム溶液２５０ｍｆにメタノールを液比１ ： ２ （５
００１０を添加しモリブデン酸塩を析出させた状態で密
閉反応装置に装入し、反応温度２５０℃、反応時間１５
０分、７００ｒｐｍの条件で反応を行い、反応溶液を固
液分離し、析出物とる液を分析し、析出物についてはＸ
線回折の結果、Ｍｏｂ、への還元は７０χとなった。[Comparison example] 1 Mo? Mix 250 mf of ammonium molybdate solution with a Q degree of 100 g/l with methanol in a liquid ratio of 1:2 (5
0010 was added to precipitate the molybdate, the mixture was charged into a closed reactor, and the reaction temperature was 250°C and the reaction time was 15.
The reaction was carried out under the conditions of 0 minutes and 700 rpm, the reaction solution was separated into solid and liquid, and the liquid containing the precipitate was analyzed.
As a result of line diffraction, the reduction to Mob was 70χ.
〔比 較 例〕２
Ｍ ｏ ｆｌ１度１００ｇ／ｌのモリブデン酸アンモニ
ウム溶液２５０ｓ１にヒドラジン５ＩＩｌを添加しＨ。[Comparative Example] 2 Mo fl: Add 5IIl of hydrazine to 250sl of 100g/l ammonium molybdate solution.
Ｏを液比１ ： ２ （５００ｍｊりを加えて密閉反応
装置に装入し、反応温度２５０℃、反応時間１５０分、
７００ｒｐ−の条件で反応を行い反応溶液を固液分離し
、析出物とる液を分析し、析出物についてはＸ線回訴の
結果Ｍ ｏ Ｏ□への還元は３１χとなった。O was added at a liquid ratio of 1:2 (500 mj) and charged into a closed reactor, reaction temperature was 250°C, reaction time was 150 minutes,
The reaction was carried out under the conditions of 700 rp-, the reaction solution was separated into solid and liquid, and the liquid containing the precipitate was analyzed. Regarding the precipitate, the reduction to M o O□ was 31χ as a result of X-ray analysis.
Claims (1)
を製造する場合、モリブデン酸塩含有水溶液にヒドラジ
ン又はアスコルビン酸と、水溶性有機溶媒を添加し密閉
容器を用いて２３０℃〜２７０℃で反応させるモリブデ
ン酸塩含有水溶液から二酸化モリブデンの製造法。(1) When producing molybdenum dioxide from a molybdate-containing aqueous solution, hydrazine or ascorbic acid and a water-soluble organic solvent are added to the molybdate-containing aqueous solution, and molybdic acid is reacted at 230°C to 270°C in a closed container. A method for producing molybdenum dioxide from a salt-containing aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63024885A JPH0623046B2 (en) | 1988-02-04 | 1988-02-04 | Method for producing molybdenum dioxide from molybdate-containing aqueous solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63024885A JPH0623046B2 (en) | 1988-02-04 | 1988-02-04 | Method for producing molybdenum dioxide from molybdate-containing aqueous solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01201029A true JPH01201029A (en) | 1989-08-14 |
| JPH0623046B2 JPH0623046B2 (en) | 1994-03-30 |
Family
ID=12150642
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63024885A Expired - Lifetime JPH0623046B2 (en) | 1988-02-04 | 1988-02-04 | Method for producing molybdenum dioxide from molybdate-containing aqueous solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0623046B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | A kind of method adopting solvothermal method to prepare MoS2 microspheres |
| CN114471442A (en) * | 2021-12-20 | 2022-05-13 | 广东省科学院资源利用与稀土开发研究所 | Nano dye wastewater adsorption material and preparation method thereof |
-
1988
- 1988-02-04 JP JP63024885A patent/JPH0623046B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | A kind of method adopting solvothermal method to prepare MoS2 microspheres |
| CN114471442A (en) * | 2021-12-20 | 2022-05-13 | 广东省科学院资源利用与稀土开发研究所 | Nano dye wastewater adsorption material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0623046B2 (en) | 1994-03-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |