JPH02141429A - Method and apparatus for production of tungsten intermediate oxide - Google Patents
Method and apparatus for production of tungsten intermediate oxideInfo
- Publication number
- JPH02141429A JPH02141429A JP63293594A JP29359488A JPH02141429A JP H02141429 A JPH02141429 A JP H02141429A JP 63293594 A JP63293594 A JP 63293594A JP 29359488 A JP29359488 A JP 29359488A JP H02141429 A JPH02141429 A JP H02141429A
- Authority
- JP
- Japan
- Prior art keywords
- ammonium tungstate
- gaseous ammonia
- extracted
- ammonia gas
- intermediate oxide
- 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
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 17
- 239000010937 tungsten Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 238000000034 method Methods 0.000 title abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 239000007858 starting material Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 10
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 238000011949 advanced processing technology Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 5
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
-
- Y02W30/54—
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野コ
本発明は、タングステン中間酸化物の生成手段に関する
。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to means for producing tungsten intermediate oxide.
［従来の技術］
タングステン製品の原料となるタングステン粉末は、そ
の製造過程でいわゆる中間酸化物（Ｗ ２゜０５８＋
ｗ、８ｏ４．、 ＷＯ２、等）に生成される。[Prior Art] Tungsten powder, which is the raw material for tungsten products, is converted into so-called intermediate oxides (W2゜058+) during the manufacturing process.
w, 8o4. , WO2, etc.).
従来のこの種の中間酸化物の生成する手段として、三酸
化タングステン（ＷＯ３）や、タングステン酸アンモニ
ウム［５（ＮＨ４）２ ・０・１２ＷＯ，・５Ｈ２０、
以下ＡＰＴと略す］を出発原料とし、これを４５０℃〜
６００℃、水素ガス雰囲気の炉内で還元する方法が知ら
れている。Conventional methods for producing this type of intermediate oxide include tungsten trioxide (WO3), ammonium tungstate [5(NH4)2 .0.12WO, .5H20,
Hereinafter abbreviated as APT] is used as a starting material, and this is heated at 450℃~
A method of reduction in a furnace at 600° C. in a hydrogen gas atmosphere is known.
［発明が解決しようとする課題］
しかしながら、従来の還元法では、高価な水素ガスの使
用を必須とする為、還元に要する費用が高額となる問題
があった。三酸化タングステンを出発原料とする場合は
他に方法がないのでやむを得ないとしても、ＡＰＴの場
合には水素ガスを使用しなくとも、その組成成分に還元
性を有するアンモニアガス（ＮＨ３）を含む。これを還
元剤として利用すれば安価に中間酸化物が生成できるは
ずである。にも拘らずこの手段が用いられないのは、手
段自体に以下の重大な欠点がある為である。[Problems to be Solved by the Invention] However, the conventional reduction method requires the use of expensive hydrogen gas, so there is a problem in that the cost required for reduction is high. When using tungsten trioxide as a starting material, there is no other method, so even if it is unavoidable, in the case of APT, even if hydrogen gas is not used, its composition contains ammonia gas (NH3), which has reducing properties. If this is used as a reducing agent, it should be possible to produce intermediate oxides at low cost. However, this method is not used because the method itself has the following serious drawbacks.
例えば、炉の供給側を開放し、取り出し側を密閉し、炉
内にＡＰＴより抽出されるアンモニアガスを充満させ、
空気を断った状態で、中間酸化物を生成しようとすると
、抽出されたアンモニアガスの処理が難しく、前記炉の
開放口より大気中に放出され、環境汚染を招いてしまう
。また、中間酸化物を生成させる処理温度が高くなるた
め、後工程であるＷ粉およびＷＣ粉の製造工程で凝集等
の問題を生じることもある。For example, the supply side of the furnace is opened, the take-out side is sealed, and the furnace is filled with ammonia gas extracted from APT.
If an attempt is made to produce an intermediate oxide with the air cut off, the extracted ammonia gas will be difficult to treat and will be released into the atmosphere through the open port of the furnace, resulting in environmental pollution. Furthermore, since the processing temperature for producing intermediate oxides becomes high, problems such as agglomeration may occur in the subsequent process of producing W powder and WC powder.
一方、炉を完全に閉じた状態では、抽出され続けるアン
モニアガスの蓄積により炉内圧力が上昇し、非常に危険
な事態を招く。On the other hand, if the furnace is completely closed, the pressure inside the furnace increases due to the accumulation of ammonia gas that continues to be extracted, leading to a very dangerous situation.
そこで本発明の技術的課題は、環境汚染を招くことなく
、低コストかつ安全に中間酸化物を生成できるタングス
テン中間酸化物の生成方法及び該方法に適した生成装置
を提供することである。Therefore, a technical object of the present invention is to provide a method for producing a tungsten intermediate oxide that can safely produce an intermediate oxide at low cost without causing environmental pollution, and a production apparatus suitable for the method.
［課題を解決するための手段］
本発明によれば、タングステン酸アンモニウムを出発原
料とし、前記タングステン酸アンモニウムから抽出され
たアンモニアガスと前記タングステン酸アンモニウムと
を循還再結合させる一方、過剰に抽出された前記アンモ
ニアガスを液化回収する工程を有することを特徴とする
タングステン中間酸化物の生成方法が得られる。また、
本発明によればタングステン酸アンモニウムからアンモ
ニアガスを抽出させる抽出手段を有するタングステン中
間酸化物の生成装置において、前記抽出されたアンモニ
アガスと前記タングステン酸アンモニウムとを循還再結
合させる還元装置と、過剰に抽出された前記アンモニア
ガスを液化回収する回収装置とを含むことを特徴とする
タングステン中間酸化物の生成装置が得られる。[Means for Solving the Problems] According to the present invention, ammonium tungstate is used as a starting material, and while the ammonia gas extracted from the ammonium tungstate and the ammonium tungstate are recycled and recombined, excessive extraction is performed. There is obtained a method for producing a tungsten intermediate oxide, which comprises a step of liquefying and recovering the ammonia gas. Also,
According to the present invention, in the tungsten intermediate oxide production device having an extraction means for extracting ammonia gas from ammonium tungstate, a reduction device for circulating and recombining the extracted ammonia gas and the ammonium tungstate; and a recovery device for liquefying and recovering the ammonia gas extracted by the tungsten intermediate oxide.
［実施例コ 以下、本発明の実施例ついて説明する。[Example code] Examples of the present invention will be described below.
本実施例のタングステン中間酸化物の生成装置は、第１
図に示すように、出発原料たるＡＰＴから、その組成成
分たるアンモニアガスを抽出するための回転炉１と、抽
出された前記アンモニアガスを前記炉内に循還させ、前
記タングステン中間酸化物と再結合させると共に、過剰
なアンモニアガスを液化回収するための回収装置２とを
有する。The tungsten intermediate oxide generating device of this example has a first
As shown in the figure, there is a rotary furnace 1 for extracting ammonia gas as a component from APT as a starting material, and a rotary furnace 1 for circulating the extracted ammonia gas into the furnace and reproducing it with the tungsten intermediate oxide. It also has a recovery device 2 for liquefying and recovering excess ammonia gas.
ＡＰＴは、回転炉１の供給口１０からケーシング１１内
に供給される。ケーシング１１内には供給物を回転運搬
可能にスクリューフィーダ１２が配設されており、前記
ＡＰＴはこのスクリューフィーダ１２に保持されつつ順
次、回転管１４内を通過する。炉体１３は加熱装置（図
示せず）によって所定の温度に保たれており、通過する
ＡＰＴを加熱する。かかる熱によりＡＰＴからまずアン
モニアガスと水が抽出される。このアンモニアガスは還
元性を有するため、再びＡＰＴと結合し水蒸気を発生さ
せる。これらアンモニアガスと水蒸気は、循環ファン２
２により回転管１４の入口側より吸引され、回収装置２
に回収される。回収装置２では、飛散品回収装置２１で
飛散品を除去した後、循還ファン２３、炉内圧力調整器
２４を介して、循還するアンモニアガスを前記回転管１
４の出口側に供給する。炉内圧力調整器２４は、例えば
、水（外部より供給）の中にアンモニアガスを導くパイ
プを差し込み、その差込長さによって圧力を調整するも
のである。これにより、回転管１４内には一定の圧力の
アンモニアガスが循還することになり、ＡＰＴの還元作
用が安全、確実に行われることになる。APT is supplied into the casing 11 from the supply port 10 of the rotary furnace 1 . A screw feeder 12 is disposed within the casing 11 so as to be able to rotatably transport the feed, and the APTs are held by the screw feeder 12 and sequentially pass through the rotary tube 14 . The furnace body 13 is maintained at a predetermined temperature by a heating device (not shown) and heats the APT passing therethrough. The heat first extracts ammonia gas and water from the APT. Since this ammonia gas has reducing properties, it combines with APT again to generate water vapor. These ammonia gas and water vapor are transferred to the circulation fan 2
2 from the inlet side of the rotating tube 14, and the recovery device 2
will be collected. In the collection device 2, after the scattered products are removed by the scattered product collection device 21, the circulating ammonia gas is sent to the rotary tube 1 via the circulation fan 23 and the furnace pressure regulator 24.
4 to the outlet side. The in-furnace pressure regulator 24 is configured, for example, by inserting a pipe for introducing ammonia gas into water (supplied from the outside) and adjusting the pressure depending on the length of the insertion. As a result, ammonia gas at a constant pressure is circulated within the rotary tube 14, and the reducing action of APT is carried out safely and reliably.
一方、過剰に抽出されたアンモニアガスは水蒸気と一緒
に、前記飛散品回収装置２１に接続されたガス冷却器２
２で冷却され、アンモニア水として液化回収される。ま
た、前記炉内圧力調整器２４で圧力調整の際、水に溶け
ずに回収されなかったアンモニアガスはアブソーバ２５
で水（外部より供給）に吸収され、排水と排気とに分離
される。On the other hand, the excessively extracted ammonia gas is collected together with water vapor in a gas cooler 2 connected to the scattered product collection device 21.
2, and is liquefied and recovered as aqueous ammonia. Furthermore, when the pressure is adjusted by the furnace pressure regulator 24, the ammonia gas that is not dissolved in water and is not recovered is removed by the absorber 25.
It is absorbed by water (supplied from outside) and separated into waste water and exhaust.
尚、本実施例では、ＡＰＴとアンモニアガスの循還再結
合と液化回収とを回収装置２を用いて行うこととしたが
、両者を別装置に構成しても良い。In this embodiment, the recycling and recombination and liquefaction recovery of APT and ammonia gas are performed using the recovery device 2, but the two may be configured as separate devices.
この様に、本実施例では、スクリューフィーダ１２に保
持されたＡＰＴが回転管１４を通過する間に水蒸気とア
ンモニアガスと中間酸化物とに分離する構成とした。し
かも、いわゆる自発生ガスであるアンモニアガスを循還
させ還元用ガスとして用い、かつ過剰のアンモニアガス
は液化して回収する手段を設けたので、従来の様に水素
ガスを用いる必要がないから低コスト化できた。また、
炉体１３の温度も所要の中間酸化物の特性（組成）に応
じて自由に変えられるようになった。この構成では、抽
出されたアンモニアガスは、還元に消費されたものを含
めると、９５％以上回収できるし、アブソーバ２５で分
離された排気ガス中のアンモニア濃度はＩＯＰＰＭ以下
、排水中のアンモニア濃度はＩｇ／ρ以下であった。In this way, this embodiment has a configuration in which the APT held in the screw feeder 12 is separated into water vapor, ammonia gas, and intermediate oxide while passing through the rotating tube 14. Moreover, since we have installed a means to circulate ammonia gas, which is a so-called naturally occurring gas, and use it as a reducing gas, and to liquefy and recover excess ammonia gas, there is no need to use hydrogen gas as in the past, resulting in low energy consumption. We were able to reduce the cost. Also,
The temperature of the furnace body 13 can also be changed freely according to the properties (composition) of the required intermediate oxide. With this configuration, more than 95% of the extracted ammonia gas, including that consumed in reduction, can be recovered, the ammonia concentration in the exhaust gas separated by the absorber 25 is less than IOPPM, and the ammonia concentration in the waste water is It was below Ig/ρ.
尚、本実施例の構成に基づき、前記回転体１４の温度を
４５０℃〜６６０℃として生成されたタングステン中間
酸化物の特性値を第１表に示す。Table 1 shows the characteristic values of the tungsten intermediate oxide produced based on the configuration of this embodiment and the temperature of the rotating body 14 being 450 DEG C. to 660 DEG C.
［発明の効果コ
以上の説明のとおり、本発明によれば、環境汚染を招く
ことなく、低コスト、かつ、安全に中間酸化物を生成で
きるタングステン中間酸化物の生成方法、及び、該方法
に適した生成装置が提供できる。[Effects of the Invention] As explained above, the present invention provides a method for producing a tungsten intermediate oxide that can safely produce an intermediate oxide at low cost without causing environmental pollution, and a method for producing a tungsten intermediate oxide. A suitable generator can be provided.
第１図は、本実施例に係るタングステン中間酸化物の生
成装置の概略構成図を示す。
図中、１：回転炉、２：回収装置、２１：飛散品回収装
置、２２：ガス冷却器、２３：循還ファン、２４：炉内
圧力調整器、２５：アブソーバ。FIG. 1 shows a schematic diagram of a tungsten intermediate oxide production apparatus according to this embodiment. In the figure, 1: rotary furnace, 2: recovery device, 21: scattered product recovery device, 22: gas cooler, 23: circulation fan, 24: furnace pressure regulator, 25: absorber.
Claims (2)
記タングステン酸アンモニウムから抽出されたアンモニ
アガスと前記タングステン酸アンモニウムとを循還再結
合させる一方、過剰に抽出された前記アンモニアガスを
液化回収する工程を有することを特徴とするタングステ
ン中間酸化物の生成方法。(1) Using ammonium tungstate as a starting material, the ammonia gas extracted from the ammonium tungstate and the ammonium tungstate are recycled and recombined, and the ammonia gas extracted in excess is liquefied and recovered. A method for producing a tungsten intermediate oxide, characterized by:
を抽出させる抽出手段を有するタングステン中間酸化物
の生成装置において、前記抽出されたアンモニアガスと
前記タングステン酸アンモニウムとを循還再結合させる
還元装置と、過剰に抽出された前記アンモニアガスを液
化回収する回収装置とを含むことを特徴とするタングス
テン中間酸化物の生成装置。(2) A tungsten intermediate oxide production device having an extraction means for extracting ammonia gas from ammonium tungstate, including a reduction device for circulating and recombining the extracted ammonia gas and the ammonium tungstate; and a recovery device for liquefying and recovering the ammonia gas produced.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63293594A JPH02141429A (en) | 1988-11-22 | 1988-11-22 | Method and apparatus for production of tungsten intermediate oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63293594A JPH02141429A (en) | 1988-11-22 | 1988-11-22 | Method and apparatus for production of tungsten intermediate oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02141429A true JPH02141429A (en) | 1990-05-30 |
Family
ID=17796740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63293594A Pending JPH02141429A (en) | 1988-11-22 | 1988-11-22 | Method and apparatus for production of tungsten intermediate oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02141429A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380618A (en) * | 2011-11-10 | 2012-03-21 | 北京科技大学 | Method for preparing nano-tungsten powder by using sulfuric acid precipitation-H2 breathable reduction process |
| CN105016393A (en) * | 2015-08-07 | 2015-11-04 | 江西稀有金属钨业控股集团有限公司 | System and method for preparing blue tungsten high in specific surface area |
| CN109368661A (en) * | 2018-11-28 | 2019-02-22 | 湖南懋天世纪新材料有限公司 | Surplus NH in alkalinity extraction tungsten production4+Utilization method |
| CN111672152A (en) * | 2020-06-05 | 2020-09-18 | 江西智府科技有限公司 | Method and equipment for recycling ammonia gas in ammonium paratungstate production |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5092806A (en) * | 1973-12-20 | 1975-07-24 |
-
1988
- 1988-11-22 JP JP63293594A patent/JPH02141429A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5092806A (en) * | 1973-12-20 | 1975-07-24 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380618A (en) * | 2011-11-10 | 2012-03-21 | 北京科技大学 | Method for preparing nano-tungsten powder by using sulfuric acid precipitation-H2 breathable reduction process |
| CN105016393A (en) * | 2015-08-07 | 2015-11-04 | 江西稀有金属钨业控股集团有限公司 | System and method for preparing blue tungsten high in specific surface area |
| CN109368661A (en) * | 2018-11-28 | 2019-02-22 | 湖南懋天世纪新材料有限公司 | Surplus NH in alkalinity extraction tungsten production4+Utilization method |
| CN111672152A (en) * | 2020-06-05 | 2020-09-18 | 江西智府科技有限公司 | Method and equipment for recycling ammonia gas in ammonium paratungstate production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4288420A (en) | Removal of nitrogen oxides and sulfur oxides by ammonia | |
| CN108793244B (en) | Method for preparing titanium dioxide by metatitanic acid double-section rotary kiln calcination | |
| JP2002516169A (en) | How to treat flue gas | |
| ES453114A1 (en) | Method and apparatus for recovering by-product silt fines from a slurry thereof | |
| CN110975578A (en) | Three-waste zero-emission nanoparticle supercritical hydrothermal synthesis system and method | |
| JPH02141429A (en) | Method and apparatus for production of tungsten intermediate oxide | |
| CN105948123A (en) | High-efficiency method for preparing low-sulfur molybdenum trioxide from molybdenite by roasting | |
| CN105423315B (en) | Coal chemical industry is vented the recoverying and utilizing method of waste gas | |
| CN115820303A (en) | Cooling dechlorination and heat recovery blast furnace gas desulfurization system and process | |
| EP0625957B1 (en) | Acid regeneration | |
| JPH02141428A (en) | Method and device for forming intermediate oxide of molybdenum | |
| CN106672920B (en) | A kind of method that room temperature liquid phase prepares selenium sulphur solid solution | |
| US5007960A (en) | Method for removing chromium from chromium containing waste material | |
| US3113086A (en) | Production of o2 from co2 by electric arc or radiant energy | |
| CN210399877U (en) | Material drying system | |
| CN211823776U (en) | External heating type rotary kiln for calcining carbonate minerals and waste heat recovery system | |
| US4596698A (en) | Apparatus for utilizing impure steam with extraction of one or more substances therefrom | |
| CN103880651B (en) | Reaction of high order prepares method and the device of oxoethanoic acid | |
| CN111076536A (en) | External heating type rotary kiln for calcining carbonate minerals, waste heat recovery system and implementation method | |
| CN110369123A (en) | A kind of deironing apparatus and technique of refractory material fine powder | |
| CN112174159A (en) | Process for calcining kaolinite coal gangue | |
| US2701761A (en) | Integrated cyclic process for producing metallic iron from iron oxide-containing material | |
| CN215524211U (en) | Steel mill sintering flue gas waste heat utilization equipment and comprehensive utilization device | |
| GB959385A (en) | Process and apparatus for the production of magnesium chloride | |
| JPS60125337A (en) | Dechlorination and oxidation of zinc secondary starting material |