JPS6365031A - Method for refining se-as alloy scrap by vacuum distillation - Google Patents
Method for refining se-as alloy scrap by vacuum distillationInfo
- Publication number
- JPS6365031A JPS6365031A JP21118786A JP21118786A JPS6365031A JP S6365031 A JPS6365031 A JP S6365031A JP 21118786 A JP21118786 A JP 21118786A JP 21118786 A JP21118786 A JP 21118786A JP S6365031 A JPS6365031 A JP S6365031A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- vacuum
- vacuum distillation
- distillation
- purity
- 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
- 229910000967 As alloy Inorganic materials 0.000 title claims abstract description 26
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims description 14
- 238000007670 refining Methods 0.000 title 1
- 239000000463 material Substances 0.000 claims description 17
- 238000000746 purification Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000004821 distillation Methods 0.000 abstract description 10
- 230000008018 melting Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 9
- 238000012733 comparative method Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000013014 purified material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (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〕
この発明は、５ｅ−Ａｓ屑材を真空蒸留することによシ
精製し、高純度５ｅ−Ａｓ再生材として回収する方法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for purifying 5e-As scrap material by vacuum distillation and recovering it as high-purity 5e-As recycled material.
一般に、５ｅ−Ａｓ合金が、例えば乾式複写機の感光ド
ラム表面に蒸着される感光剤として用いられ、この感光
ドラム表面への感光剤の蒸着が、ドラムと５ｅ−Ａｓ合
金ショットを真空蒸着炉に装入し、前記５ｅ−Ａｓ合金
を加熱して蒸発させ、前記ドラム表面に蒸着させること
によシ行なわれ、この場合５ｅ−Ａｓ合金蒸気の残シの
多くが真空蒸着炉の内壁にも付着し、これが５ｅ−Ａｓ
合金屑材として回収され、さらに仁の８ｅ−Ａｓ合金滑
材が精製され、再生材として用いられることは良く知ら
れるところである。In general, 5e-As alloy is used as a photosensitive agent that is deposited on the surface of a photosensitive drum of a dry copying machine, for example. This is done by charging the 5e-As alloy, heating it to evaporate it, and depositing it on the drum surface. In this case, most of the residue of the 5e-As alloy vapor also adheres to the inner wall of the vacuum deposition furnace. And this is 5e-As
It is well known that the 8e-As alloy lubricant is recovered as alloy scrap material, further refined, and used as recycled material.
上記のように５ｅ−Ａｓ合金屑材は、例えば真空蒸着炉
の内壁から混入したと見られるＦｅを主体とする不純物
をかなシの割合で含有するので、これを再生材とし・て
用いるために精製処理されるが、この代表的精製方法と
して、例えば特開昭６１−１４１０７号公報および特開
昭６１−１４１１０８号公報に記載される方法が知られ
ている。As mentioned above, the 5e-As alloy scrap material contains a small proportion of impurities, mainly Fe, which are thought to have entered from the inner wall of the vacuum deposition furnace. A typical purification method is known, for example, as described in JP-A-61-14107 and JP-A-61-141108.
しかし、上記の従来精製方法は、いずれも酸化焙焼工程
や加圧抽出工程、濾過工程、還元工程、さらに精製工程
などの多くの工程を経て、高純度Ｓｅと高純度Ａｓを別
々に回収し、ついでこれらを溶解して合金とすることに
よって再生材とする方法であるため、歩留シが低く、か
つ長い処理時間を必要とするばかりでなく、排ガスや排
液の大規模な処理設備を必要とし、さらに多くの薬剤を
使用することなどから、コスト高となるのを避けること
ができないのが現状である。However, in all of the above conventional purification methods, high-purity Se and high-purity As are recovered separately through many steps such as an oxidation roasting process, a pressure extraction process, a filtration process, a reduction process, and a purification process. This method is then used to produce recycled materials by melting them into an alloy, which not only has a low yield and requires a long processing time, but also requires large-scale treatment equipment for exhaust gas and liquid. Currently, it is impossible to avoid high costs because more drugs are required and more drugs are used.
そこで、本発明者等は、上述のような観点から、簡単な
工程で、歩留りよく、かつコスト安く、Ｓθ−Ａｓ合金
屑材を再使用可能な純度にまで精製することのできる方
法を開発すべく研究を行なった結果、５ｅ−Ａｓ合金屑
材を、真空蒸留炉において、真空度、１０ 〜１０
ｔｔａｘＨｇ。Therefore, from the above-mentioned viewpoint, the present inventors developed a method that can purify Sθ-As alloy scrap material to a purity that can be reused with a simple process, high yield, and low cost. As a result of research, we found that 5e-As alloy scrap material was heated to a vacuum degree of 10 to 10 in a vacuum distillation furnace.
ttaxHg.
温度−５００〜７００℃、
の条件にて真空蒸留し、ついで凝縮すると、この結果得
られた５ｅ−Ａｓ合金精製材は、９９．９９％以上の高
純度を有し、このままの状態で再使用可能であるという
知見を得たのである。Vacuum distillation is performed at a temperature of -500 to 700°C, followed by condensation. The resulting purified 5e-As alloy material has a high purity of 99.99% or more and can be reused as is. We have learned that it is possible.
この発明は、上記知見にもとづいてなされたものであっ
て、真空蒸留条件を上記の通シに限定したのは、真空度
かｌｏａｎＨｇ未満でも、また蒸留温度が５００℃未満
でも、蒸留を効率よく行なうことができず、一方真空度
か１０ ａｍＨｇを越えても、蒸留温度が７００℃を
越えても精製材に不純物が混入するようになって、高純
度の５ｅ−Ａｓ合金材を得ることができないという理由
にもとづくものである。This invention has been made based on the above knowledge, and the reason why the vacuum distillation conditions are limited to the above-mentioned standard is that distillation can be carried out efficiently even if the degree of vacuum is less than 1000 degrees Hg or the distillation temperature is less than 500°C. On the other hand, even if the degree of vacuum exceeds 10 amHg or the distillation temperature exceeds 700°C, impurities will be mixed into the purified material, making it impossible to obtain a high-purity 5e-As alloy material. This is based on the reason that it is not possible.
つぎに、この発明の方法を実施例によシ具体的に説明す
る。Next, the method of the present invention will be specifically explained using examples.
第１図に概略縦断面図で示される真空蒸留炉を用い、こ
れの蒸留槽１（６はヒーターを示す）内に第１表に示さ
れる組成をもった５ｅ−Ａｓ合金屑材２を５に９装入し
、同じく第１表に示される真空蒸留条件にて蒸留し、蒸
発した５ｅ−Ａｓ合金蒸気をコンデンサ３（６′はヒー
ターを示す）にて凝縮し、蒸留槽１にコンデンサ３を介
して連結した回収槽４（６“はヒーターを示す）のるつ
ぼ５内に溶融状態で５ｅ−Ａｓ合金精製材７として回収
することによって本発明法１〜５および比較法１〜４を
それぞれ実施し、蒸留終了に至るまでの時間（蒸留時間
という）および歩留を測定し、さらに得られた５ｅ−Ａ
ｓ合金材の純度および組成を測定した。これらの測定結
果を第１表に示した。また、第１表には上記の従来法に
よって精製された５ｅ−Ａｓ合金材の純度および組成も
示した。A vacuum distillation furnace shown in a schematic vertical cross-sectional view in FIG. The 5e-As alloy vapor was distilled under the same vacuum distillation conditions shown in Table 1, and the evaporated 5e-As alloy vapor was condensed in the condenser 3 (6' indicates a heater). Methods 1 to 5 of the present invention and comparative methods 1 to 4 were collected in a molten state as a 5e-As alloy refined material 7 into a crucible 5 of a collection tank 4 (6" indicates a heater) connected via a The time taken to complete the distillation (referred to as distillation time) and the yield were measured, and the obtained 5e-A
The purity and composition of the s-alloy material were measured. The results of these measurements are shown in Table 1. Table 1 also shows the purity and composition of the 5e-As alloy material refined by the above-mentioned conventional method.
なお、比較法１〜４は、真空蒸留条件をこの発明の範囲
から外した条件で行なったものである。In Comparative Methods 1 to 4, the vacuum distillation conditions were outside the scope of the present invention.
第１表に示される結果から、本発明法１〜５においては
、従来法によって精製された５ｅ−Ａｓ合金材と同等の
９９．９９％以上の高純度を有するＳｅ −Ａｓ合金材
を９８％以上の高い歩留シで、かつきわめて短かい蒸留
時間（ちなみに従来法では、同程度の量で２４時間程度
の処理時間を要し、かつ歩留も低く、−次実収で８５％
程度）で回収することができるのに対して、比較法１〜
４に見られるように、真空蒸留条件がこの発明の範囲か
ら外れると、歩留りが低下したシ、相対的に長い蒸留時
間を要するようになったシ、さらに純度の低下をきたす
ようになることが明らかである。From the results shown in Table 1, in Methods 1 to 5 of the present invention, Se-As alloy material having a high purity of 99.99% or higher, which is equivalent to the 5e-As alloy material refined by the conventional method, is 98% This high yield and extremely short distillation time (by the way, the conventional method requires about 24 hours of processing time for the same amount and has a low yield, with an actual yield of 85%.
Comparative method 1~
As seen in 4, when the vacuum distillation conditions are outside the scope of the present invention, the yield may be reduced, the distillation time may be relatively long, and the purity may be reduced. it is obvious.
上述のように、この発明の方法によれば、Ｓｅ −Ａｓ
合金屑材から、９８％以上の高純度をもった５ｅ−Ａｓ
合金精製材を、特定な条件下で真空蒸留するという簡単
な工程で、歩留りよく、かつ短時間で製造することがで
き、このままの状態で、あるいは別途用意した高純度Ｓ
ｅあるいは高純度Ａｓを、溶融状態で加えて成分調製す
るだけで、再生材として用いることができ、著しいコス
ト低減がはかれるなど工業上有用な効果がもたらされる
のである。As mentioned above, according to the method of the present invention, Se-As
5e-As with high purity of over 98% from alloy scrap material
Through a simple process of vacuum distilling refined alloy materials under specific conditions, it can be produced with high yield and in a short time.
By simply adding e or high-purity As in a molten state and preparing the components, it can be used as a recycled material, resulting in industrially useful effects such as significant cost reduction.
第１図は真空蒸留炉を示す概略縦断面図である。
１・・・蒸留槽、 ２・・・Ｓ’ｅ−Ａｓ合金屑
材、３・・・コンデンサ、 ４・・・回収槽、５・
・・るつぼ、 ６．６’、 ６’・・・ヒーター
、７・・・５ｅ−Ａｓ合金精製材。FIG. 1 is a schematic vertical sectional view showing a vacuum distillation furnace. DESCRIPTION OF SYMBOLS 1... Distillation tank, 2... S'e-As alloy scrap material, 3... Capacitor, 4... Recovery tank, 5...
... Crucible, 6.6', 6'... Heater, 7...5e-As alloy refined material.
Claims (1)
１０＾−＾２〜１０＾−＾４ｍｍＨｇ、温度：５００〜
７００℃、 の条件で真空蒸留し、ついで凝縮することにより精製し
、高純度Ｓｅ−Ａｓ合金再生材として回収することを特
徴とするＳｅ−Ａｓ合金屑材の真空蒸留精製方法。[Claims] Se-As alloy scrap material is processed in a vacuum distillation furnace at a vacuum degree of:
10^-^2~10^-^4mmHg, temperature: 500~
1. A vacuum distillation purification method for Se-As alloy scrap material, which comprises vacuum distilling at 700° C., followed by condensation to purify the material and recovering it as a high-purity Se-As alloy recycled material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21118786A JPS6365031A (en) | 1986-09-08 | 1986-09-08 | Method for refining se-as alloy scrap by vacuum distillation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21118786A JPS6365031A (en) | 1986-09-08 | 1986-09-08 | Method for refining se-as alloy scrap by vacuum distillation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6365031A true JPS6365031A (en) | 1988-03-23 |
Family
ID=16601844
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21118786A Pending JPS6365031A (en) | 1986-09-08 | 1986-09-08 | Method for refining se-as alloy scrap by vacuum distillation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6365031A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105483384A (en) * | 2015-12-08 | 2016-04-13 | 昆明理工大学 | Method for recovering valuable metals from copper anode mud flotation tailings |
-
1986
- 1986-09-08 JP JP21118786A patent/JPS6365031A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105483384A (en) * | 2015-12-08 | 2016-04-13 | 昆明理工大学 | Method for recovering valuable metals from copper anode mud flotation tailings |
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