JPH0318497Y2 - - Google Patents
Info
- Publication number
- JPH0318497Y2 JPH0318497Y2 JP19218985U JP19218985U JPH0318497Y2 JP H0318497 Y2 JPH0318497 Y2 JP H0318497Y2 JP 19218985 U JP19218985 U JP 19218985U JP 19218985 U JP19218985 U JP 19218985U JP H0318497 Y2 JPH0318497 Y2 JP H0318497Y2
- Authority
- JP
- Japan
- Prior art keywords
- core tube
- arsenic
- furnace core
- ascl
- liquid
- 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.)
- Expired
Links
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 229910052785 arsenic Inorganic materials 0.000 claims description 9
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 9
- OEYOHULQRFXULB-UHFFFAOYSA-N arsenic trichloride Chemical compound Cl[As](Cl)Cl OEYOHULQRFXULB-UHFFFAOYSA-N 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- LULLIKNODDLMDQ-UHFFFAOYSA-N arsenic(3+) Chemical compound [As+3] LULLIKNODDLMDQ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Description
【考案の詳細な説明】
〔産業上の利用分野〕
本考案は精製塩化砒素を還元して高純度砒素を
得る装置の改善に関し、不純物の除去を可能とし
たものである。[Detailed Description of the Invention] [Industrial Field of Application] The present invention relates to an improvement in an apparatus for reducing purified arsenic chloride to obtain high-purity arsenic, and makes it possible to remove impurities.
従来、還元炉を用いて精製AsCl3を還元ガスと
しての水素と反応させて金属砒素を析出させるた
めに、還元炉炉芯管入口部に液状のAsCl3を滴下
させ、電気炉等で加熱された炉芯管の予熱により
AsCl3を気化させ、これを水素気流により高温加
熱部で還元し、生成した砒素蒸気をさらに下流の
温度をやゝ下げた析出部で析出させていた。然る
に従来の装置では、一般的には液状AsCl3を炉芯
管内に直接滴下して気化させていたため、炉芯管
の接合部分から液状物が洩れることがあつてきわ
めて危険であり、また気化の速度も必ずしも一定
とはならなかつた。
Conventionally, in order to precipitate metallic arsenic by reacting purified AsCl 3 with hydrogen as a reducing gas using a reduction furnace, liquid AsCl 3 was dropped into the inlet of the reduction furnace core pipe and heated in an electric furnace, etc. By preheating the furnace core tube
AsCl 3 was vaporized and reduced by a hydrogen stream in a high-temperature heating section, and the arsenic vapor produced was precipitated further downstream in a precipitation section whose temperature was slightly lowered. However, in conventional equipment, liquid AsCl 3 is generally vaporized by dropping it directly into the furnace core tube, which is extremely dangerous as the liquid may leak from the joints of the furnace core tube. The speed was not necessarily constant either.
本考案は上記した問題点を解決し、炉芯管の接
合部からの漏洩がなく、AsCl3の気化速度が一定
となり、且つAsCl3中に混在するMgやCaなどの
不純物の除去にも効果のある高純度砒素の還元装
置を提供することにある。
This invention solves the above problems, eliminates leakage from the joints of the furnace core tube, keeps the vaporization rate of AsCl 3 constant, and is effective in removing impurities such as Mg and Ca mixed in AsCl 3 . An object of the present invention is to provide a high-purity arsenic reduction device.
本考案はこの目的を達成するために液状の精製
塩化砒素を炉芯管入口部より滴下し、還元ガスに
て金属砒素を還元析出する装置において、炉芯管
内の塩化砒素滴下部直下から炉芯管の加熱部に跨
がつて液状物保持用受け皿を設け、滴下した液状
塩化砒素を受け皿に受け、こゝから塩化砒素を逐
次気化させるようにしたものである。
In order to achieve this objective, the present invention uses a device in which purified arsenic chloride in liquid form is dropped from the inlet of the furnace core tube, and metal arsenic is reduced and precipitated using reducing gas. A tray for holding a liquid substance is provided across the heating section of the tube, and the dropped liquid arsenic chloride is received in the tray, and the arsenic chloride is successively vaporized from there.
本考案では炉芯管入口部から滴下したAsCl3液
を、一旦滴下部直下から炉芯管加熱部に跨がつて
設けられた受け皿に溜め、加熱部のヒーターによ
り溜つたAsCl3があたためられて、逐次揮発して
送入された水素ガスによつて還元されるので、
AsCl3液が直接反応管内に落ちることがなく
AsCl3の揮発速度も一定となる。還元された砒素
は低温加熱部で大部分が凝縮析出する。
In the present invention, the AsCl 3 liquid dripped from the inlet of the furnace core tube is stored in a saucer installed directly below the dripping section and across the furnace core tube heating section, and the AsCl 3 that has accumulated is heated by the heater in the heating section. , as it is successively evaporated and reduced by the injected hydrogen gas,
The AsCl 3 solution does not fall directly into the reaction tube.
The volatilization rate of AsCl 3 also remains constant. Most of the reduced arsenic is condensed and precipitated in the low-temperature heating section.
本考案の一実施例を第１図に従つて説明する。
１は横断面円形で直管状の透明石英製炉芯管で、
この炉芯管は電気炉の高温加熱部２及び低温加熱
部３が、その中間に冷却部４を挾んで設けられた
中を貫通して設置されている。５は炉芯管のキヤ
ツプ部で、還元ガス導入管６及びAsCl3滴下管７
が取付けられている。８は炉芯管１の一端がラツ
パ状に拡がつた部分で、この部分にキヤツプ部５
の開放端がすり合せで接合されている。９は液状
物保持用受け皿で、キヤツプ部の塩化砒素の滴下
管７の直下から、炉芯管１の高温加熱部２の部分
に跨つた長さになつていて、その横断面の形状は
炉芯管の下半分とほヾ同形で、管内での安定性が
良くなつていることが好ましい。
An embodiment of the present invention will be described with reference to FIG.
1 is a straight transparent quartz furnace core tube with a circular cross section.
This furnace core tube is installed so as to pass through the high-temperature heating section 2 and low-temperature heating section 3 of the electric furnace, with a cooling section 4 sandwiched therebetween. 5 is the cap part of the furnace core tube, which includes a reducing gas introduction tube 6 and an AsCl 3 dripping tube 7.
is installed. Reference numeral 8 denotes a part where one end of the furnace core tube 1 expands into a flap shape, and a cap part 5 is attached to this part.
The open ends of are joined by grinding. Reference numeral 9 denotes a liquid holding tray, which has a length extending from just below the arsenic chloride dripping tube 7 in the cap section to the high temperature heating section 2 of the furnace core tube 1, and its cross-sectional shape is similar to that of the furnace. It is preferable that it has almost the same shape as the lower half of the core tube to improve stability within the tube.
以上詳細に説明したように、この考案によれば
滴下された液状AsCl3は直接反応用炉芯管に落下
することがないため、炉芯管とキヤツプ部との接
合部から液状物が浸出することがなく、また液状
AsCl3は一旦受け皿にたまつて高温加熱帯からの
熱で遂次揮発して行くので、受け皿には揮発しに
くい不純物が残留し、得られた蒸着金属砒素中の
不純物含有量はMg、Caはいずれも0.05ppm以下
となる効果があつた。
As explained in detail above, according to this invention, the dropped liquid AsCl 3 does not fall directly into the reactor core tube, so the liquid material oozes out from the joint between the furnace core tube and the cap part. It is also liquid without being
Once AsCl 3 accumulates in the saucer, it is successively volatilized by the heat from the high-temperature heating zone, so impurities that are difficult to volatilize remain in the saucer, and the impurity content in the obtained vapor-deposited metal arsenic is reduced to Mg, Ca. Both had the effect of reducing the concentration to 0.05 ppm or less.
第１図は本考案の還元装置の概要を示す断面図
である。
１……炉芯管、２……高温加熱部、３……低温
加熱部、４……冷却部、５……キヤツプ部、７…
…Ascl3滴下管、９……受け皿。
FIG. 1 is a sectional view showing an outline of the reduction device of the present invention. 1... Furnace core tube, 2... High temperature heating section, 3... Low temperature heating section, 4... Cooling section, 5... Cap section, 7...
...Ascl 3 dripping tube, 9... saucer.
Claims (1)
し、還元ガスにて金属砒素を還元析出させる高純
度砒素の還元装置において、炉芯管内の塩化砒素
滴下部直下から炉芯管加熱部に跨がつて液状物保
持用受け皿を設けたことを特徴とする高純度砒素
の還元装置。 In a high-purity arsenic reduction device in which liquid purified arsenic chloride is dripped from the inlet of a furnace core tube and metal arsenic is reduced and precipitated using reducing gas, a process is carried out from just below the arsenic chloride dripping section in the furnace core tube to the furnace core tube heating section. A high-purity arsenic reduction device characterized by being provided with a saucer for holding a liquid substance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19218985U JPH0318497Y2 (en) | 1985-12-16 | 1985-12-16 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19218985U JPH0318497Y2 (en) | 1985-12-16 | 1985-12-16 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62101858U JPS62101858U (en) | 1987-06-29 |
| JPH0318497Y2 true JPH0318497Y2 (en) | 1991-04-18 |
Family
ID=31147030
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19218985U Expired JPH0318497Y2 (en) | 1985-12-16 | 1985-12-16 |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0318497Y2 (en) |
-
1985
- 1985-12-16 JP JP19218985U patent/JPH0318497Y2/ja not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62101858U (en) | 1987-06-29 |
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