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JP2009228106A - Method for collecting metal arsenic - Google Patents

Method for collecting metal arsenic Download PDF

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JP2009228106A
JP2009228106A JP2008078289A JP2008078289A JP2009228106A JP 2009228106 A JP2009228106 A JP 2009228106A JP 2008078289 A JP2008078289 A JP 2008078289A JP 2008078289 A JP2008078289 A JP 2008078289A JP 2009228106 A JP2009228106 A JP 2009228106A
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activated carbon
arsenic
metal arsenic
arsine
temperature
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JP5547870B2 (en
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Takayuki Sato
貴之 佐藤
Kazunobu Shibuya
和信 渋谷
Kazuhiro Miyazawa
和浩 宮澤
Mitsuru Kiyotaki
充 清瀧
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Nippon Sanso Holdings Corp
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for collecting high-purity metal arsenic from an activated carbon which has been used for removing arsine, with a simple operation. <P>SOLUTION: The collecting method includes: placing the activated carbon which has been used for removing arsine, on a heating region A of a reaction pipe 1; passing an inert gas such as nitrogen into the reaction pipe 1 while operating a heater 4 for heating and thereby controlling the temperature in the heating region A at 600 to 800°C. Then, gaseous metal arsenic is released from the activated carbon and is solidified in a cooling region B. Thus, the metal arsenic is collected. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

この発明は、アルシン（ＡｓＨ３）を除害処理した活性炭から金属ヒ素を簡単な操作で回収する方法に関する。
なお、本発明での金属ヒ素とは、灰色ヒ素、黄色ヒ素、黒色ヒ素の３種の同素体（変態）を包含するものとする。 The present invention relates to a method for recovering metal arsenic from activated carbon from which arsine (AsH 3 ) has been detoxified by a simple operation.
The metal arsenic in the present invention includes three allotropes (transformations) of gray arsenic, yellow arsenic, and black arsenic.

半導体製造設備からはアルシンなどを含む排ガスが排出され、この排ガスは、活性炭などの除害剤によって除害処理されたのち、系外に排出されている。この除害処理によって、ヒ素などの有害な化合物が吸着した活性炭が副生する。
一方、ヒ素は希少金属であり、このヒ素化合物が吸着された活性炭を廃棄物として廃棄処分にするのではなく、このものからヒ素を回収する技術が求められている。 Exhaust gas containing arsine and the like is discharged from the semiconductor manufacturing facility, and this exhaust gas is exhausted out of the system after being detoxified by a detoxifying agent such as activated carbon. By this detoxification treatment, activated carbon adsorbed with harmful compounds such as arsenic is by-produced.
On the other hand, arsenic is a rare metal, and there is a need for a technique for recovering arsenic from the activated carbon on which the arsenic compound is adsorbed, instead of disposing it as waste.

また、近年地球環境保護の立場からヒ素系廃棄物を埋立処分することが困難になりつつあり、その対策が切望されている。有害物であるヒ素も有効利用な形で分離、回収すれば、ヒ素系廃棄物を大幅に減少させることができる。   In recent years, it has become difficult to dispose of arsenic wastes in landfills from the standpoint of protecting the global environment. Arsenic waste can be greatly reduced if arsenic, which is a harmful substance, is also separated and recovered in an effective manner.

従来、ヒ素含有廃棄物からヒ素を回収する方法として、特開平１０−５９７２２号公報には、ヒ化ガリウムスクラップなどのヒ素含有廃棄物を酸素雰囲気下で４００〜６００℃で加熱して、高純度のヒ素酸化物を回収する方法が開示されている。
また、特開２００１−３０２２４３号公報には、金属酸化物などからなる除害剤を用いてアルシンなどの金属水素化ガスを除害処理し、この除害剤を酸で溶解し、不溶成分からヒ素を硫化物として回収する方法が開示されている。 Conventionally, as a method for recovering arsenic from arsenic-containing waste, Japanese Patent Application Laid-Open No. 10-59722 discloses that arsenic-containing waste such as gallium arsenide scrap is heated at 400 to 600 ° C. in an oxygen atmosphere to obtain high purity. A method for recovering the arsenic oxide is disclosed.
Japanese Patent Laid-Open No. 2001-302243 discloses that a hydrogenation gas such as arsine is detoxified using a detoxifying agent composed of a metal oxide or the like, the detoxifying agent is dissolved with an acid, A method for recovering arsenic as a sulfide is disclosed.

しかしながら、これら先行発明では、回収されるヒ素が酸化物や硫化物であるため、金属ヒ素とするには、さらなる精錬工程が必要である。また、回収処理操作が複雑で回収コストが高くなる不都合もある。
さらに、アルシンを除害処理した活性炭からヒ素を回収する技術は知られていない。
特開平１０−５９７２２号公報 特開２００１−３０２２４３号公報 However, in these prior inventions, since the recovered arsenic is an oxide or a sulfide, a further refining process is required to obtain metal arsenic. In addition, there is a disadvantage that the collection processing operation is complicated and the collection cost becomes high.
Furthermore, a technique for recovering arsenic from activated carbon from which arsine has been removed is not known.
Japanese Patent Laid-Open No. 10-59722 JP 2001-302243 A

よって、この発明における課題は、アルシンを除害処理した活性炭から簡単な操作により高純度の金属ヒ素を回収する方法を得ることにある。   Accordingly, an object of the present invention is to obtain a method for recovering high-purity metal arsenic from activated carbon from which arsine has been removed by a simple operation.

かかる課題を解決するため、
請求項１にかかる発明は、アルシンを除害処理した活性炭を不活性ガス雰囲気下で加熱して、金属ヒ素を回収することを特徴とする金属ヒ素の回収方法である。 To solve this problem,
The invention according to claim 1 is a method for recovering metal arsenic, comprising recovering metal arsenic by heating activated carbon detoxified with arsine in an inert gas atmosphere.

請求項２にかかる発明は、加熱温度が６００〜８００℃であることを特徴とする請求項１記載の金属ヒ素の回収方法である。   The invention according to claim 2 is the metal arsenic recovery method according to claim 1, wherein the heating temperature is 600 to 800 ° C.

請求項３にかかる発明は、アルシンを除害処理した活性炭を水分含有不活性ガスと接触させて、水分の吸着熱により活性炭を自己発熱させて、金属ヒ素を回収することを特徴とする金属ヒ素の回収方法である。   The invention according to claim 3 is characterized in that activated carbon from which arsine has been removed is brought into contact with a moisture-containing inert gas, and activated carbon is self-heated by moisture adsorption heat to recover metallic arsenic. This is a recovery method.

請求項４にかかる発明は、活性炭の温度が６００〜８００℃であることを特徴とする請求項３記載の金属ヒ素の回収方法である。   The invention according to claim 4 is the metal arsenic recovery method according to claim 3, wherein the temperature of the activated carbon is 600 to 800 ° C.

本発明によれば、アルシンを除害処理した活性炭を単に不活性ガス雰囲気下で加熱するだけの簡単な操作により高純度の金属ヒ素を回収することができる。
また、水分含有不活性ガスと接触させることで、吸着熱により活性炭を自己発熱させるものでは、外部からの熱源が不要であり、エネルギーコストを削減することができる。 According to the present invention, high-purity metal arsenic can be recovered by a simple operation in which activated carbon from which arsine has been detoxified is simply heated in an inert gas atmosphere.
In addition, when the activated carbon is self-heated by heat of adsorption by being brought into contact with a moisture-containing inert gas, an external heat source is unnecessary, and energy costs can be reduced.

図１は、この発明の回収方法の第１の例を実施するために好適に用いられる装置を示すものである。
図１中符号１は、反応管を示す。この反応管１は、シリカ、アルミナ、ステンレス鋼などの耐熱材料からなるもので、その長手方向が水平に配置されている。この反応管１の一方の開口端は窒素などの不活性ガスの導入口２となっており、他方の開口端は反応後の生成ガスの導出口３となっている。 FIG. 1 shows an apparatus suitably used for carrying out a first example of the recovery method of the present invention.
Reference numeral 1 in FIG. 1 indicates a reaction tube. The reaction tube 1 is made of a heat-resistant material such as silica, alumina, stainless steel, and the longitudinal direction thereof is horizontally arranged. One open end of the reaction tube 1 is an inlet 2 for an inert gas such as nitrogen, and the other open end is an outlet 3 for a product gas after reaction.

反応管１の導入口２側の約半分の部分には加熱用ヒータ４が巻回されて取り付けられて、加熱領域Ａとなっている。この加熱用ヒータ４はガラスウールなどの耐熱性に富む断熱材５に取り囲まれている。
この反応管１の加熱領域Ａの温度を測定するための温度センサ６が加熱領域Ａのほぼ中間の管壁に取り付けられている。
さらに、反応管１の導出口３側の約半分の部分は、その管外壁が露出しており、外気により冷却される冷却領域Ｂとなっている。 A heating heater 4 is wound around and attached to about half of the reaction tube 1 on the inlet 2 side to form a heating region A. The heater 4 is surrounded by a heat insulating material 5 having a high heat resistance such as glass wool.
A temperature sensor 6 for measuring the temperature of the heating region A of the reaction tube 1 is attached to a substantially intermediate tube wall of the heating region A.
Further, about a half of the reaction tube 1 on the outlet 3 side is an outer wall of the tube, which is a cooling region B that is cooled by outside air.

ついで、この装置を用いて金属ヒ素を回収する方法を説明する。
まず、アルシンを除害処理した活性炭を反応管１の加熱領域Ａに置く。
ここでの活性炭としては、アルシンを除害処理したものであればどのようなタイプのものでもよく、特に限定されない。 Next, a method for recovering metal arsenic using this apparatus will be described.
First, activated carbon from which arsine is removed is placed in the heating region A of the reaction tube 1.
The activated carbon here may be of any type as long as it has been subjected to an arsine detoxification treatment, and is not particularly limited.

また、アルシンを除害処理した活性炭としては、例えば半導体製造設備から排出されるアルシンを含む排ガスを活性炭が充填された吸着塔に導入し、この活性炭でアルシンを除害する処理工程において生成するものが主に用いられるが、これに限定されるものでもない。
なお、活性炭で除害処理されたアルシンは活性炭の触媒作用により亜ヒ酸（三酸化二ヒ素）に変化し、この化学種の状態で活性炭に化学吸着されていると考えられる。 In addition, the activated carbon from which arsine has been detoxified is produced, for example, by introducing exhaust gas containing arsine discharged from a semiconductor manufacturing facility into an adsorption tower filled with activated carbon, and in the process of detoxifying arsine with this activated carbon. Is mainly used, but is not limited thereto.
In addition, it is considered that arsine treated with activated carbon is converted to arsenous acid (arsenic trioxide) by the catalytic action of activated carbon and chemisorbed on activated carbon in this chemical species state.

ついで、反応管１の導入口２から窒素、アルゴンなどの不活性ガスを流して内部を不活性ガス雰囲気とし、加熱用ヒータ４を作動して加熱領域Ａの温度を６００〜８００℃、好ましくは６００〜７００℃とする。
この加熱により、活性炭に化学吸着している亜ヒ酸が脱着し、還元して金属ヒ素に変化する。 Next, an inert gas such as nitrogen or argon is flowed from the inlet 2 of the reaction tube 1 to make the inside an inert gas atmosphere, and the heater 4 is operated to set the temperature of the heating region A to 600 to 800 ° C., preferably Set to 600 to 700 ° C.
By this heating, arsenous acid chemically adsorbed on the activated carbon is desorbed and reduced to metal arsenic.

生成した金属ヒ素は、加熱領域Ａの温度が昇華温度よりも高くなっているのガス状となって不活性ガスに同伴されて冷却領域Ｂに流れ、ここで冷却されて固体の金属ヒ素となって、反応管１の内壁面に凝固する。
冷却領域Ｂの長さが十分であれば、生成した金属ヒ素のほとんどがその内壁面に凝固し、導出口３から洩れることはほとんどない。
このようにして回収された金属ヒ素は、黒色を呈し、純度９９．９％以上であり、そのまま工業原料として再利用できる品質である。 The produced metal arsenic becomes a gaseous state in which the temperature of the heating region A is higher than the sublimation temperature, is entrained by the inert gas, flows into the cooling region B, and is cooled here to become solid metal arsenic. Then, it solidifies on the inner wall surface of the reaction tube 1.
If the length of the cooling region B is sufficient, most of the generated metal arsenic solidifies on the inner wall surface and hardly leaks from the outlet 3.
The metal arsenic recovered in this way has a black color and a purity of 99.9% or more, which is a quality that can be reused as an industrial raw material.

前記加熱領域Ａの温度が６００℃未満であると、亜ヒ酸の還元が十分に進行せず、冷却領域Ｂに白色の亜ヒ酸と黒色の金属ヒ素とが混合して析出するため、金属ヒ素の回収には不適当である。また、温度が８００℃を越えると金属ヒ素のみを回収できるが、エネルギー効率が低下すること、反応管１を構成する材料の耐熱温度を考慮することなどの問題が生じる。   When the temperature of the heating region A is less than 600 ° C., the reduction of arsenous acid does not proceed sufficiently, and white arsenous acid and black metal arsenic are mixed and deposited in the cooling region B. Not suitable for arsenic recovery. Further, when the temperature exceeds 800 ° C., only metal arsenic can be recovered, but problems such as reduction in energy efficiency and consideration of the heat resistant temperature of the material constituting the reaction tube 1 arise.

図２は、この発明の回収方法の第２の例において、用いられる装置を示すものである。
図２中符号１１は、反応筒を示す。この反応筒１１は、ステンレス鋼などからなるもので、その上部開口部には蓋１２が設けられ、この蓋１２には、ガス導入口１３が形成されている。
反応筒１１の長手方向のほぼ中間には目皿１４が設けられ、下部開口部には、フィルター１５が設けられ、外気に連通されている。 FIG. 2 shows an apparatus used in the second example of the recovery method of the present invention.
Reference numeral 11 in FIG. 2 indicates a reaction cylinder. The reaction cylinder 11 is made of stainless steel or the like, and a lid 12 is provided at an upper opening portion of the reaction cylinder 11, and a gas inlet 13 is formed in the lid 12.
An eye plate 14 is provided in the middle of the reaction tube 11 in the longitudinal direction, and a filter 15 is provided in the lower opening to communicate with the outside air.

反応筒１１の目皿１４上には、活性炭が充填されて活性炭充填層１６となっている。目皿１３の下方は、空洞となって冷却領域Ｂとなっている。活性炭充填層１６には、活性炭の温度を測定するための温度センサ１７が挿入されている。
反応筒１１の活性炭充填層１６に相当する部分の外周部は、ガラスウールなどからなる断熱材１８で包囲されている。この断熱材１８は、必要に応じて取り付け、取り外し可能となっており、反応筒１１の使用形態に対応して取り付けられ、あるいは取り外した状態とされる。 On the eye plate 14 of the reaction cylinder 11, activated carbon is filled to form an activated carbon packed layer 16. Below the eye plate 13 is a cooling region B that is a cavity. A temperature sensor 17 for measuring the temperature of the activated carbon is inserted into the activated carbon packed bed 16.
The outer peripheral portion of the reaction cylinder 11 corresponding to the activated carbon packed layer 16 is surrounded by a heat insulating material 18 made of glass wool or the like. This heat insulating material 18 can be attached and detached as necessary, and is attached or removed in accordance with the usage form of the reaction tube 11.

次に、この装置を用いたヒ素の回収方法を説明する。
第１ステップでは、反応筒１１を排ガス中のアルシンを吸着、除去する除害筒として機能させる。
すなわち、反応筒１１から断熱材１８を取り外した状態とし、活性炭充填層１６が保温されないようにする。また、活性炭充填層１６の活性炭は、未吸着の状態とされている。
この状態の反応筒１１のガス導入口１３から半導体製造設備から排出されたアルシンを含む排ガスを反応筒１１内に導入する。 Next, an arsenic recovery method using this apparatus will be described.
In the first step, the reaction cylinder 11 is caused to function as an abatement cylinder that adsorbs and removes arsine in the exhaust gas.
That is, the heat insulating material 18 is removed from the reaction cylinder 11 so that the activated carbon packed bed 16 is not kept warm. Moreover, the activated carbon of the activated carbon packed bed 16 is in an unadsorbed state.
In this state, exhaust gas containing arsine discharged from the semiconductor manufacturing facility is introduced into the reaction tube 11 from the gas inlet 13 of the reaction tube 11.

排ガスは反応筒１１の活性炭充填層１６に流れ込み、排ガス中のアルシンが活性炭により除害される。活性炭充填層１６が破過する前に排ガスの導入を停止する。
この状態では、活性炭充填層１６の活性炭には、活性炭の触媒作用により亜ヒ酸に変化したアルシンが化学吸着されている。 The exhaust gas flows into the activated carbon packed bed 16 of the reaction cylinder 11, and the arsine in the exhaust gas is detoxified by the activated carbon. The introduction of exhaust gas is stopped before the activated carbon packed bed 16 breaks through.
In this state, the activated carbon of the activated carbon packed bed 16 is chemisorbed with arsine that has been converted to arsenous acid by the catalytic action of the activated carbon.

次に、第２ステップに移行する。第２ステップでは、反応筒１１に断熱材１８を取り付け、活性炭充填層１６を保温可能な状態とする。
ついで、反応筒１１のガス導入口１３から水分含有不活性ガスを反応筒１１内に導入する。
水分含有不活性ガスとは、窒素、アルゴンなどの不活性ガスに水分を水蒸気の状態で同伴させたもので、水分含有量としては、不活性ガスの温度での飽和水分量に近い量であることが、活性炭の吸着熱の発生量が大きくなって好ましい。 Next, the process proceeds to the second step. In the second step, the heat insulating material 18 is attached to the reaction cylinder 11 so that the activated carbon packed bed 16 can be kept warm.
Next, a water-containing inert gas is introduced into the reaction tube 11 from the gas inlet 13 of the reaction tube 11.
The moisture-containing inert gas is a gas in which moisture is entrained in an inert gas such as nitrogen or argon, and the moisture content is close to the saturated moisture content at the temperature of the inert gas. It is preferable because the amount of heat generated by adsorption of activated carbon increases.

水分含有不活性ガスの生成方法には、乾燥状態の窒素、アルゴンなどの不活性ガスを公知のバブリング装置に導入して、水分を含ませる方法などがある。   As a method for generating a moisture-containing inert gas, there is a method in which an inert gas such as nitrogen or argon in a dry state is introduced into a known bubbling apparatus to contain moisture.

通常、乾燥状態にある活性炭が水分を吸着すると吸着熱が発生し、活性炭が自己発熱する性質を有している。
このため、水分含有不活性ガスの導入により、活性炭充填層１６の活性炭は発熱し、活性炭充填層１６の外側には断熱材１８が存在するので、活性炭充填層１６の温度が上昇する。そして、活性炭充填層１６の温度が６００〜８００℃、好ましくは６００〜７００℃となるように温度センサ１７で温度を監視しつつ、水分含有不活性ガスの導入量を制御する。 Normally, when activated carbon in a dry state adsorbs moisture, heat of adsorption is generated, and the activated carbon has a property of self-heating.
For this reason, by the introduction of the moisture-containing inert gas, the activated carbon in the activated carbon packed layer 16 generates heat, and since the heat insulating material 18 exists outside the activated carbon packed layer 16, the temperature of the activated carbon packed layer 16 rises. The introduction amount of the moisture-containing inert gas is controlled while monitoring the temperature with the temperature sensor 17 so that the temperature of the activated carbon packed bed 16 is 600 to 800 ° C., preferably 600 to 700 ° C.

活性炭充填層１６の温度が６００〜８００℃になると、先の例と同様にガス状の金属ヒ素が生成し、これは不活性ガスの流れに同伴して活性炭充填層１６から目皿１４を通過して冷却領域Ｂに流れ込む。冷却領域Ｂに流れ込んだガス状の金属ヒ素は、ここで冷却され、冷却領域Ｂの内壁に凝固する。
以上によって、活性炭に吸着されていた亜ヒ酸を高純度の金属ヒ素として回収できる。 When the temperature of the activated carbon packed bed 16 reaches 600 to 800 ° C., gaseous metallic arsenic is generated as in the previous example, and this is accompanied by the flow of the inert gas and passes through the eye plate 14 from the activated carbon packed bed 16. And flows into the cooling region B. The gaseous metal arsenic flowing into the cooling zone B is cooled here and solidifies on the inner wall of the cooling zone B.
As described above, arsenous acid adsorbed on the activated carbon can be recovered as high-purity metal arsenic.

以下、具体例を示す。
（実施例１） −不活性ガス中に水分を添加せず加熱する場合−
アルシンを除害処理した活性炭０．５ｇを図１に示す反応管１の加熱領域Ａに装入し、窒素ガスを１Ｌ／ｍｉｎ流して窒素雰囲気を形成し、温度を４００℃、５００℃、６００℃、７００℃、８００Ｃに保ちつつ、それぞれ２時間加熱した。
その後、冷却領域Ｂに凝固したヒ素生成物を捕集し、これに含まれる金属ヒ素濃度を測定した。 Specific examples are shown below.
(Example 1) -When heating without adding moisture to an inert gas-
1 g of activated carbon detoxified with arsine is charged into the heating region A of the reaction tube 1 shown in FIG. 1, and a nitrogen atmosphere is formed by flowing nitrogen gas at a rate of 1 L / min. While maintaining at ℃, 700 ℃ and 800C, each was heated for 2 hours.
Thereafter, the solidified arsenic product was collected in the cooling region B, and the concentration of metal arsenic contained therein was measured.

図３は、ヒ素生成物中の金属ヒ素濃度と加熱温度との関係を示すグラフである。
加熱温度が４００℃では、冷却領域Ｂに凝固したヒ素生成物は白色であった。これは、４００℃では活性炭より脱着した亜ヒ酸が還元せず、そのまま冷却領域Ｂで凝固したためである。
５００℃では、冷却領域Ｂに凝固したヒ素生成物は灰白色と黒色の混合物であった。この温度付近では亜ヒ酸と金属ヒ素とが混合して析出することがわかる。
６００℃以上では、冷却領域Ｂで凝固したヒ素生成物は黒色で、金属ヒ素が生成しており、その濃度は９９．９％であった。 FIG. 3 is a graph showing the relationship between the metal arsenic concentration in the arsenic product and the heating temperature.
When the heating temperature was 400 ° C., the arsenic product solidified in the cooling region B was white. This is because arsenous acid desorbed from the activated carbon was not reduced at 400 ° C. and solidified in the cooling region B as it was.
At 500 ° C., the arsenic product solidified in the cooling zone B was a mixture of grayish white and black. It can be seen that near this temperature, arsenous acid and metal arsenic are mixed and precipitated.
Above 600 ° C., the arsenic product solidified in the cooling zone B was black and metal arsenic was produced, and its concentration was 99.9%.

（実施例２） −不活性ガス中に水分を添加して加熱しない場合−
図２に示す活性炭充填層１６を備えた反応筒１１にアルシンを含む排ガスを流し、アルシンを除害した。
その後、断熱材１８を設置して、バブリング装置にて水分を含有させた窒素ガス５Ｌ／ｍｉｎを流した。
反応筒１１に設置した温度センサ１７で活性炭充填層１６の温度が上昇するのが確認できた。 (Example 2) -When water is added to an inert gas and heating is not performed-
An exhaust gas containing arsine was passed through the reaction cylinder 11 provided with the activated carbon packed bed 16 shown in FIG. 2 to remove arsine.
Then, the heat insulating material 18 was installed, and nitrogen gas 5 L / min containing water was supplied by a bubbling device.
It was confirmed that the temperature of the activated carbon packed bed 16 increased by the temperature sensor 17 installed in the reaction cylinder 11.

活性炭充填層１６の温度が６００℃以上７００℃未満を維持するよう、水分含有窒素ガスを反応筒１１へ流入させたり流入させなかったりして３時間保った。
その後、窒素ガスのみを流して温度センサー１７で温度を監視しつつ、１００℃以下まで冷却した後、内部を開放したところ、冷却領域Ｂの壁面に黒色の生成物が凝固しているのを確認した。この生成物の金属ヒ素濃度を測定した結果、９９．９％であった。 In order to maintain the temperature of the activated carbon packed bed 16 at 600 ° C. or higher and lower than 700 ° C., the moisture-containing nitrogen gas was allowed to flow into the reaction tube 11 or not for 3 hours.
Then, after flowing only nitrogen gas and monitoring the temperature with the temperature sensor 17, cooling to 100 ° C. or less and then opening the interior, it is confirmed that the black product is solidified on the wall surface of the cooling region B did. As a result of measuring the metal arsenic concentration of this product, it was 99.9%.

本発明は、有効利用できるヒ素を回収することで環境への影響を考慮するとともに、経済的に有利な半導体製造工程に適用することができる。   The present invention can be applied to an economically advantageous semiconductor manufacturing process while taking into consideration the influence on the environment by collecting arsenic that can be used effectively.

本発明の回収方法に用いられる装置の一例を示す概略構成図である。It is a schematic block diagram which shows an example of the apparatus used for the collection | recovery method of this invention. 本発明の回収方法に用いられる装置の他の例を示す概略構成図である。It is a schematic block diagram which shows the other example of the apparatus used for the collection | recovery method of this invention. 実施例１での金属ヒ素濃度と加熱温度との関係を示すグラフである。4 is a graph showing the relationship between the metal arsenic concentration and the heating temperature in Example 1.

符号の説明Explanation of symbols

１・・・反応管、２・・・導入口、４・・・加熱用ヒータ、Ａ・・・加熱領域、Ｂ・・・冷却領域 DESCRIPTION OF SYMBOLS 1 ... Reaction tube, 2 ... Inlet, 4 ... Heating heater, A ... Heating area, B ... Cooling area

Claims (4)

アルシンを除害処理した活性炭を不活性ガス雰囲気下で加熱して、金属ヒ素を回収することを特徴とする金属ヒ素の回収方法。   A method for recovering metal arsenic, comprising recovering metal arsenic by heating activated carbon detoxified with arsine in an inert gas atmosphere. 加熱温度が６００〜８００℃であることを特徴とする請求項１記載の金属ヒ素の回収方法。   The method for recovering metal arsenic according to claim 1, wherein the heating temperature is 600 to 800 ° C. アルシンを除害処理した活性炭を水分含有不活性ガスと接触させて、水分の吸着熱により活性炭を自己発熱させて、金属ヒ素を回収することを特徴とする金属ヒ素の回収方法。   A method for recovering metal arsenic, comprising bringing activated carbon detoxified from arsine into contact with a moisture-containing inert gas and allowing the activated carbon to self-heat by moisture adsorption heat to recover metal arsenic. 活性炭の温度が６００〜８００℃であることを特徴とする請求項３記載の金属ヒ素の回収方法。   The method for recovering metal arsenic according to claim 3, wherein the temperature of the activated carbon is 600 to 800 ° C.
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CN119710294A (en) * 2025-03-01 2025-03-28 中南大学 Method and device for catalytic cracking of gaseous arsenides

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