JP2010001246A - Method of treating trialkyl indium and method of recovering indium sludge obtained by above treatment - Google Patents

Method of treating trialkyl indium and method of recovering indium sludge obtained by above treatment Download PDF

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JP2010001246A
JP2010001246A JP2008161463A JP2008161463A JP2010001246A JP 2010001246 A JP2010001246 A JP 2010001246A JP 2008161463 A JP2008161463 A JP 2008161463A JP 2008161463 A JP2008161463 A JP 2008161463A JP 2010001246 A JP2010001246 A JP 2010001246A
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indium
trialkylindium
sludge
treating
trimethylindium
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JP5376113B2 (en
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Koji Takebayashi
浩二 竹林
Hiroyuki Monobe
浩之 物部
Hirotaka Yakushigami
啓孝 藥師神
Susumu Yoshitomi
晋 吉冨
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Ube Corp
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Ube Industries Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an industrially applicable method safely and easily treating indium waste and recovering indium sludge. <P>SOLUTION: Provided is a post treatment method for a trialkyl indium which is characterized by dissolving or suspending a trialkyl indium in an organic solvent and subsequently bringing it into contact with a ketone compound. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、トリアルキルインジウムの処理方法及び当該処理によって得られたインジウム汚泥を回収する方法に関する。トリアルキルインジウムは、高純度品においては半導体成膜として有用な化合物であり、その製造過程において副生するインジウム汚泥を回収することは、資源の有効利用ともなり得る。   The present invention relates to a method for treating trialkylindium and a method for recovering indium sludge obtained by the treatment. Trialkylindium is a useful compound for semiconductor film formation in high-purity products, and recovery of indium sludge produced as a by-product in the manufacturing process can be an effective use of resources.

半導体成膜材料等として用途があるトリアルキルインジウムは有用な化合物であるが、空気中の空気や水分と爆発的に反応する化合物であることから、その製造や取り扱いについては十分な注意を払う必要がある。特に、高い性能を有する高純度トリアルキルインジウムは、その製造過程において生じるトリアルキルインジウムを含有する初留分や釜残（以下、インジウム廃棄物と称する）であったとしても、その処理方法（例えば、トリアルキルインジウムを酸化的分解して酸化インジウムとする、トリアルキルインジウムと水と接触させることにより水酸化インジウムとする等）には十分に注意が必要である。更に、副生するインジウム汚泥（酸化インジウムや水酸化インジウム等）を回収することで、環境上及び経済的なメリットがあると十分に考えられる。
従来、例えば、鉛とインジウムとを含有する溶液へ活性炭を添加し鉛を吸着させる工程と、当該溶液中へ、当該溶液中に残留する鉛を硫化するに足る量の硫化剤を添加し、当該残留する鉛を硫化物として除去する工程と、当該鉛の硫化物を除去した溶液からインジウムを採取する工程と、を有することを特徴とするインジウム含有溶液の処理方法が開示されていた（例えば、特許文献１参照）。
しかしながら、トリアルキルインジウム廃棄物の安全な処理方法及びインジウム汚泥の回収方法については、特段優れた技術はなく、現実的には廃棄業者が引き取って埋め立て処理をしているというのが現状である。
特開２００８−８８４９４号公報 Trialkylindium, which is used as a semiconductor film-forming material, is a useful compound, but since it reacts explosively with air and moisture in the air, careful attention must be paid to its production and handling. There is. In particular, even if the high-purity trialkylindium having high performance is an initial fraction or residual residue (hereinafter referred to as indium waste) containing trialkylindium produced in the production process, its treatment method (for example, Careful attention must be paid to oxidative decomposition of trialkylindium to form indium oxide, or indium hydroxide by contacting trialkylindium with water. Furthermore, it is considered that there is an environmental and economic advantage by collecting by-produced indium sludge (indium oxide, indium hydroxide, etc.).
Conventionally, for example, a step of adding activated carbon to a solution containing lead and indium to adsorb lead, and adding a sulphurizing agent in an amount sufficient to sulfidize lead remaining in the solution, There has been disclosed a method for treating an indium-containing solution characterized by having a step of removing residual lead as sulfide and a step of collecting indium from the solution from which the lead sulfide has been removed (for example, Patent Document 1).
However, there is no particularly excellent technique for the safe treatment method of trialkylindium waste and the recovery method of indium sludge, and the actual situation is that the waste disposal company actually takes the landfill treatment.
JP 2008-88494 A

本発明の課題は、即ち、安全且つ簡便な方法にて、インジウム廃棄物を処理し、インジウム汚泥を回収することが可能な工業的に採用できる方法を提供することにある。   An object of the present invention is to provide an industrially adoptable method capable of treating indium waste and recovering indium sludge by a safe and simple method.

本発明の課題は、トリアルキルインジウムを有機溶媒に溶解又は懸濁させた後、ケトン化合物と接触させることを特徴とする、トリアルキルインジウムの処理方法によって解決される。又、本発明は、当該処理溶液から有機溶媒を除去することによるインジウム汚泥の回収方法によっても解決される。   The object of the present invention is solved by a method for treating trialkylindium, wherein trialkylindium is dissolved or suspended in an organic solvent and then contacted with a ketone compound. The present invention is also solved by a method for recovering indium sludge by removing an organic solvent from the treatment solution.

本発明により、安全且つ簡便な方法にて、インジウム廃棄物を処理し、インジウム汚泥を回収することが可能な工業的に採用できる方法を提供することにある。   An object of the present invention is to provide an industrially adoptable method capable of treating indium waste and recovering indium sludge by a safe and simple method.

本発明において使用するトリアルキルインジウムとしては、例えば、トリメチルインジウム、トリエチルインジウム等が挙げられるが、これらの中に少量のハロゲン化物（例えば、ジアルキルハロゲノインジウムやトリハロゲノインジウム等）を含んでいても良い。   Examples of the trialkylindium used in the present invention include trimethylindium and triethylindium, and a small amount of a halide (for example, dialkylhalogenoindium and trihalogenoindium) may be included therein. .

本発明で使用するトリアルキルインジウムを溶解又は懸濁させることができる有機溶媒としては、好ましくはトリアルキルインジウムと反応しない溶媒、更に好ましくは、例えば、ペンタン、ヘキサン、ヘプタン、オクタン、シクロヘキサン、シクロヘプタン、シクロオクタン等の脂肪族炭化水素類；ベンゼン、トルエン、キシレン（各種異性体を含む）等の芳香族炭化水素類が使用される。なお、これらの有機溶媒は単独又は二種以上を混合して使用しても良い。   The organic solvent that can dissolve or suspend trialkylindium used in the present invention is preferably a solvent that does not react with trialkylindium, more preferably, for example, pentane, hexane, heptane, octane, cyclohexane, cycloheptane. Aliphatic hydrocarbons such as cyclooctane; aromatic hydrocarbons such as benzene, toluene and xylene (including various isomers). In addition, you may use these organic solvents individually or in mixture of 2 or more types.

前記有機溶媒の使用量は、トリアルキルインジウム１ｇに対して、好ましくは１．５〜２５ｍｌ、更に好ましくは２〜２０ｍｌ、特に好ましくは５〜１５ｍｌである。   The amount of the organic solvent used is preferably 1.5 to 25 ml, more preferably 2 to 20 ml, and particularly preferably 5 to 15 ml with respect to 1 g of trialkylindium.

本発明で使用するケトン化合物としては、例えば、アセトン、メチルエチルケトン、ジエチルケトン、ｔ−ブチルメチルケトン、シクロヘキサノン等が挙げられるが、好ましくはアセトン、メチルエチルケトン、更に好ましくはアセトンが使用される。なお、これらのケトン化合物は単独又は二種以上を混合して使用しても良い。   Examples of the ketone compound used in the present invention include acetone, methyl ethyl ketone, diethyl ketone, t-butyl methyl ketone, and cyclohexanone. Preferably, acetone, methyl ethyl ketone, and more preferably acetone is used. In addition, you may use these ketone compounds individually or in mixture of 2 or more types.

前記ケトン化合物の使用量は、トリアルキルインジウム１ｇに対して、好ましくは０．５〜１００ｍｌ、更に好ましくは０．８〜５０ｍｌ、特に好ましくは１〜１０ｍｌである。   The amount of the ketone compound used is preferably 0.5 to 100 ml, more preferably 0.8 to 50 ml, and particularly preferably 1 to 10 ml with respect to 1 g of trialkylindium.

有機溶媒中のトリアルキルインジウムとケトン化合物とを接触させることによって（必要ならば更に水と接触させる）トリメチルインジウムがインジウム汚泥に変換される。その際の温度は特に制限されず、通常は室温で行うが、反応熱により溶液の温度上昇が確認される場合もある。   Trimethylindium is converted to indium sludge by contacting the trialkylindium in an organic solvent with a ketone compound (and further contacting with water if necessary). The temperature at that time is not particularly limited, and it is usually performed at room temperature, but the temperature rise of the solution may be confirmed by reaction heat.

前記インジウム汚泥とは、酸化インジウム、水酸化インジウム又はそれらの混合物を示すが、水との接触が実質的にない場合には酸化インジウムが優先して生成し、水との接触がある場合には水酸化インジウムが優先して生成する。但し、完全な非水系で行うことや完全な無酸素系で行うことは困難であるので、酸化インジウムと水酸化インジウムの混合物となることはしばしばある。   The indium sludge indicates indium oxide, indium hydroxide or a mixture thereof, but in the case where there is substantially no contact with water, indium oxide is preferentially generated, and when there is contact with water. Indium hydroxide is preferentially produced. However, since it is difficult to perform completely non-aqueous or completely oxygen-free system, it often becomes a mixture of indium oxide and indium hydroxide.

なお、これらの後処理、回収等は、全て工場敷地内の安全な場所において行われ、人為的ミスが生じないルールやマニュアルも徹底していることにより、実施に際しては特段の問題はない。   These post-treatments, collections, etc. are all performed in a safe place on the factory premises, and there are no particular problems during implementation because of the thorough rules and manuals that do not cause human error.

次に、実施例を挙げて本発明を具体的に説明するが、本発明の範囲はこれらに限定されるものではない。   Next, the present invention will be specifically described with reference to examples, but the scope of the present invention is not limited thereto.

実施例１（トリメチルインジウムの後処理及びインジウム汚泥の回収）
トリメチルインジウムを主成分とする溶液を蒸留して高純度トリメチルインジウムを取得するに当たり、初留分７８ｇを初留受器に留出させた後、高純度トリメチルインジウムを含む主留分を留出させた。蒸留後、釜残としてトリメチルインジウムを含む溶液を８９ｇ得た。初留分及び釜残を併せたインジウム廃棄物１６７ｇを得た。これをキシレン１.１Ｌに溶解させた後、アセトン２００ｍｌをゆるやかに加えて、含有するトリメチルインジウムをインジウム汚泥とし、有機溶媒を除去してインジウム汚泥を得た（当該汚泥は主として酸化インジウムを含有する）。得られたインジウム汚泥は大気中に暴露しても特段変化しなかった。 Example 1 (Aftertreatment of trimethylindium and recovery of indium sludge)
In obtaining a high purity trimethylindium by distilling a solution containing trimethylindium as a main component, after distilling 78 g of the first fraction into the first fraction receiver, the main fraction containing the high purity trimethylindium is distilled. It was. After distillation, 89 g of a solution containing trimethylindium as a residue was obtained. 167 g of indium waste combined with the first fraction and the residue was obtained. After this was dissolved in 1.1 L of xylene, 200 ml of acetone was gently added to make trimethylindium contained therein as indium sludge, and the organic solvent was removed to obtain indium sludge (the sludge mainly contains indium oxide). ). The indium sludge obtained did not change particularly even when exposed to the atmosphere.

実施例２（トリメチルインジウムの後処理及びインジウム汚泥の回収）
トリメチルインジウムを主成分とする溶液を蒸留して高純度トリメチルインジウムを取得するに当たり、初留分６０ｇを初留受器に留出させた後、高純度トリメチルインジウムを含む主留を留出させた。蒸留後、釜残としてトリメチルインジウムを含む溶液を８０ｇ得た。初留分及び釜残を併せたインジウム廃棄物１４０ｇを得た。これをキシレン１Ｌに溶解させた後、アセトン２００ｍｌをゆるやかに加えて、そののち、水１５０ｍｌをゆるやかに加えて、含有するトリメチルインジウムをインジウム汚泥とし、有機溶媒を除去してインジウム汚泥を得た（当該汚泥は主として水酸化インジウムを含有する）。得られたインジウム汚泥は大気中に暴露しても特段変化しなかった。 Example 2 (Aftertreatment of trimethylindium and recovery of indium sludge)
In obtaining a high-purity trimethylindium by distilling a solution containing trimethylindium as a main component, 60 g of an initial fraction was distilled to an initial fraction receiver, and then a main fraction containing high-purity trimethylindium was distilled. . After distillation, 80 g of a solution containing trimethylindium as a residue was obtained. The indium waste 140g which combined the first fraction and the kettle residue was obtained. After dissolving this in 1 L of xylene, 200 ml of acetone was gently added, and then 150 ml of water was added gently to make the contained trimethylindium into indium sludge, and the organic solvent was removed to obtain indium sludge ( The sludge mainly contains indium hydroxide). The indium sludge obtained did not change particularly even when exposed to the atmosphere.

実施例３（トリメチルインジウムの後処理及びインジウム汚泥の回収）
トリメチルインジウムを主成分とする溶液を蒸留して高純度トリメチルインジウムを取得するに当たり、初留分７２ｇを初留受器に留出させた後、高純度トリメチルインジウムを含む主留を留出させた。蒸留後、釜残としてトリメチルインジウムを含む溶液を１０８ｇ得た。初留分及び釜残を併せたインジウム廃棄物１８０ｇを得た。これをヘキサン１Ｌに加え、アセトン２００ｍｌをゆるやかに加え溶解させた後、大気中に放置して空気と接触させ、含有するトリメチルインジウムをインジウム汚泥とし、有機溶媒を除去して酸化インジウムを得た（当該汚泥は主として水酸化インジウムを含有する）。得られたインジウム汚泥は大気中に暴露しても特段変化しなかった。 Example 3 (Aftertreatment of trimethylindium and recovery of indium sludge)
In obtaining a high-purity trimethylindium by distilling a solution containing trimethylindium as a main component, 72 g of an initial fraction was distilled to an initial fraction receiver, and then a main fraction containing high-purity trimethylindium was distilled. . After distillation, 108 g of a solution containing trimethylindium as a residue was obtained. The indium waste 180g which combined the first fraction and the kettle residue was obtained. This was added to 1 L of hexane, 200 ml of acetone was gently added and dissolved, and then left in the atmosphere to be brought into contact with air. The trimethylindium contained was used as indium sludge, and the organic solvent was removed to obtain indium oxide ( The sludge mainly contains indium hydroxide). The indium sludge obtained did not change particularly even when exposed to the atmosphere.

実施例４（トリメチルインジウムの後処理及びインジウム汚泥の回収）
トリメチルインジウムを主成分とする溶液を蒸留して高純度トリメチルインジウムを取得するに当たり、初留分４０ｇを初留受器に留出させた後、高純度トリメチルインジウムを含む主留を留出させた。蒸留後、釜残としてトリメチルインジウムを含む溶液を１１２ｇ得た。初留分及び釜残を併せたインジウム廃棄物１５２ｇを得た。これをヘキサン１Ｌに加え、アセトン２００ｍｌをゆるやかに加え溶解させた後、水１５０ｍｌをゆるやかに加えて、含有するトリメチルインジウムをインジウム汚泥とし、有機溶媒を除去してインジウム汚泥を得た（当該汚泥は主として水酸化インジウムを含有する）。得られたインジウム汚泥は大気中に暴露しても特段変化しなかった。 Example 4 (Aftertreatment of trimethylindium and recovery of indium sludge)
In obtaining a high-purity trimethylindium by distilling a solution containing trimethylindium as a main component, 40 g of an initial fraction was distilled to an initial fraction receiver, and then a main fraction containing high-purity trimethylindium was distilled. . After distillation, 112 g of a solution containing trimethylindium as a residue was obtained. The indium waste 152g which combined the first fraction and the kettle residue was obtained. This was added to 1 L of hexane, 200 ml of acetone was gently added and dissolved, and then 150 ml of water was slowly added to make trimethylindium contained as indium sludge, and the organic solvent was removed to obtain indium sludge (the sludge is Mainly contains indium hydroxide). The indium sludge obtained did not change particularly even when exposed to the atmosphere.

本発明により、安全且つ簡便な方法にて、インジウム廃棄物を処理し、インジウム汚泥を回収することが可能な工業的に採用できる方法を提供することにある。   An object of the present invention is to provide an industrially adoptable method capable of treating indium waste and recovering indium sludge by a safe and simple method.

Claims (6)

トリアルキルインジウムの後処理方法であって、トリアルキルインジウムを有機溶媒に溶解又は懸濁させた後、ケトン化合物と接触させることを特徴とする、トリアルキルインジウムの処理方法。   A method for post-treatment of trialkylindium, wherein trialkylindium is dissolved or suspended in an organic solvent and then contacted with a ketone compound. 請求項１記載の方法によって処理されて得られる溶液から有機溶媒を除去することによるインジウム汚泥を回収するトリアルキルインジウムの処理方法。   The processing method of the trialkyl indium which collect | recovers indium sludge by removing an organic solvent from the solution obtained by processing by the method of Claim 1. トリアルキルインジウムの後処理方法であって、トリアルキルインジウムを有機溶媒に溶解又は懸濁させた後、ケトン化合物と接触させた後、得られた溶液から有機溶媒を除去することによりインジウム汚泥を回収する請求項１記載のトリアルキルインジウムの処理方法。   A post-treatment method for trialkylindium, in which trialkylindium is dissolved or suspended in an organic solvent, contacted with a ketone compound, and then the indium sludge is recovered by removing the organic solvent from the resulting solution. The method for treating trialkylindium according to claim 1. インジウム汚泥が酸化インジウム、水酸化インジウム又はそれらの混合物である請求項２又は３にいずれか記載のトリアルキルインジウムの処理方法。   The method for treating trialkylindium according to claim 2 or 3, wherein the indium sludge is indium oxide, indium hydroxide, or a mixture thereof. 有機溶媒が炭化水素類である請求項１乃至３にいずれか記載のトリアルキルインジウムの処理方法。   The method for treating trialkylindium according to any one of claims 1 to 3, wherein the organic solvent is a hydrocarbon. ケトン化合物がジアルキルケトンである請求項１又は３いずれか記載のトリアルキルインジウムの処理方法。   The method for treating trialkylindium according to claim 1, wherein the ketone compound is a dialkyl ketone.
JP2008161463A 2008-06-20 2008-06-20 Method for treating trialkylindium and method for recovering indium sludge obtained by the treatment Expired - Fee Related JP5376113B2 (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01100178A (en) * 1987-10-12 1989-04-18 Nippon Mining Co Ltd Method for purifying trialkylindium

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01100178A (en) * 1987-10-12 1989-04-18 Nippon Mining Co Ltd Method for purifying trialkylindium

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* Cited by examiner, † Cited by third party
Title
JPN6013022226; 化学大辞典６ , 19631215, ５２１〜５２２頁, 共立出版株式会社 *

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