JP2018123358A - Metal recovery method - Google Patents

Metal recovery method Download PDF

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JP2018123358A
JP2018123358A JP2017014705A JP2017014705A JP2018123358A JP 2018123358 A JP2018123358 A JP 2018123358A JP 2017014705 A JP2017014705 A JP 2017014705A JP 2017014705 A JP2017014705 A JP 2017014705A JP 2018123358 A JP2018123358 A JP 2018123358A
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metal
aqua regia
lead frame
recovery method
solution
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JP6754137B2 (en
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裕司 小森
Yuji Komori
裕司 小森
英二 井上
Eiji Inoue
英二 井上
井上　信宏
Nobuhiro Inoue
信宏 井上
政和 古西
Masakazu Konishi
政和 古西
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Astec Irie Co Ltd
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Astec Irie Co Ltd
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
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Abstract

PROBLEM TO BE SOLVED: To provide a metal recovery method which efficiently recovers metal of high purity from an integrated circuit package.SOLUTION: A metal recovery method which recovers metal from an integrated circuit package having a metal wire and a lead frame includes: a step of making the integrated circuit package carbonizes a resin component by heat treatment, and classifying the lead frame, and a residue containing the metal wire and a carbide; and a step of subjecting the classified residue containing the metal wire and the carbide to aqua regia treatment to obtain an aqua regia solution in which noble metal is dissolved in the aqua regia.SELECTED DRAWING: None

Description

本発明は、集積回路パッケージより金属を回収する、金属回収方法に関する。   The present invention relates to a metal recovery method for recovering metal from an integrated circuit package.

一般に自動車、家電製品、通信機器又はコンピュータ等には、内部に集積回路パッケージ等の電子部品を搭載したプリント基板が使用されており、その集積回路パッケージは集積回路にリードやボンディングワイヤ等の金属ワイヤ等が接続され、リードフレームにより支持固定されている。集積回路パッケージには、金、銀、銅、鉛、亜鉛、パラジウムその他の金属等、貴金属やレアメタル等の有価金属が含まれており、資源として利用価値がある。しかし電子機器や通信機器等に含まれる貴金属やレアメタルの含有量は僅かであり、回収することは容易でない。   Generally, a printed circuit board in which electronic components such as an integrated circuit package are mounted is used in automobiles, home appliances, communication devices, computers, and the like, and the integrated circuit package includes metal wires such as leads and bonding wires. Etc. are connected and supported and fixed by a lead frame. The integrated circuit package contains valuable metals such as gold, silver, copper, lead, zinc, palladium and other metals, such as noble metals and rare metals, and is useful as a resource. However, the contents of noble metals and rare metals contained in electronic devices and communication devices are very small and are not easy to recover.

例えば、特許文献１においては、貴金属粉末に水、塩酸および硝酸等からなる王水を加えた原料液を加熱溶解し、その後ろ過し、また発生する酸性ガスを中和処理することで安全無臭の貴金属溶液を回収する際の加熱方法が開示されている。   For example, in Patent Document 1, a raw material solution obtained by adding aqua regia composed of water, hydrochloric acid, nitric acid, etc. to noble metal powder is heated and dissolved, and then filtered, and the generated acidic gas is neutralized to neutralize safety. A heating method for recovering the noble metal solution is disclosed.

特許文献２においては、金および金以外の金属を含む試料から金を回収する方法において、前記資料を王水以外の酸混合物に溶解させ、不溶成分を採取し、不溶成分を王水に溶解させて還元処理し、金を析出させる方法が開示されている。   In Patent Document 2, in a method of recovering gold from a sample containing gold and a metal other than gold, the material is dissolved in an acid mixture other than aqua regia, insoluble components are collected, and insoluble components are dissolved in aqua regia. A method for reducing the amount of gold and precipitating gold is disclosed.

特開平６−１５８１９０号公報JP-A-6-158190 特開２０１３−１８１１８１号公報JP2013-181181A

特許文献１に開示された方法においては、貴金属粉末に多様な金属が含まれる場合、金以外の金属が急激に王水に溶解し、発煙・発泡が発生して危険であり作業性が悪い。また、特許文献２に記載された方法では、試料に含有される有機物と、酸混合物とが反応し、有毒なニトロベンゼンを発生したり、金属との反応により硫黄酸化物や窒素酸化物を発生させる虞がある。   In the method disclosed in Patent Document 1, when various metals are contained in the noble metal powder, metals other than gold are rapidly dissolved in aqua regia, and smoke and foaming occur, which is dangerous and workability is poor. In addition, in the method described in Patent Document 2, an organic substance contained in a sample and an acid mixture react to generate toxic nitrobenzene, or to generate sulfur oxide or nitrogen oxide by reaction with a metal. There is a fear.

本発明は、前述した事情に鑑みてなされたものであり、その目的は、集積回路パッケージより高純度の金属を効率良く回収する、金属回収方法を提供することにある。   The present invention has been made in view of the above-described circumstances, and an object of the present invention is to provide a metal recovery method that efficiently recovers high-purity metal from an integrated circuit package.

上記課題は下記手段により達成することができる。すなわち、本発明は下記の通りである。   The said subject can be achieved by the following means. That is, the present invention is as follows.

〔１〕
金属ワイヤとリードフレームを備えた集積回路パッケージより金属を回収する金属回収方法であって、
前記集積回路パッケージは、加熱処理して樹脂成分を炭化し、
前記リードフレームと、前記金属ワイヤ及び炭化物を含む残渣とに分別する工程と、
分別した金属ワイヤ及び炭化物を含む残渣を、王水処理し、貴金属が王水に溶解した王水溶解液を得る工程とを含む、
金属回収方法。
〔２〕
前記リードフレームと、前記金属ワイヤ及び炭化物を含む残渣との分別を、篩い、水力、風力、又は磁力により分別する、〔１〕に記載の金属回収方法。
〔３〕
更に、分別したリードフレームを、塩化第二鉄を含む処理溶液に浸漬して金属を溶解させ、得られた処理済液より金属を回収する工程を含む、
〔１〕又は〔２〕に記載の金属回収方法。
〔４〕
前記処理済液より金属を回収する工程は、処理済液をろ過によりろ液とろ物とに分ける工程と、該ろ液に鉄粉を添加することにより金属を回収する工程と、該ろ物を王水処理し、貴金属が王水に溶解した王水溶解液を得る工程とを含む、
〔３〕に記載の金属回収方法。 [1]
A metal recovery method for recovering metal from an integrated circuit package comprising a metal wire and a lead frame,
The integrated circuit package is heat-treated to carbonize the resin component,
Separating the lead frame and the residue including the metal wire and carbide;
Treating the residue containing the separated metal wires and carbides with aqua regia to obtain an aqua regia solution in which noble metals are dissolved in aqua regia,
Metal recovery method.
[2]
The metal recovery method according to [1], wherein the separation between the lead frame and the residue including the metal wire and carbide is performed by sieving, hydraulic power, wind power, or magnetic force.
[3]
Furthermore, the separated lead frame is immersed in a treatment solution containing ferric chloride to dissolve the metal, and includes a step of recovering the metal from the obtained treated liquid.
The metal recovery method according to [1] or [2].
[4]
The step of recovering the metal from the treated liquid includes a step of separating the treated liquid into a filtrate and a filtrate by filtration, a step of collecting metal by adding iron powder to the filtrate, and the filtrate. Aquifer treatment, and obtaining a aqua regia solution in which noble metals are dissolved in aqua regia,
[3] The metal recovery method according to [3].

本発明の金属回収方法によれば、集積回路パッケージを加熱処理により樹脂成分を炭化し、リードフレームと、金属ワイヤ及び炭化物を含む残渣とに分別してからその後の処理に供することにより、高純度の金属を回収することができる。   According to the metal recovery method of the present invention, the resin component is carbonized by heat treatment of the integrated circuit package, and is separated into a lead frame and a residue containing metal wires and carbides, and then subjected to subsequent processing, whereby high purity is obtained. Metal can be recovered.

以下、本発明の金属回収方法について説明する。
本発明の金属回収方法は、金属ワイヤとリードフレームを備えた集積回路パッケージより金属を回収する金属回収方法であって、前記集積回路パッケージは、加熱処理して樹脂成分を炭化し、前記リードフレームと、前記金属ワイヤ及び炭化物を含む残渣とに分別する工程と、分別した金属ワイヤ及び炭化物を含む残渣を、王水と混合して貴金属を溶解させ、ろ過により貴金属が王水に溶解した王水溶解液を得る工程とを含む、金属回収方法である。 Hereinafter, the metal recovery method of the present invention will be described.
The metal recovery method of the present invention is a metal recovery method for recovering metal from an integrated circuit package having a metal wire and a lead frame, wherein the integrated circuit package carbonizes a resin component by heat treatment, and the lead frame And the step of separating the metal wire and the residue containing carbide, the residue containing the separated metal wire and carbide is mixed with aqua regia to dissolve the noble metal, and the aqua regia in which the noble metal is dissolved in the aqua regia by filtration. And a step of obtaining a solution.

〔集積回路パッケージ〕
電子機器等に用いられるプリント基板には、集積回路にリードやボンディングワイヤ等の金属ワイヤ等が接続され、リードフレームにより支持固定された集積回路パッケージが搭載されている。
本発明における集積回路パッケージは、金属ワイヤとリードフレームを備えたものであれば特に制限はなく、材質や形状、サイズ等に関わらず様々な種類の集積回路パッケージであってもよい。リードフレームの材質としては、銅合金系素材、鉄合金系素材、その他の機械的強度、電気伝導度、熱伝導度、耐食性などの優れた金属素材、樹脂素材が用いられる。リードフレームの材質にかかわらず、本発明の金属回収方法に供することができる。 [Integrated circuit package]
A printed circuit board used for an electronic device or the like is mounted with an integrated circuit package in which metal wires such as leads and bonding wires are connected to the integrated circuit and supported and fixed by a lead frame.
The integrated circuit package according to the present invention is not particularly limited as long as it includes a metal wire and a lead frame, and may be various types of integrated circuit packages regardless of material, shape, size, and the like. As the material of the lead frame, a copper alloy material, an iron alloy material, other metal materials having excellent mechanical strength, electrical conductivity, thermal conductivity, corrosion resistance, and resin materials are used. Regardless of the material of the lead frame, the metal recovery method of the present invention can be used.

集積回路パッケージは、電子部品が取り付けられたプリント基板から加熱等により分離させたものであることが好ましい。
例えば、プリント基板を搬送手段にて搬送しながら加熱中若しくは加熱後に、搬送手段から落下させて前記プリント基板に対して衝撃を加え、プリント基板から前記電子部品を分離することが好ましい。加熱したプリント基板を落下させた落下衝撃によって、プリント基板から電子部品を瞬間的かつ容易に分離することができる。この結果、振動装置などの機械を必要とせずに、プリント基板から電子部品を分離できる。
分離した電子部品より、目視による手作業や、画像処理による自動選別等により集積回路パッケージを分別することができる。電子部品と、プリント基板に電子部品を取り付けていたはんだと、電子部品が分離されたプリント基板とが分離されており、破砕等を行っていないためそれぞれを判別し易く、容易に分別することができる。そして、分別の正確性を飛躍的に向上することにより、高純度の金属を効率良く回収できる。 The integrated circuit package is preferably separated from a printed circuit board on which electronic components are attached by heating or the like.
For example, it is preferable that the electronic component is separated from the printed circuit board by dropping it from the transport unit and applying an impact to the printed circuit board during or after heating while transporting the printed circuit board by the transport unit. The electronic component can be instantaneously and easily separated from the printed board by a drop impact caused by dropping the heated printed board. As a result, the electronic component can be separated from the printed circuit board without requiring a machine such as a vibration device.
From the separated electronic components, the integrated circuit package can be sorted by visual manual operation, automatic sorting by image processing, or the like. The electronic component, the solder that has attached the electronic component to the printed circuit board, and the printed circuit board from which the electronic component has been separated are separated and are not crushed. it can. And by improving the accuracy of sorting dramatically, it is possible to efficiently recover high-purity metals.

〔加熱処理〕
集積回路パッケージは、加熱処理して樹脂成分を炭化し、リードフレームと、金属ワイヤ及び炭化物を含む残渣とに分別する。
加熱処理した集積回路パッケージは、樹脂成分が充分に炭化するため、リードフレームと、金属ワイヤ及び加熱処理により炭化した樹脂（炭化物）を含む残渣とを容易に分別することができる。リードフレームが樹脂材料であった場合は、リードフレームも炭化するため金属材料のリードフレームを分別すればよい。 [Heat treatment]
The integrated circuit package is heat-treated to carbonize the resin component, and is separated into a lead frame and a residue containing metal wires and carbides.
Since the resin component is sufficiently carbonized in the heat-treated integrated circuit package, the lead frame and the residue containing the metal wire and the resin (carbide) carbonized by the heat treatment can be easily separated. When the lead frame is made of a resin material, the lead frame is also carbonized so that the metal lead frame may be separated.

集積回路パッケージは粗破砕してもよいが、粗破砕せずに加熱処理することで、工程が簡略化されるだけでなく、展延性に富む金の形状を変化させることなく分離出来るため金を高純度に回収することができる。   Integrated circuit packages may be roughly crushed, but heat treatment without rough crushing not only simplifies the process, but also allows separation without changing the shape of the gold, which is highly extensible. It can be recovered with high purity.

加熱処理における加熱の温度は、集積回路パッケージに含まれる樹脂材料が分解する温度である必要がある。具体的には５００℃〜９００℃が好ましく、５５０℃〜８００℃であることが更に好ましく、６１０℃〜７３０℃であることが特に好ましい。
加熱処理における加熱に供する時間は加熱の温度によって異なるが、１０分〜５時間が好ましく、１０分〜３時間であることが更に好ましい。加熱時間を上記の範囲にすることで、金属ワイヤをモールドしている樹脂成分を完全に分解させ、モールド樹脂より金属ワイヤーを分離することができ、金等の貴金属を効率良く高純度に回収することができる。 The heating temperature in the heat treatment needs to be a temperature at which the resin material included in the integrated circuit package is decomposed. Specifically, it is preferably 500 ° C to 900 ° C, more preferably 550 ° C to 800 ° C, and particularly preferably 610 ° C to 730 ° C.
Although the time for heating in the heat treatment varies depending on the heating temperature, it is preferably 10 minutes to 5 hours, and more preferably 10 minutes to 3 hours. By setting the heating time within the above range, the resin component molding the metal wire can be completely decomposed, and the metal wire can be separated from the mold resin, and the noble metal such as gold is efficiently recovered with high purity. be able to.

加熱方法は、加熱流体を集積回路パッケージに吹き付けるのでもよく、加熱流体の雰囲気炉内に滞留させるものでもよく、加熱効率、処理装置の建設コストを勘案して処理できるものである。
加熱流体は高温空気による加熱でもよいが、水蒸気加熱、特に過熱水蒸気は熱容量が大きく、熱効率が良いので過熱水蒸気による加熱が最も好ましい。該加熱により集積回路パッケージに含まれる樹脂を効率よく脆性化、分解して炭化するものである。
加熱流体の雰囲気が炉内に滞留する方が熱容量は大きく短時間で処理できる。加熱流体を吹き付ける方法は熱容量が小さく、処理時間が長くなるが装置が簡素化できるメリットはある。加熱温度、加熱方法、及び加熱時間については全体の処理コストを勘案して処理できる。 The heating method may be that the heating fluid is sprayed on the integrated circuit package or may be retained in the atmosphere furnace of the heating fluid, and can be processed in consideration of the heating efficiency and the construction cost of the processing apparatus.
The heating fluid may be heated by high-temperature air, but steam heating, particularly superheated steam, has a large heat capacity and good thermal efficiency, so heating by superheated steam is most preferable. By this heating, the resin contained in the integrated circuit package is efficiently embrittled, decomposed and carbonized.
If the atmosphere of the heating fluid stays in the furnace, the heat capacity is larger and the treatment can be performed in a shorter time. The method of spraying the heating fluid has a merit that the apparatus can be simplified although the heat capacity is small and the processing time becomes long. The heating temperature, heating method, and heating time can be processed in consideration of the entire processing cost.

該加熱流体の加熱はガス等燃料の燃焼での加熱、電熱ヒーター等による加熱、誘導加熱装置による加熱等が利用できる。樹脂が酸化しないように真空加熱炉を使用することも可能である。炉は横型でも、縦型でも可能である。   The heating fluid can be heated by combustion of fuel such as gas, heating by an electric heater, heating by an induction heating device, or the like. It is also possible to use a vacuum heating furnace so that the resin does not oxidize. The furnace can be horizontal or vertical.

加熱処理により炭化した樹脂（炭化物）は脆く壊れやすいので、殆どの炭化物は分離されるが、炭化物の一部は金属片から分離されずに表面に付着したまま残ることがある。金属片と炭化物の分離を促進するため、振動又は機械的外力を与えてもよい。振動と機械的外力を組み合わせて与えることもできる。機械的外力としては、ブラシ、ショットブラスト等による処理が挙げられる。
機械的な外力を与えることにより、炭化物は、リードフレームや金属ワイヤから剥離することができる。
リードフレームと、金属ワイヤ及び炭化物を含む残渣とを分別は、篩い、水力、風力、又は磁力による分別であることが好ましい。銅等を多く含有するリードフレームを金属ワイヤと分別してから溶解処理を行うことにより、高純度の金属を安全性高く得ることができる。 Since the resin (carbide) carbonized by the heat treatment is brittle and fragile, most of the carbide is separated, but a part of the carbide may remain attached to the surface without being separated from the metal piece. Vibration or mechanical external force may be applied to promote separation of the metal piece and carbide. A combination of vibration and mechanical external force can also be applied. Examples of the mechanical external force include treatment with a brush, shot blast, and the like.
By applying a mechanical external force, the carbide can be peeled off from the lead frame or the metal wire.
The separation of the lead frame and the residue including the metal wire and carbide is preferably performed by sieving, hydraulic power, wind power, or magnetic force. By separating the lead frame containing a large amount of copper and the like from the metal wire and then performing the melting treatment, a high-purity metal can be obtained with high safety.

更に、振動篩いによる分別処理として、タイラー（Ｔｙｌｅｒ）標準篩９メッシュ〜１５０メッシュの範囲のいずれかの篩い目を有する振動篩い機を用いることができる。これにより、リードフレームと、金属ワイヤ及び炭化物を含む残渣とを分別することができ、さらに金属ワイヤを効率よく分別し回収することができる。
なお、前記した９メッシュ、１５０メッシュのタイラー標準篩とは、それぞれ篩目の開き量が２ｍｍ、１０６μｍとなるような篩いである。
さらに、水力分別や風力分別等による比重選別、又は磁力分別によって、金属ワイヤを分別することができる。 Furthermore, a vibration sieving machine having any sieve mesh in the range of 9 mesh to 150 mesh of Tyler standard sieve can be used as the separation process by the vibration sieve. Thereby, a lead frame and the residue containing a metal wire and a carbide | carbonized_material can be fractionated, and also a metal wire can be fractionated and collect | recovered efficiently.
The 9-mesh and 150-mesh Tyler standard sieves mentioned above are sieves with openings of 2 mm and 106 μm, respectively.
Furthermore, the metal wires can be separated by specific gravity sorting by hydraulic separation, wind separation, or the like, or by magnetic separation.

〔金属の回収〕
分別した金属ワイヤ及び炭化物を含む残渣は、王水処理し、貴金属が王水に溶解した王水溶解液を得る。 [Metal recovery]
The separated metal wire and carbide-containing residue is subjected to aqua regia treatment to obtain an aqua regia solution in which noble metals are dissolved in aqua regia.

（王水処理）
金属ワイヤ及び炭化物を含む残渣を、王水処理し、貴金属が王水に溶解した王水溶解液を得る工程は、上記金属ワイヤ及び炭化物を含む残渣を、王水と混合して貴金属を溶解させ、ろ過により貴金属が王水に溶解した王水溶解液を得る工程であることが好ましい。金属ワイヤ及び炭化物を含む残渣を王水で処理することにより、金属ワイヤ及び炭化物を含む残渣のうち金属ワイヤが王水に溶解した王水溶解液と、炭化物の残渣との混合物である王水処理済液が得られる。この王水処理済液をろ過することにより、王水溶解液を得ることができる。ろ過は、真空ろ過により行うことが好ましい。
金属ワイヤには、金ワイヤと金以外の金属ワイヤが含まれ、リードフレームには銅が多く含まれる。リードフレームと金属ワイヤ及び炭化物を含む残渣とを分別して、金属ワイヤ及び炭化物を含む残渣のみを王水で処理することにより、王水と反応する金属の量を低減でき、突沸を防ぐことができる。また、金等の貴金属を高い濃度で含む王水溶解液とすることができる。該貴金属としては、金、パラジウム、ロジウム、白金、銀が挙げられる。 (Aqua regia treatment)
The step of treating the residue containing metal wire and carbide with aqua regia to obtain an aqua regia solution in which the noble metal is dissolved in aqua regia is performed by mixing the residue containing metal wire and carbide with aqua regia to dissolve the noble metal. The step is preferably a step of obtaining an aqua regia solution in which a noble metal is dissolved in aqua regia by filtration. The aqua regia treatment which is a mixture of the aqua regia solution in which the metal wire is dissolved in the aqua regia among the residues containing the metal wire and the carbide and the carbide residue by treating the residue containing the metal wire and the carbide with aqua regia. A finished solution is obtained. An aqua regia solution can be obtained by filtering the aqua regia treated solution. Filtration is preferably performed by vacuum filtration.
The metal wire includes a gold wire and a metal wire other than gold, and the lead frame includes a large amount of copper. By separating the lead frame from metal wire and carbide-containing residues and treating only the metal wire and carbide-containing residues with aqua regia, the amount of metal that reacts with aqua regia can be reduced and bumping can be prevented. . Moreover, it can be set as the aqua regia solution which contains noble metals, such as gold | metal | money, with high concentration. Examples of the noble metal include gold, palladium, rhodium, platinum, and silver.

王水は、塩酸と硝酸の混合溶液であれば特に制限されるものではない。通常用いられる濃塩酸と濃硝酸の体積混合比が３：１の王水を使用してもよいし、濃塩酸と濃硝酸の体積混合比が１〜１．５：２．５〜３．０の逆王水を使用することもできる。   The aqua regia is not particularly limited as long as it is a mixed solution of hydrochloric acid and nitric acid. Aqua regia having a volume mixing ratio of concentrated hydrochloric acid and concentrated nitric acid of 3: 1 that is usually used may be used, or a volume mixing ratio of concentrated hydrochloric acid and concentrated nitric acid is 1 to 1.5: 2.5 to 3.0. The reverse aqua regia can also be used.

王水による処理は、金属ワイヤ及び炭化物を含む残渣を王水に浸漬することにより行うことが好ましい。王水の温度は特に制限されるものではないが、例えば１０℃〜８０℃が好ましく、２０℃〜４０℃がより好ましい。浸漬時間は特に制限されるものではないが、例えば１〜１００時間が好ましく、５〜５０時間がより好ましく、１０〜２４時間が更に好ましい。   The treatment with aqua regia is preferably performed by immersing a residue containing metal wires and carbides in aqua regia. The temperature of the aqua regia is not particularly limited, but is preferably 10 ° C to 80 ° C, and more preferably 20 ° C to 40 ° C, for example. Although immersion time is not specifically limited, For example, 1 to 100 hours are preferable, 5 to 50 hours are more preferable, and 10 to 24 hours are still more preferable.

以上の方法により、集積回路パッケージに含まれる貴金属を回収することができる。   By the above method, the noble metal contained in the integrated circuit package can be recovered.

（溶解処理）
本発明の金属回収方法は、更に、分別したリードフレームを、塩化第二鉄を含む処理溶液に浸漬して金属を溶解させ、得られた処理済液より金属を回収する工程を含むことが好ましい。
処理済液より金属を回収する工程は、処理済液をろ過によりろ液とろ物とに分ける工程と、該ろ液に鉄粉を添加することにより金属を回収する工程と、該ろ物を王水と混合して貴金属を溶解させ、ろ過により貴金属が王水に溶解した王水溶解液を得る工程とを含むことが好ましい。
ろ過は、真空ろ過（到達圧力０．０〜６．６ｋＰａ）により行うことが好ましい。 (Dissolution treatment)
The metal recovery method of the present invention preferably further includes a step of immersing the sorted lead frame in a treatment solution containing ferric chloride to dissolve the metal and recovering the metal from the obtained treated solution. .
The process of recovering the metal from the treated liquid includes a process of separating the treated liquid into a filtrate and a filtrate by filtration, a process of recovering metal by adding iron powder to the filtrate, and the filtration of the filtrate. It is preferable to include a step of mixing with water to dissolve the noble metal and obtaining an aqua regia solution in which the noble metal is dissolved in aqua regia by filtration.
Filtration is preferably performed by vacuum filtration (attainment pressure: 0.0 to 6.6 kPa).

塩化第二鉄を含む処理溶液は、塩化第二鉄水溶液、又は塩酸が添加された塩化第二鉄水溶液であることが好ましい。
ここで、使用する塩化第二鉄水溶液中の塩化第二鉄（ＦｅＣｌ3）の濃度は、概ね１０質量％以上（望ましくは３０質量％以上）でよいが、経済性を考慮すれば、６０質量％以下（好ましくは５５質量％以下）である。
また、塩化第二鉄水溶液中に、更に塩酸（ＨＣｌ）を添加することも可能であるが、この場合、塩化水素３５質量％水溶液の塩酸と塩化第二鉄５０質量％水溶液を２０：８０〜５０：５０の体積比率で混合するのがよい。 The treatment solution containing ferric chloride is preferably a ferric chloride aqueous solution or a ferric chloride aqueous solution to which hydrochloric acid is added.
Here, the concentration of ferric chloride (FeCl 3 ) in the aqueous ferric chloride solution to be used may be approximately 10% by mass or more (preferably 30% by mass or more). % Or less (preferably 55% by mass or less).
Further, hydrochloric acid (HCl) can be further added to the aqueous ferric chloride solution. In this case, hydrochloric acid in a 35% by weight aqueous solution of hydrogen chloride and an aqueous solution of 50% by weight ferric chloride in 20:80 to Mixing at a volume ratio of 50:50 is preferred.

上記した塩化第二鉄水溶液と、塩酸が添加された塩化第二鉄水溶液には、新たに製造した新液と、新液を使用した後の処理済液（例えば、塩化銅や塩化ニッケルが溶存している液、更には塩化第一鉄が存在している液）、又は新液と処理済み液の混合液のいずれも使用できる。
これにより、リードフレーム中の各種金属は塩化物を形成し、塩化第二鉄水溶液に溶解する。 In the ferric chloride aqueous solution and the ferric chloride aqueous solution to which hydrochloric acid is added, the newly produced new solution and the treated solution after using the new solution (for example, copper chloride and nickel chloride are dissolved). Or a mixture of a fresh solution and a treated solution can be used.
As a result, various metals in the lead frame form chlorides and dissolve in the aqueous ferric chloride solution.

具体的には、銅は塩化銅（ＣｕＣｌ2）、ニッケルは塩化ニッケル（ＮｉＣｌ2）、クロムは塩化クロム（ＣｒＣｌ3）、錫は塩化錫（ＳｎＣｌ2）、鉛は塩化鉛（ＰｂＣｌ2）、ルテニウムは塩化ルテニウム（ＲｕＣｌ3）、アルミニウムは塩化アルミニウム（ＡｌＣｌ3）、インジウムは塩化インジウム（ＩｎＣｌ3）となる。 Specifically, copper is copper chloride (CuCl 2 ), nickel is nickel chloride (NiCl 2 ), chromium is chromium chloride (CrCl 3 ), tin is tin chloride (SnCl 2 ), lead is lead chloride (PbCl 2 ), Ruthenium is ruthenium chloride (RuCl 3 ), aluminum is aluminum chloride (AlCl 3 ), and indium is indium chloride (InCl 3 ).

リードフレームを構成する金属が溶解した溶解液から、金属を析出させて回収する。この方法としては、従来公知の方法を使用でき、例えば、金属成分が、銅とニッケルを含んでいる場合には、特開平６−１２７９４６号公報に記載の方法を使用できる。また、錫や銀、インジウム等も、同様の方法を使用できる。なお、クロムとアルミニウムは、水酸化物として回収される。
この具体的な方法は、特許第４０１８８３２号公報に記載されているため、以下簡単に説明する。 The metal is deposited and recovered from the solution in which the metal constituting the lead frame is dissolved. As this method, a conventionally known method can be used. For example, when the metal component contains copper and nickel, the method described in JP-A-6-127946 can be used. The same method can be used for tin, silver, indium, and the like. Note that chromium and aluminum are recovered as hydroxides.
This specific method is described in Japanese Patent No. 4018832 and will be briefly described below.

上記した金属成分を含有する塩化第二鉄水溶液（処理済液又はろ液）中に鉄粉を添加し、塩化第二鉄水溶液中に溶存する塩化銅（塩化物）を置換させ、銅を析出させて分離回収する。なお、塩化第二鉄水溶液中に塩化第二鉄が残存している場合は、鉄粉を添加して先に塩化第一鉄に還元しておく方が、銅の回収効率が向上し、望ましい。
次に、銅が除去された脱銅水溶液中に鉄粉を添加し、かつ鉄イオン濃度を制御してニッケルを析出させ分離回収する。これにより、塩化第二鉄水溶液中から銅とニッケルを回収できる。
以上の方法により、集積回路パッケージより貴金属以外の金属成分も回収することで、これらを再利用できるので、資源の有効利用が図れる。 Add iron powder into ferric chloride aqueous solution (treated solution or filtrate) containing the above metal components, replace copper chloride (chloride) dissolved in ferric chloride aqueous solution, and deposit copper Separated and recovered. In addition, when ferric chloride remains in the ferric chloride aqueous solution, it is preferable to add iron powder and reduce it to ferrous chloride first because the copper recovery efficiency is improved. .
Next, iron powder is added to the copper removal aqueous solution from which copper has been removed, and the iron ion concentration is controlled to precipitate and separate and recover nickel. Thereby, copper and nickel can be recovered from the aqueous ferric chloride solution.
By recovering metal components other than noble metals from the integrated circuit package by the above method, these can be reused, so that resources can be effectively used.

本発明の金属回収方法は、金等の貴金属と、その他の金属をそれぞれ分離回収することができる。貴金属やその他の金属を種類ごとに回収できることから、有価金属を高純度に回収し、資源として再利用することが可能となる。   The metal recovery method of the present invention can separate and recover noble metals such as gold and other metals. Since noble metals and other metals can be recovered for each type, valuable metals can be recovered with high purity and reused as resources.

以下、本発明にかかる金属回収方法の作用、効果の確認のために行った実施例について説明する。   Examples performed for confirming the operation and effect of the metal recovery method according to the present invention will be described below.

〔実施例〕
（加熱処理１）
集積回路パッケージ１５ｋｇを７００℃の過熱水蒸気雰囲気の加熱炉に投入し、２時間加熱した。
加熱炉より回収したものを、篩目の開き量が１０６μｍの篩を備えた円筒篩にて篩処理を行い、篩上にリードフレームを含む金属片６．６ｋｇと、篩下に金属ワイヤ及び加熱により炭化した樹脂の炭化物とを含む残渣５．４ｋｇとを回収した。 〔Example〕
(Heat treatment 1)
15 kg of the integrated circuit package was put into a heating furnace in a superheated steam atmosphere at 700 ° C. and heated for 2 hours.
The material collected from the heating furnace is subjected to a sieving process using a cylindrical sieve equipped with a sieve having a sieve opening of 106 μm, and 6.6 kg of a metal piece including a lead frame on the sieve, and a metal wire and heating under the sieve. 5.4 kg of a residue containing the carbide of the resin carbonized by the above was recovered.

（溶解処理１）
加熱処理１で得られたリードフレームを含む金属片６．６ｋｇを籠に入れて、濃度が３９質量％、３０℃の塩化第二鉄水溶液６３Ｌが貯液された槽に１２時間浸漬し金属成分を塩化第二鉄水溶液に溶解させた。ろ過処理により処理済液と、濾物とに濾別した。特開平６−１２７９４６に記載の方法を用いて、処理済液より溶解金属である銅を回収した。回収した銅の純度は９０％以上であった。 (Dissolution treatment 1)
6.6 kg of the metal piece containing the lead frame obtained in the heat treatment 1 is put in a basket and immersed in a tank in which 63 L of ferric chloride aqueous solution having a concentration of 39% by mass and 30 ° C. is stored for 12 hours. Was dissolved in an aqueous ferric chloride solution. The filtrate was separated into a treated liquid and a filtrate by filtration. Using the method described in JP-A-6-127946, copper as a dissolved metal was recovered from the treated liquid. The purity of the recovered copper was 90% or more.

（王水処理１）
加熱処理１で得られた金属ワイヤ及び炭化物を含む残渣５．４ｋｇを、温度が２０℃の王水１６Ｌ中に浸漬させ、含有される金属成分を王水に溶解させた。なお、使用した王水は濃塩酸（塩化水素の３７．２質量％水溶液）と、濃硝酸（無水硝酸の７０質量％水溶液）とを体積比３：１で混合して得られた混合液であり、王水への浸漬時間は２４時間とした。
王水溶解液と、未溶解の炭化物とをろ過により濾別し、金３０ｇを王水溶解液中に回収した。 (Aqua regia treatment 1)
5.4 kg of the residue containing the metal wire and carbide obtained in the heat treatment 1 was immersed in 16 L of aqua regia having a temperature of 20 ° C., and the contained metal components were dissolved in aqua regia. The aqua regia used was a mixed solution obtained by mixing concentrated hydrochloric acid (37.2 mass% aqueous solution of hydrogen chloride) and concentrated nitric acid (70 mass% aqueous solution of nitric anhydride) at a volume ratio of 3: 1. Yes, the immersion time in aqua regia was 24 hours.
The aqua regia solution and undissolved carbide were separated by filtration, and 30 g of gold was recovered in the aqua regia solution.

（王水処理２）
溶解処理１で得られた濾物を、温度が２０℃の王水２０Ｌ中に浸漬させ、含有される金属成分を王水に溶解させた。なお、使用した王水は濃塩酸（塩化水素の３７．２質量％水溶液）と、濃硝酸（無水硝酸の７０質量％水溶液）とを体積比３：１で混合して得られた混合液であり、王水への浸漬時間は２４時間とした。
王水溶解液をろ過し、金４ｇを王水溶解液中に回収した。 (Aqua regia treatment 2)
The filtrate obtained in the dissolution treatment 1 was immersed in 20 L of aqua regia having a temperature of 20 ° C., and the contained metal components were dissolved in aqua regia. The aqua regia used was a mixed solution obtained by mixing concentrated hydrochloric acid (37.2 mass% aqueous solution of hydrogen chloride) and concentrated nitric acid (70 mass% aqueous solution of nitric anhydride) at a volume ratio of 3: 1. Yes, the immersion time in aqua regia was 24 hours.
The aqua regia solution was filtered, and 4 g of gold was recovered in the aqua regia solution.

以上のことから、本発明の金属回収方法により、処理コストや設備コストを過剰にかけることなく、集積回路パッケージから金等の有価金属を個別に高純度に回収して再利用でき、資源の有効利用が図れることを確認できた。   From the above, the metal recovery method of the present invention can recover valuable metals such as gold from an integrated circuit package with high purity and reuse them without excessive processing costs and equipment costs, and can effectively use resources. We were able to confirm that we could use it.

以上、本発明を、実施の形態を参照して説明してきたが、本発明は何ら上記した実施の形態に記載の構成に限定されるものではなく、特許請求の範囲に記載されている事項の範囲内で考えられるその他の実施の形態や変形例も含むものである。   As described above, the present invention has been described with reference to the embodiment. However, the present invention is not limited to the configuration described in the above embodiment, and the matters described in the scope of claims. Other embodiments and modifications conceivable within the scope are also included.

Claims (4)

金属ワイヤとリードフレームを備えた集積回路パッケージより金属を回収する金属回収方法であって、
前記集積回路パッケージは、加熱処理して樹脂成分を炭化し、
前記リードフレームと、前記金属ワイヤ及び炭化物を含む残渣とに分別する工程と、
分別した金属ワイヤ及び炭化物を含む残渣を、王水処理し、貴金属が王水に溶解した王水溶解液を得る工程とを含む、
金属回収方法。 A metal recovery method for recovering metal from an integrated circuit package comprising a metal wire and a lead frame,
The integrated circuit package is heat-treated to carbonize the resin component,
Separating the lead frame and the residue including the metal wire and carbide;
Treating the residue containing the separated metal wires and carbides with aqua regia to obtain an aqua regia solution in which noble metals are dissolved in aqua regia,
Metal recovery method. 前記リードフレームと、前記金属ワイヤ及び炭化物を含む残渣との分別を、篩い、水力、風力、又は磁力により分別する、請求項１に記載の金属回収方法。   The metal recovery method according to claim 1, wherein the separation of the lead frame and the residue including the metal wire and carbide is performed by sieving, hydraulic power, wind power, or magnetic force. 更に、分別したリードフレームを、塩化第二鉄を含む処理溶液に浸漬して金属を溶解させ、得られた処理済液より金属を回収する工程を含む、
請求項１又は２に記載の金属回収方法。 Furthermore, the separated lead frame is immersed in a treatment solution containing ferric chloride to dissolve the metal, and includes a step of recovering the metal from the obtained treated liquid.
The metal recovery method according to claim 1 or 2. 前記処理済液より金属を回収する工程は、処理済液をろ過によりろ液とろ物とに分ける工程と、該ろ液に鉄粉を添加することにより金属を回収する工程と、該ろ物を王水処理し、貴金属が王水に溶解した王水溶解液を得る工程とを含む、
請求項３に記載の金属回収方法。
The step of recovering the metal from the treated liquid includes a step of separating the treated liquid into a filtrate and a filtrate by filtration, a step of collecting metal by adding iron powder to the filtrate, and the filtrate. Aquifer treatment, and obtaining a aqua regia solution in which noble metals are dissolved in aqua regia,
The metal recovery method according to claim 3.
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JPS5637699A (en) * 1979-09-05 1981-04-11 Mitsui Mining & Smelting Co Device for separating and recovering solder for printed board
JPH0813051A (en) * 1994-06-30 1996-01-16 Hokkai Can Co Ltd Gold collecting method
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