TW201816127A - Method to extract the indium, gallium and zinc from wastes - Google Patents

Method to extract the indium, gallium and zinc from wastes Download PDF

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TW201816127A
TW201816127A TW105134890A TW105134890A TW201816127A TW 201816127 A TW201816127 A TW 201816127A TW 105134890 A TW105134890 A TW 105134890A TW 105134890 A TW105134890 A TW 105134890A TW 201816127 A TW201816127 A TW 201816127A
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gallium
zinc
indium
acid
extracting
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TWI636139B (en
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陳偉聖
王裕齊
陳天佑
陳為忠
陳為荃
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國立成功大學
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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

The present invention relates to a method to extract the indium, gallium and zinc from wastes. The method mainly focus on the recycling of indium, gallium and zinc containing wastes and is considered to extract three metals in one process. The invention combines solvent extraction technology and chemical precipitation technique. By the high selectivity of solvent extraction, the separation rate of the metal ions are enhanced and the produce high purity product.

Description

由含銦、鎵和鋅之廢棄物中提取該等金屬之方法Method for extracting such metals from wastes containing indium, gallium and zinc

本發明係關於一種金屬資源回收之方法，尤指一種對於含銦、鎵和鋅之廢棄物中提取該等金屬之方法。The present invention relates to a method for recovering metal resources, and more particularly to a method for extracting such metals from wastes containing indium, gallium and zinc.

銦、鎵與鋅為蘊藏量相當少之金屬，而現代由於光電領域大量的採氧化鎵鋅(GZO, Gallium Zinc Oxide)和氧化銦鎵鋅(IGZO, Indium Gallium Zinc Oxide)等作為靶材，而使得前開之金屬消耗量增多，但由於靶材在濺鍍製程中僅有少數會形成沉積，而大多數之靶材在製程中可能耗損在設備的腔壁或是披覆板(shielding)、擋板(shutter)等邊際設備或空間而產生相當多之廢棄物，除了增加工業廢棄物之來源，亦耗費資源。Indium, gallium and zinc are relatively rare metals, and modern ones use a large number of gallium oxide (GZO, Gallium Zinc Oxide) and indium gallium zinc oxide (IGZO, Indium Gallium Zinc Oxide) as targets. The metal consumption of the front opening is increased, but only a few deposits are formed in the sputtering process, and most of the targets may be depleted in the process chamber wall or shield or shield. A considerable amount of waste is generated by marginal equipment or space such as a shutter, and it also consumes resources in addition to increasing the source of industrial waste.

雖然在各個工業領域中對於前述金屬(銦、鎵與鋅)有在個別產業製程或物質中個別回收而對於，例如但不限於台灣發明專利I402356「回收具有高含量鋅及硫酸鹽之殘餘物的方法」、I516449「含鎵、銦集塵灰資源回收之方法」、I487790「有價金屬回收的方法」及I398526「回收鎵的方法」等。Although in the various industrial fields, the aforementioned metals (indium, gallium and zinc) are separately recovered in individual industrial processes or substances, for example, but not limited to Taiwan invention patent I402356 "recovering residues with high content of zinc and sulfate" Method, I516449 "Method for recovering gallium and indium dust collection ash resources", I487790 "Method for recovering valuable metals" and I398526 "Method for recovering gallium".

但前揭技術並非針對同時含有銦、鎵與鋅之廢棄物(通常為前述靶材氧化鎵鋅(GZO, Gallium Zinc Oxide)和氧化銦鎵鋅(IGZO, Indium Gallium Zinc Oxide)。However, the prior art is not directed to wastes containing both indium, gallium and zinc (usually the aforementioned targets gallium zinc oxide (GZO, Gallium Zinc Oxide) and indium gallium zinc oxide (IGZO, Indium Gallium Zinc Oxide).

雖然也有研發者取得台灣專利I432609號「從銦-鋅氧化物廢料回收有價金屬之方法」，此方法主要係從使用過之銦-鋅氧化物(IZO)濺鍍靶或在製造時所產生之IZO端材等IZO廢料回收有價金屬之方法。該發明主要係自IZO廢料回收有價金屬，若予以電解之IZO廢料本身為高純度之材料所構成的廢料，則可直接維持其純度，並能以高純度之氫氧化銦與氫氧化鋅之混合物或氧化銦及氧化鋅之混合物的形態來進行回收。但仍然未見對於特定對於同時具有銦(In)、鎵(Ga)與鋅(Zn)三種金屬之廢棄物，以整合方式處理回收。且該I432609號專利，以電解法進行，過程較為繁瑣，且耗費資源較大。Although some developers have obtained Taiwan Patent No. I432609 "Method for recovering valuable metals from indium-zinc oxide waste", this method is mainly generated from the used indium-zinc oxide (IZO) sputtering target or at the time of manufacture. A method of recovering valuable metals from IZO scraps such as IZO end materials. The invention mainly recovers valuable metals from IZO scrap. If the IZO scrap which is electrolyzed is a waste material composed of high-purity materials, the purity can be directly maintained, and a mixture of high-purity indium hydroxide and zinc hydroxide can be used. It is recovered in the form of a mixture of indium oxide and zinc oxide. However, it has not been found that the waste is treated in an integrated manner for wastes having three metals of indium (In), gallium (Ga) and zinc (Zn). And the patent No. I432609 is carried out by an electrolysis method, which is cumbersome and consumes a large amount of resources.

此外，亦有許多研究，均著重在於ITO中之In的回收，ITO(Indium Tin Oxide；銦錫氧化物)是由90%的銦(Indium)加10%的錫(Tin)所組成，或是半導體GaAs中之Ga的回收，運用之回收程序雖然回收率高，但純度較低。且相同的方法對於含In,Ga,Zn之廢棄物中In,Ga的回收欠佳且分離效果差。In addition, there are many studies focusing on the recovery of In in ITO. Indium Tin Oxide (ITO) consists of 90% indium (Indium) plus 10% tin (Tin), or In the recovery of Ga in semiconductor GaAs, the recovery procedure used is high, but the purity is low. And the same method is poor in the recovery of In, Ga in the waste containing In, Ga, Zn and the separation effect is poor.

有鑑於先前技術之問題，本發明者認為應有一種由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，步驟至少包括：
(1).選取含銦、鎵和鋅之廢棄物；
(2).以無機酸以及去離子水酸浸；得到含有銦、鎵和鋅之浸出液；
(3).第一階段以有機磷酸類物加煤油之混合液對該浸出液進行萃取而萃取出油相含銦之有機物；剩下為水相而含有鎵與鋅之萃餘液；
(4).第二階段以有機磷酸類物加煤油之混合液對該萃餘液進行萃取，而萃取出油相含鎵之有機物；剩餘為含鋅之酸溶液；
(5).對於油相含銦之有機物以及油相含鎵之有機物，分別以無機酸進行反萃取，分別得到含銦之酸溶液以及含鎵之酸溶液；
(6).將含銦之酸溶液、含鎵之酸溶液以及含鋅之酸溶液，分別以鹼性物質進行化學沉澱；
(7).分別對6步驟之化學沉澱物，進行煆燒，以得到In2 O3 , Ga2 O3 and ZnO。
本發明係可以廣泛對於顯示面板的廢棄物以及靶材進行回收，尤其是例氧化鎵鋅(GZO, Gallium Zinc Oxide)和氧化銦鎵鋅(IGZO, Indium Gallium Zinc Oxide)等靶材。亦不限於此類靶材，本發明出可以先以浸出用硝酸目標並單獨提取前揭銦、鎵和鋅。然後再以二個步驟分別去進一步提取，在第一步驟中，銦是通過有機磷酸類物(較佳為濃度0.010-0.025mol/L之2-乙基己基磷酸(D2EHPA)加煤油，控制進行使得鎵和鋅留在銦被提取後再進行萃取，然後在第二步驟中以有機磷酸類物(較佳為濃度0.010-0.02mol/L之2-乙基己基磷酸(D2EHPA)加煤油將提取，然後通過鹽酸分別反萃取。分離後再將分別再循環並通過沉澱和煅燒，將銦、鎵、鋅以金屬氧化物之形式回收，並行資源再利用，最終之金屬回收率可高達99.9%。本發明主要對於同時含有銦、鎵和鋅之廢棄物進行回收，作業上能夠一體考量。
而值得說明的是，本發明之步驟並非簡易之酸解、化學沉澱等複合，更利用溶媒萃取技術，在以化學反應方法以外複合介面萃取(所謂高度選擇性)，更有效率地提升金屬離子之分離效果；產出並純化產物。In view of the problems of the prior art, the inventors believe that there should be a method for extracting such metals from wastes containing indium, gallium and zinc, the steps including at least:
(1). Select wastes containing indium, gallium and zinc;
(2) leaching with a mineral acid and deionized water; obtaining a leach solution containing indium, gallium and zinc;
(3) In the first stage, the leachate is extracted by extracting the leachate with an organic phosphate and kerosene mixture; the organic phase containing the indium is extracted; and the raffinate containing gallium and zinc is left in the aqueous phase;
(4). In the second stage, the raffinate is extracted by a mixture of organic phosphoric acid and kerosene, and the organic phase containing the gallium is extracted; the remaining is a zinc-containing acid solution;
(5). For the oil phase indium containing organic matter and the oil phase gallium containing organic matter, respectively, back extraction with a mineral acid to obtain an indium containing acid solution and a gallium containing acid solution;
(6) chemically precipitating an indium-containing acid solution, a gallium-containing acid solution, and a zinc-containing acid solution with an alkaline substance;
(7). The chemical precipitates of the 6 steps were respectively calcined to obtain In 2 O 3 , Ga 2 O 3 and ZnO.
In the present invention, wastes and targets of the display panel can be widely recovered, and in particular, targets such as gallium zinc oxide (GZO, Gallium Zinc Oxide) and indium gallium zinc oxide (IGZO, Indium Gallium Zinc Oxide) are used. It is not limited to such a target, and the present invention can first extract the indium, gallium and zinc by leaching with a nitric acid target and separately extracting it. Then, the extraction is further carried out in two steps. In the first step, the indium is controlled by adding an organic phosphoric acid (preferably a concentration of 0.010-0.025 mol/L of 2-ethylhexylphosphoric acid (D2EHPA) plus kerosene. The gallium and zinc are left to be extracted after the indium is extracted, and then extracted in the second step with an organic phosphoric acid (preferably a concentration of 0.010-0.02 mol/L of 2-ethylhexylphosphoric acid (D2EHPA) plus kerosene). Then, it is separately back-extracted by hydrochloric acid. After separation, it is separately recycled and precipitated and calcined, and indium, gallium, and zinc are recovered as metal oxides, and the resources are reused in parallel, and the final metal recovery rate can be as high as 99.9%. The invention mainly recovers wastes containing both indium, gallium and zinc, and can be integrated into the operation.
It should be noted that the steps of the present invention are not simple acid hydrolysis, chemical precipitation and the like, and the use of solvent extraction technology, in addition to chemical reaction methods, composite interface extraction (so-called high selectivity), more efficient metal ions The separation effect; the product is produced and purified.

第一圖係本發明流程圖。The first figure is a flow chart of the present invention.

以下藉由圖式之配合，說明本發明之構造、特點以及實施例，俾使貴審查委員對本發明有更進一步之理解。
請參閱第一圖所示，本發明係由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，步驟至少包括：
(1).選取含銦、鎵和鋅之廢棄物；該廢棄物包括IGZO之靶材，惟不侷限於靶材之廢棄物。
(2).以無機酸以及去離子水酸浸；得到含有銦、鎵和鋅之浸出液；該無機酸選自於鹽酸(HCl)，硝酸(HNO3 )和鹽酸(H2 SO4 )之其一，考量浸出時間與浸出率之平衡，其中以硝酸為較佳。
(3).第一階段以有機磷酸類物加煤油之混合液對該浸出液進行萃取而萃取出油相含銦之有機物；該煤油主要作為劑量擴增之載體，在此階段先就考量到以有機磷酸類物加煤油作為萃取劑，可以先將銦分離出。剩下為水相而含有鎵與鋅之萃餘液；該有機磷酸類物質係為濃度0.010-0.025mol/L之2-乙基己基磷酸(D2EHPA)。
(4).第二階段以有機磷酸類物加煤油之混合液對該萃餘液進行萃取，而萃取出油相含鎵之有機物；剩餘為含鋅之水溶液；該有機磷酸類物質係為濃度0.010-0.02mol/L之2-乙基己基磷酸(D2EHPA)。通過二個階段分別以有機磷酸類物加煤油作為「溶媒」，本發明結合溶媒萃取技術與化學沉澱技術，利用溶媒萃取之高度選擇性，提升金屬離子之分離效果。
(5).對於油相含銦之有機物以及油相含鎵之有機物，分別以無機酸進行反萃取，分別得到含銦之酸溶液以及含鎵之酸溶液；無機酸皆為1-3mole/L之鹽酸。
(6).將含銦之酸溶液、含鎵之酸溶液以及含鋅之水溶液，分別以鹼性物質進行化學沉澱；鹼性物質為氫氧化鈉。
(7).分別對6步驟之化學沉澱物，進行煆燒，以得到In2 O3 , Ga2 O3 and ZnO。
從化學沉澱法得到的氫氧化物，然後通過煆燒脫水變成氧化銦，氧化鎵和氧化鋅。
本發明透過浸出溶液，然後行溶劑萃取處理的兩級彼此分開銦、鎵和鋅。萃取後，鋅留在萃餘液，而銦和鎵是由鹽酸剝離(即反萃取)。然後這三個金屬沉澱，是用鹼性物質中之氫氧化鈉(NaOH)和通過煅燒轉化為金屬氧化物。
本發明主要對於同時含有銦、鎵和鋅之廢棄物進行回。而值得說明的是，本發明之步驟並非簡易之酸解、化學沉澱等複合，更利用溶媒萃取技術，在以化學反應方法以外複合介面萃取(所謂高度選擇性)，更有效率地提升金屬離子之分離效果；產出並精煉產物。
綜上所述，本發明確實符合產業利用性，且未於申請前見於刊物或公開使用，亦未為公眾所知悉，且具有非顯而易知性，符合可專利之要件，爰依法提出專利申請。惟上述所陳，為本發明產業上一較佳實施例，舉凡依本發明申請專利範圍所作之均等變化，皆屬本案訴求標的之範疇。The structure, features, and embodiments of the present invention will be described in conjunction with the drawings.
Referring to the first figure, the present invention is a method for extracting the metals from wastes containing indium, gallium and zinc, and the steps include at least:
(1). Select wastes containing indium, gallium, and zinc; this waste includes targets for IGZO, but is not limited to waste from targets.
(2) leaching with a mineral acid and deionized water; obtaining a leach solution containing indium, gallium and zinc; the inorganic acid being selected from the group consisting of hydrochloric acid (HCl), nitric acid (HNO 3 ) and hydrochloric acid (H 2 SO 4 ) First, consider the balance between leaching time and leaching rate, of which nitric acid is preferred.
(3). In the first stage, the leachate is extracted by extracting the leachate with organic phosphoric acid and kerosene to extract the organic phase containing the indium in the oil phase; the kerosene is mainly used as a carrier for dose amplification, and at this stage, The organic phosphoric acid and kerosene are used as an extracting agent, and the indium can be separated first. The remaining is an aqueous phase containing a raffinate of gallium and zinc; the organic phosphoric acid is 2-ethylhexylphosphoric acid (D2EHPA) having a concentration of 0.010-0.025 mol/L.
(4). In the second stage, the raffinate is extracted by a mixture of organic phosphoric acid and kerosene, and the organic phase containing gallium is extracted; the remaining is an aqueous solution containing zinc; the organic phosphoric acid is a concentration 0.010-0.02 mol/L of 2-ethylhexylphosphoric acid (D2EHPA). The organic phosphates and kerosene are used as "solvents" in two stages. The present invention combines solvent extraction technology and chemical precipitation technology, and utilizes the high selectivity of solvent extraction to enhance the separation effect of metal ions.
(5). For the organic phase containing the indium in the oil phase and the organic substance containing the gallium in the oil phase, respectively, back-extracting with the inorganic acid to obtain the acid solution containing indium and the acid solution containing gallium; the inorganic acid is 1-3 mole/L. Hydrochloric acid.
(6) The indium-containing acid solution, the gallium-containing acid solution, and the zinc-containing aqueous solution are respectively chemically precipitated with an alkaline substance; the basic substance is sodium hydroxide.
(7). The chemical precipitates of the 6 steps were respectively calcined to obtain In 2 O 3 , Ga 2 O 3 and ZnO.
The hydroxide obtained from the chemical precipitation method is then dehydrated by calcination to become indium oxide, gallium oxide and zinc oxide.
The present invention separates indium, gallium and zinc from each other through a leaching solution and then solvent extraction. After extraction, zinc remains in the raffinate, while indium and gallium are stripped (ie, back-extracted) by hydrochloric acid. These three metals are then precipitated using sodium hydroxide (NaOH) in a basic material and converted to a metal oxide by calcination.
The present invention is mainly directed to wastes containing both indium, gallium and zinc. It should be noted that the steps of the present invention are not simple acid hydrolysis, chemical precipitation and the like, and the use of solvent extraction technology, in addition to chemical reaction methods, composite interface extraction (so-called high selectivity), more efficient metal ions The separation effect; the product is produced and refined.
In summary, the present invention is indeed in line with industrial utilization, and is not found in publications or publicly used before application, nor is it known to the public, and has non-obvious knowledge, conforms to patentable requirements, and patents are filed according to law. . However, the above description is a preferred embodiment of the industry of the present invention, and all the equivalent changes made by the scope of the patent application of the present invention are within the scope of the claim.

Claims (6)

鎵和鋅之廢棄物中提取該等金屬之方法，步驟至少包括： (1).選取含銦、鎵和鋅之廢棄物； (2).以無機酸以及去離子水酸浸；得到含有銦、鎵和鋅之浸出液； (3).第一階段以有機磷酸類物加煤油之混合液對該浸出液進行萃取而萃取出油相含銦之有機物；剩下為水相而含有鎵與鋅之萃餘液； (4).第二階段以有機磷酸類物加煤油之混合液對該萃餘液進行萃取，而萃取出油相含鎵之有機物；剩餘為含鋅之水溶液； (5).對於油相含銦之有機物以及油相含鎵之有機物，分別以無機酸進行反萃取，分別得到含銦之酸溶液以及含鎵之酸溶液； (6).將含銦之酸溶液、含鎵之酸溶液以及含鋅之水溶液，分別以鹼性物質進行化學沉澱； (7).分別對6步驟之化學沉澱物，進行煆燒，以得到In2 O3 , Ga2 O3 and ZnO。The method for extracting the metals from the gallium and zinc wastes comprises at least: (1) selecting wastes containing indium, gallium, and zinc; (2) extracting with inorganic acid and deionized water; obtaining indium , leaching solution of gallium and zinc; (3). The first stage extracts the leaching solution by extracting the leaching solution with organic phosphoric acid and kerosene to extract the organic phase containing the indium in the oil phase; the remaining is the aqueous phase containing gallium and zinc The raffinate; (4). The second stage extracts the raffinate with a mixture of organic phosphoric acid and kerosene, and extracts the organic phase containing the gallium in the oil phase; the remaining is an aqueous solution containing zinc; (5). For the organic phase containing the indium in the oil phase and the organic substance containing the gallium in the oil phase, respectively, back-extracting with the inorganic acid to obtain the acid solution containing indium and the acid solution containing gallium; (6) the acid solution containing indium, containing gallium The acid solution and the zinc-containing aqueous solution are each chemically precipitated with an alkaline substance; (7) The 6-step chemical precipitate is separately calcined to obtain In 2 O 3 , Ga 2 O 3 and ZnO. 如申請專利範圍第1項所述之由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，其中該(2)步驟之無機酸選自於HCl，HNO3 和H2 SO4 之其一。A method for extracting the metals from wastes containing indium, gallium and zinc as described in claim 1, wherein the inorganic acid of the step (2) is selected from the group consisting of HCl, HNO 3 and H 2 SO 4 One of them. 如申請專利範圍第1項所述之由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，其中該第一階段之有機磷酸類物質係為濃度0.010-0.025mol/L之2-乙基己基磷酸(D2EHPA)。The method for extracting the metals from the wastes containing indium, gallium and zinc according to the first aspect of the patent application, wherein the first stage of the organic phosphoric acid is a concentration of 0.010-0.025 mol/L. Ethylhexylphosphoric acid (D2EHPA). 如申請專利範圍第1項所述之由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，其中該第一階段之有機磷酸類物質係為濃度0.010-0.02mol/L之2-乙基己基磷酸(D2EHPA)。The method for extracting the metals from wastes containing indium, gallium and zinc as described in claim 1 wherein the first stage organic phosphates are in a concentration of from 0.010 to 0.02 mol/L. Ethylhexylphosphoric acid (D2EHPA). 如申請專利範圍第1項所述之由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，其中該(5)步驟之無機酸皆為1-3mole/L之鹽酸。A method for extracting the metals from wastes containing indium, gallium and zinc as described in claim 1, wherein the inorganic acid in the step (5) is 1-3 mole/L hydrochloric acid. 如申請專利範圍第1項所述之由含銦、鎵和鋅之廢棄物中提取該等金屬之方法，其中該(6)步驟之鹼性物質為氫氧化鈉。A method for extracting the metals from wastes containing indium, gallium and zinc as described in claim 1 wherein the alkaline substance of the step (6) is sodium hydroxide.
TW105134890A 2016-10-28 2016-10-28 Method to extract the indium, gallium and zinc from spent igzo target TWI636139B (en)

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