JP4534591B2 - Recovery method of high purity oxalic acid aqueous solution - Google Patents
Recovery method of high purity oxalic acid aqueous solution Download PDFInfo
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- JP4534591B2 JP4534591B2 JP2004146086A JP2004146086A JP4534591B2 JP 4534591 B2 JP4534591 B2 JP 4534591B2 JP 2004146086 A JP2004146086 A JP 2004146086A JP 2004146086 A JP2004146086 A JP 2004146086A JP 4534591 B2 JP4534591 B2 JP 4534591B2
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- oxalic acid
- aqueous solution
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims description 119
- 235000006408 oxalic acid Nutrition 0.000 title claims description 39
- 238000000034 method Methods 0.000 title claims description 15
- 239000007864 aqueous solution Substances 0.000 title claims description 13
- 238000011084 recovery Methods 0.000 title description 3
- 238000005530 etching Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 23
- 239000003957 anion exchange resin Substances 0.000 claims description 20
- 229910052738 indium Inorganic materials 0.000 claims description 18
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 229920001429 chelating resin Polymers 0.000 description 3
- 238000005349 anion exchange Methods 0.000 description 2
- 239000003729 cation exchange resin Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- APCLRHPWFCQIMG-UHFFFAOYSA-N 4-(5,6-dimethoxy-1-benzothiophen-2-yl)-4-oxobutanoic acid Chemical compound C1=C(OC)C(OC)=CC2=C1SC(C(=O)CCC(O)=O)=C2 APCLRHPWFCQIMG-UHFFFAOYSA-N 0.000 description 1
- 229940125791 MSA-2 Drugs 0.000 description 1
- 108010057081 Merozoite Surface Protein 1 Proteins 0.000 description 1
- 101710162106 Merozoite surface antigen 2 Proteins 0.000 description 1
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 description 1
- 101100083855 Rattus norvegicus Pou2f3 gene Proteins 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 101150040893 skn-1 gene Proteins 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction, e.g. ion-exchange, ion-pair, ion-suppression or ion-exclusion
- B01D15/361—Ion-exchange
- B01D15/363—Anion-exchange
-
- 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
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- ing And Chemical Polishing (AREA)
- Liquid Crystal (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
本発明は、高純度シュウ酸水溶液の回収方法に関し、詳しくは、インジウム含有被エッチング材を処理したシュウ酸エッチング廃液から溶解した金属成分を分離して高純度のシュウ酸水溶液を回収する方法に関する。 The present invention relates to a method for recovering a high-purity oxalic acid aqueous solution, and more particularly to a method for recovering a high-purity oxalic acid aqueous solution by separating a dissolved metal component from an oxalic acid etching waste liquid obtained by treating an indium-containing material to be etched.
液晶表示装置、エレクトロルミネッセンス表示装置などの透明電極としては、インジウム含有被エッチング材、例えば、酸化インジウム―酸化錫（Ｉｎｄｉｕｍ−Ｔｉｎ−Ｏｘｉｄｅ、以下ＩＴＯと略す。）膜を所定のパターンにエッチン処理したものが使用されている。 As a transparent electrode of a liquid crystal display device, an electroluminescence display device, or the like, an indium-containing material to be etched, for example, indium-tin-oxide (hereinafter abbreviated as ITO) film is etched into a predetermined pattern. Things are used.
すなわち、ＩＴＯ透明電極は、ガラス等の基板上にＩＴＯ膜を形成し、レジストマスクを施し、ＩＴＯ膜をエッチング処理して形成される。そして、ＩＴＯ膜のエッチング液として、シュウ酸水溶液の使用が知られている。
しかしながら、上述の方法では、エッチング廃液が廃棄処理されているため、エッチング処理コストが高くなると共に、環境の悪化が問題となる。 However, in the above-described method, the etching waste liquid is discarded, so that the cost of the etching process becomes high and the deterioration of the environment becomes a problem.
本発明は、上記実情に鑑みてなされたものであり、その目的は、インジウム含有被エッチング材を処理したシュウ酸エッチング廃液から高純度シュウ酸水溶液の回収方法を提供することにある。 This invention is made | formed in view of the said situation, The objective is to provide the collection | recovery method of high purity oxalic acid aqueous solution from the oxalic acid etching waste liquid which processed the indium containing to-be-etched material.
本発明の要旨は、インジウム含有被エッチング材を処理したシュウ酸エッチング廃液から溶解した金属成分を分離して高純度のシュウ酸水溶液を回収するにあたり、シュウ酸エッチング廃液と、強塩基性陰イオン交換樹脂をシュウ酸で接触処理することにより得られるシュウ酸形陰イオン交換樹脂とを接触処理させることから成る高純度シュウ酸水溶液の回収方法に存する。 Gist of the present invention, the metal component dissolved oxalic acid etching waste liquid was treated with indium-containing material to be etched is separated Upon recovering high purity aqueous solution of oxalic acid, and oxalic acid etching waste liquid, strongly basic anion-exchange The present invention resides in a method for recovering a high-purity oxalic acid aqueous solution comprising contacting an oxalic acid-type anion exchange resin obtained by contact-treating a resin with oxalic acid .
本発明の方法によれば、高純度のシュウ酸水溶液が回収でき、そして、エッチング液として再利用できるため、エッチング処理におけるシュウ酸の使用量を軽減することが出来、その結果、透明電極の製造コストを低減することが出来る。 According to the method of the present invention, since a high-purity oxalic acid aqueous solution can be recovered and reused as an etching solution, the amount of oxalic acid used in the etching process can be reduced, and as a result, production of a transparent electrode Cost can be reduced.
以下、本発明を詳細に説明する。本発明の回収方法は、インジウム含有被エッチング材を処理したシュウ酸エッチング廃液を陰イオン交換樹脂と接触処理させることにより、溶解した金属成分を分離して高純度のシュウ酸水溶液を回収する方法である。 Hereinafter, the present invention will be described in detail. The recovery method of the present invention is a method for recovering a high-purity oxalic acid aqueous solution by separating the dissolved metal component by contacting the oxalic acid etching waste liquid treated with the indium-containing material to be etched with an anion exchange resin. is there.
具体的には、エッチング工程からシュウ酸エッチング液の全量または一部を抜出し、陰イオン交換樹脂と接触処理して金属成分、例えば、インジウム、錫などを陰イオン交換樹脂に吸着させて、高純度シュウ酸水溶液を回収する。そして、回収された高純度シュウ酸水溶液は、シュウ酸エッチング液として再利用する。 Specifically, all or a part of the oxalic acid etching solution is extracted from the etching process and contact-treated with an anion exchange resin to adsorb metal components such as indium and tin onto the anion exchange resin, thereby achieving high purity. Collect the aqueous oxalic acid solution. The recovered high-purity oxalic acid aqueous solution is reused as an oxalic acid etching solution.
本発明で処理するシュウ酸エッチング廃液は、ＩＴＯ膜などのインジウム含有被エッチング材をシュウ酸溶液でエッチン処理した際に生ずる廃液である。このシュウ酸エッチング廃液には、インジウム、錫などの金属成分がアニオン化してシュウ酸の錯体化合物として存在する。 The oxalic acid etching waste liquid to be treated in the present invention is a waste liquid generated when an indium-containing material to be etched such as an ITO film is etched with an oxalic acid solution. In this oxalic acid etching waste liquid, metal components such as indium and tin are anionized and exist as a complex compound of oxalic acid.
シュウ酸エッチング廃液におけるシュウ酸濃度は、通常３重量％以上、好ましくは３〜１０重量％、より好ましくは３〜７重量％である。シュウ酸濃度が３重量％未満の場合は、エッチング廃液に含まれている金属成分のアニオン化錯体化合物の生成が不十分で、陰イオン交換樹脂によって高純度のシュウ酸水溶液を回収することが出来ない。 The oxalic acid concentration in the oxalic acid etching waste liquid is usually 3% by weight or more, preferably 3 to 10% by weight, more preferably 3 to 7% by weight. When the oxalic acid concentration is less than 3% by weight, the anion exchange complex compound of the metal component contained in the etching waste liquid is insufficient, and a high purity oxalic acid aqueous solution can be recovered by the anion exchange resin. Absent.
陰イオン交換樹脂との接触処理は、カラムに充填された陰イオン交換樹脂を使用して行うことが好ましい。また、使用される陰イオン交換樹脂は、シュウ酸形陰イオン交換樹脂であり、強塩基性陰イオン交換樹脂をシュウ酸で接触処理することにより得られる。 The contact treatment with the anion exchange resin is preferably performed using the anion exchange resin packed in the column. Further, the anion exchange resin used is a sheet oxalic acid type anion exchange resin obtained by contact treatment of the strongly basic anion exchange resin with oxalic acid.
強塩基性陰イオン交換樹脂としてシュウ酸形陰イオン交換樹脂を使用することにより、廃液処理の最初からシュウ酸が回収でき、そのままエッチング液として再利用することが出来る。 By using an oxalic acid type anion exchange resin as a strongly basic anion exchange resin, oxalic acid can be recovered from the beginning of the waste liquid treatment and can be reused as it is as an etching solution.
強塩基性陰イオン交換樹脂としては、４級アンモニウム基を交換基として有する樹脂が使用でき、例えば、三菱化学（株）製のダイヤイオンSA10A（商品名）、ダイヤイオンSA20A（商品名）、ダイヤイオンPA316（商品名）、ダイヤイオンPA416（商品名）、ローム アンド ハッス社製のAmberlite IRA400（商品名）、Amberlite IRA410（商品名）、Amberlite IRA900（商品名）、Amberlite IRA910（商品名）、ザ ダウ ケミカル社製のDowex SBR（商品名）、Dowex SAR（商品名）、Dowex MSA-1（商品名）、Dowex MSA-2（商品名）が挙げられる。 As the strongly basic anion exchange resin, a resin having a quaternary ammonium group as an exchange group can be used. For example, Diaion SA10A (trade name), Diaion SA20A (trade name), diamond made by Mitsubishi Chemical Corporation AEON PA316 (product name), Diaion PA416 (product name), Amberlite IRA400 (product name), Amberlite IRA410 (product name), Amberlite IRA900 (product name), Amberlite IRA910 (product name) Examples include Dowex SBR (trade name), Dowex SAR (trade name), Dowex MSA-1 (trade name), and Dowex MSA-2 (trade name) manufactured by Dow Chemical.
金属成分の吸着が飽和状態となった陰イオン交換樹脂は、公知の方法、例えば、焼成して金属酸化物として回収する。 The anion exchange resin in which the adsorption of the metal component is saturated is recovered as a metal oxide by a known method, for example, baking.
以下、本発明を実施例により更に詳細に説明するが、本発明は、その要旨を超えない限り、以下の実施例に限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention still in detail, this invention is not limited to a following example, unless the summary is exceeded.
実施例１
５％シュウ酸溶液１．０Ｌに対しインジウム（Ｉｎ）を１．６４ｇ、スズ（Ｓｎ）を０．１５ｇの割合で溶解し、インジウム濃度１．６４ｇ／Ｌ、スズ濃度０．１５ｇ／Ｌのシュウ酸溶液を作成し、これをエッチング廃液とした。
Example 1
1.64 g of indium (In) and 0.15 g of tin (Sn) were dissolved in 1.0 L of a 5% oxalic acid solution at a ratio of 1.64 g / L indium and 0.15 g / L tin. An acid solution was prepared and used as an etching waste solution.
別に、ガラスカラム（内径１５ｍｍ×高さ４５０ｍｍ）にＯＨ形の強塩基性陰イオン交換樹脂（ダイヤイオンＳＡＮ−１、三菱化学（株）製）３０ｍｌを充填し、表１に示すような条件で強塩基性陰イオン交換樹脂のイオン形をＯＨ形からシュウ酸形へ変換した。 Separately, a glass column (inner diameter: 15 mm × height: 450 mm) was filled with 30 ml of OH-type strongly basic anion exchange resin (Diaion SAN-1, manufactured by Mitsubishi Chemical Corporation) under the conditions shown in Table 1. The ionic form of the strongly basic anion exchange resin was converted from the OH form to the oxalic acid form.
シュウ酸形とした陰イオン交換樹脂に対しエッチング廃液１．５Ｌを９０ｍｌ／ｈで通液し、流出した処理液を採取した。処理液のインジウム、スズ濃度をＩＣＰ−ＡＥＳ（誘導結合プラズマ発光分析装置）で測定した。処理液のインジウム、スズ濃度変化を図１に示す。なお、横軸は、単位樹脂量当たりの処理液量（Ｌ／Ｌ−樹脂）、および、縦軸は、インジウム又はスズの処理液濃度（ｍｇ／Ｌ）を示す。図１中、インジウムの濃度変化をＡ−１で示し、スズの濃度変化をＡ−２で示す。 Etching waste liquid 1.5 L was passed through the anion exchange resin in the oxalic acid form at 90 ml / h, and the outflowing processing liquid was collected. The indium and tin concentrations of the treatment liquid were measured with ICP-AES (inductively coupled plasma emission spectrometer). FIG. 1 shows changes in indium and tin concentrations in the treatment liquid. The horizontal axis represents the amount of treatment liquid per unit resin amount (L / L-resin), and the vertical axis represents the treatment liquid concentration (mg / L) of indium or tin. In FIG. 1, the change in indium concentration is indicated by A-1, and the change in tin concentration is indicated by A-2.
比較例１
実施例１において、イオン交換樹脂をH形の強酸性陽イオン交換樹脂（SKN１、三菱化学（株）製）に変えた（シュウ酸処理は行わず）以外は、実施例１と同様にしてエッチング廃液の処理を行った。処理液のインジウム、スズ濃度変化を図１に示す。図１中、インジウムの濃度変化をＢ−１で示し、スズの濃度変化をＢ−２で示す。
Comparative Example 1
Etching is performed in the same manner as in Example 1 except that the ion exchange resin is changed to an H-type strong acid cation exchange resin (SKN1, manufactured by Mitsubishi Chemical Corporation) (no oxalic acid treatment is performed). The waste liquid was treated. FIG. 1 shows changes in indium and tin concentrations in the treatment liquid. In FIG. 1, the concentration change of indium is indicated by B-1, and the concentration change of tin is indicated by B-2.
図１から、強塩基性陰イオン交換樹脂を使用した場合、シュウ酸エッチング廃液中の金属成分が吸着・除去されるが、陽イオン交換樹脂を使用した場合は、殆ど吸着されていないことが明らかである。 From FIG. 1, it is clear that when a strongly basic anion exchange resin is used, metal components in the oxalic acid etching waste liquid are adsorbed and removed, but when a cation exchange resin is used, it is hardly adsorbed. It is.
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
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| JP2004146086A JP4534591B2 (en) | 2004-05-17 | 2004-05-17 | Recovery method of high purity oxalic acid aqueous solution |
| TW94115241A TWI380953B (en) | 2004-05-17 | 2005-05-11 | Recovery of High Purity Oxalic Acid Aqueous Solution |
| KR20050040697A KR101206174B1 (en) | 2004-05-17 | 2005-05-16 | A Method for Recovering Aqueous Oxalic Acid Solution with High Purity |
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| JP2004146086A JP4534591B2 (en) | 2004-05-17 | 2004-05-17 | Recovery method of high purity oxalic acid aqueous solution |
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| JP4534591B2 true JP4534591B2 (en) | 2010-09-01 |
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| JP4643541B2 (en) * | 2006-10-17 | 2011-03-02 | 東亞合成株式会社 | Method for producing indium compound from ferrous chloride solution |
| JP5817123B2 (en) * | 2011-01-18 | 2015-11-18 | 栗田工業株式会社 | Apparatus for recovering oxalate ions from indium oxalate aqueous solution, and method for recovering oxalate ions from indium oxalate aqueous solution |
| CN102703699B (en) * | 2012-06-26 | 2013-12-04 | 西部鑫兴金属材料有限公司 | Recycling method of acid waste liquid after treatment of high-lead rhenium-containing molybdenum concentrate |
| CN102935298A (en) * | 2012-11-28 | 2013-02-20 | 湖北益泰药业有限公司 | Method for recovering refined oxalate mother liquor |
| CN113929226A (en) * | 2021-10-29 | 2022-01-14 | 西安泰金工业电化学技术有限公司 | Oxalic acid waste liquid recovery system and recovery method |
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2004
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- 2005-05-16 KR KR20050040697A patent/KR101206174B1/en active IP Right Grant
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01102033A (en) * | 1987-10-15 | 1989-04-19 | Sumitomo Chem Co Ltd | Removal of organic acid |
| JPH05339197A (en) * | 1992-06-10 | 1993-12-21 | Asahi Glass Co Ltd | Separation and recovery of oxalic acid |
| JPH06322563A (en) * | 1993-05-10 | 1994-11-22 | Tsurumi Soda Co Ltd | Treating method of etching waste liquid |
| JPH07141932A (en) * | 1993-11-18 | 1995-06-02 | Kanto Chem Co Inc | Etching liquid composition for transparent conductive film |
| JPH1192840A (en) * | 1997-09-22 | 1999-04-06 | Daiichi Kigensokagaku Kogyo Co Ltd | Refining of zirconium |
| JP2001040434A (en) * | 1999-07-29 | 2001-02-13 | Sumitomo Chem Co Ltd | Method for recovering and refining indium |
| JP2002124506A (en) * | 2000-10-12 | 2002-04-26 | Toshiba Corp | Etching solution and etching method for indium tin oxide films |
| JP2003155361A (en) * | 2001-08-28 | 2003-05-27 | Asahi Glass Engineering Co Ltd | Method for producing anion exchange membrane |
| JP2004130175A (en) * | 2002-10-09 | 2004-04-30 | Mitsubishi Materials Corp | Method for separating metal ion from solution of metal complex |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101206174B1 (en) | 2012-11-28 |
| TW200600464A (en) | 2006-01-01 |
| JP2005325082A (en) | 2005-11-24 |
| KR20060047945A (en) | 2006-05-18 |
| TWI380953B (en) | 2013-01-01 |
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