JP4918839B2 - Disposal of display panel waste - Google Patents
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- JP4918839B2 JP4918839B2 JP2006274945A JP2006274945A JP4918839B2 JP 4918839 B2 JP4918839 B2 JP 4918839B2 JP 2006274945 A JP2006274945 A JP 2006274945A JP 2006274945 A JP2006274945 A JP 2006274945A JP 4918839 B2 JP4918839 B2 JP 4918839B2
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- 239000002699 waste material Substances 0.000 title claims description 35
- 239000011521 glass Substances 0.000 claims description 85
- 239000000843 powder Substances 0.000 claims description 37
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 29
- 230000005484 gravity Effects 0.000 claims description 27
- 238000000926 separation method Methods 0.000 claims description 21
- 238000010298 pulverizing process Methods 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 17
- 239000004973 liquid crystal related substance Substances 0.000 claims description 16
- 238000003672 processing method Methods 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 15
- 238000004090 dissolution Methods 0.000 claims description 13
- 150000002739 metals Chemical class 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 description 37
- 239000000463 material Substances 0.000 description 20
- 239000000047 product Substances 0.000 description 18
- 239000010408 film Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000011282 treatment Methods 0.000 description 9
- 239000006063 cullet Substances 0.000 description 7
- 229910052738 indium Inorganic materials 0.000 description 7
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- -1 indium Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical group [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/60—Glass recycling
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- Liquid Crystal (AREA)
- Processing Of Solid Wastes (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
- Glass Melting And Manufacturing (AREA)
Description
本発明は、液晶パネルやプラズマディスプレイパネルなど(これら含めて表示パネルと云う)の廃棄物について、ガラス基板に付着されているインジウム等の有価金属を回収すると共に、該表示パネル廃棄物の粉砕物からガラス粉末と付着物とを分離し、再利用に適するガラス粉末を回収することができる処理方法に関する。 The present invention recovers valuable metals such as indium adhering to a glass substrate from wastes such as liquid crystal panels and plasma display panels (including display panels) and pulverizes the display panel wastes. The present invention relates to a processing method capable of separating glass powder and deposits from the glass and recovering glass powder suitable for reuse.
液晶パネルは、例えば、ガラス基板の間に配向膜やカラーフィルター等が挟み込まれ、これらはゲートラインやソーズラインによって縦横に区画され、ここに対向電極やアクティブ素子が組み込まれており、外表面は偏光板によって覆われ、これらが一体に積層された構造を有している。偏光板、配向膜およびカラーフィルター等は樹脂製であり、電極はITO(In-Sn合金酸化物)などによって形成されており、ゲートラインやソーズラインはクロム、アルミニウムなどの蒸着によって形成されている。 In the liquid crystal panel, for example, an alignment film, a color filter, etc. are sandwiched between glass substrates, and these are partitioned vertically and horizontally by a gate line and a saws line, in which counter electrodes and active elements are incorporated, and the outer surface is polarized. It is covered with a plate and has a structure in which these are laminated together. The polarizing plate, the alignment film, the color filter, and the like are made of resin, the electrodes are formed of ITO (In-Sn alloy oxide) or the like, and the gate lines and the source lines are formed by vapor deposition of chromium, aluminum, or the like.
このように液晶パネル等はガラス基板表面に有価金属が蒸着等によって付着形成されているので、液晶パネル廃棄物からこれらの有価金属を回収し、あるいはガラス表面を無害化する方法が従来知られている。 As described above, since valuable metals are attached to the surface of a glass substrate by vapor deposition or the like in a liquid crystal panel or the like, a method for recovering these valuable metals from liquid crystal panel waste or detoxifying the glass surface is conventionally known. Yes.
例えば、特開平11−197641号(特許文献1)には、FPDを破砕した後に、このガラス粉砕物と研作材とを混ぜてタンク内に入れ、さらに細粒状に粉砕する物理的処理と、粉砕ガラスを各種洗浄剤に浸漬し洗浄する化学的処理との組み合わせからなるガラス表面無害化処理方法が知られている。 For example, in JP-A-11-197641 (Patent Document 1), after pulverizing FPD, this glass pulverized product and polishing material are mixed and placed in a tank, and further pulverized into a physical process and pulverization. A glass surface detoxification method comprising a combination of chemical treatments in which glass is immersed in various cleaning agents and washed is known.
しかし、この方法は、ガラスの種別を選別していないので、ガラスの再利用には適さない。ガラスを再利用するには単一品種のガラスカレットが必要であり、この方法では単一品種のガラスカレットを回収することができない。また、この方法は、ガラス粉砕物に研作材を混合して細粒粉砕しているので、研作材が残留すると、これがガラス再利用の妨げになる。 However, this method is not suitable for glass reuse because it does not select the type of glass. Reusing glass requires a single type of glass cullet, and this method cannot recover a single type of glass cullet. Further, in this method, the polishing material is mixed with the pulverized glass and finely pulverized. Therefore, if the polishing material remains, this hinders glass reuse.
特開2001−305501号(特許文献2)には、液晶パネル廃棄物について、偏向板剥離、パネル切断、液晶回収の各工程を経て、蛍光X線分析でパネルのガラスを種類別に選別し、ガラス破砕してガラス表面の薄膜を機械的方法(ボールミル等)で剥離(除去)することによって、金属粉とガラスカレットとに分離する廃液晶パネル処理方法が記載されている。分離した金属粉からはIn、Cr等の金属を回収し、ガラスカレットは単一品種なので原料ガラスとして再利用する。 In JP-A-2001-305501 (Patent Document 2), liquid crystal panel waste is subjected to deflection plate peeling, panel cutting, and liquid crystal recovery steps, and the glass of the panel is sorted by type by fluorescent X-ray analysis. A waste liquid crystal panel processing method is described in which a thin film on a glass surface is crushed and peeled (removed) by a mechanical method (such as a ball mill) to separate it into metal powder and glass cullet. Metals such as In and Cr are recovered from the separated metal powder, and since the glass cullet is a single product, it is reused as raw glass.
この方法は、薄膜除去工程でガラス表面の薄膜を機械的に剥離して金属粉とガラスカレットとに分離するが、粉砕物の粒径が大きいと十分な剥離効果が得られず、しかも剥離した金属粉とガラス粉の分離については開示されておらず、これを分離回収する工程が不十分である。因みに、剥離した金属粉とガラス粉を篩等で分級しても、これらを十分に分離することは出来ない。 In this method, the thin film on the glass surface is mechanically peeled in the thin film removal step to separate the metal powder and the glass cullet, but if the pulverized product has a large particle size, a sufficient peeling effect cannot be obtained, and the film is peeled off. The separation of metal powder and glass powder is not disclosed, and the process of separating and recovering this is insufficient. Incidentally, even if the separated metal powder and glass powder are classified with a sieve or the like, they cannot be sufficiently separated.
特開2001−170603号(特許文献3)には、廃棄パソコン類を超臨界反応器に投入して分解・溶解し固体残渣を得る処理方法が記載されており、特開2000−84531号(特許文献4)には、液晶パネルを破砕してカレットを非鉄製錬炉に投入する処理方法が記載されている。さらに、特開2001−350137号(特許文献5)には、熱分解したガラス基板の分離処理にサンドブラストを行なう処理方法が記載されている。 Japanese Patent Application Laid-Open No. 2001-170603 (Patent Document 3) describes a treatment method in which waste personal computers are put into a supercritical reactor to be decomposed and dissolved to obtain a solid residue. Document 4) describes a treatment method in which a liquid crystal panel is crushed and cullet is put into a non-ferrous smelting furnace. Furthermore, Japanese Patent Application Laid-Open No. 2001-350137 (Patent Document 5) describes a processing method of performing sandblasting for separation processing of a thermally decomposed glass substrate.
しかし、超臨界反応や非鉄製錬炉を利用する方法は、処理物がスラグとなりガラスとして再利用ができず、しかも超臨界反応を利用するには設備費が嵩む問題がある。一方、サンドブラストを利用する方法は、液晶パネルのガラス基板の厚さが0.7mmと非常に薄いため破損し易く、この方法でガラス表面の蒸着金属を剥離するのは困難である。
本発明は、液晶パネル等の表示パネル廃棄物の処理方法について、従来方法の上記問題を解決したものであり、ガラス基板に金属電極や樹脂フィルム等(これらを含めて付着物と云う)が施されている表示パネルについて、付着されているインジウム等の有価金属を回収すると共に、該表示パネル廃棄物の粉砕物からガラス粉末と付着物とを効果的に分離し、再利用に適するガラス粉末を回収することができる処理方法を提供する。 The present invention solves the above-mentioned problems of conventional methods for the treatment of display panel waste such as liquid crystal panels, and a glass substrate is provided with a metal electrode, a resin film, etc. (including these materials). In addition to recovering attached valuable metals such as indium, the display panel waste is effectively separated from the crushed material of the display panel waste, and a glass powder suitable for reuse is obtained. A processing method that can be recovered is provided.
本発明は、以下に示す構成によって上記問題を解決した、表示パネル廃棄物の処理方法に関する。
〔1〕 ガラス基板上に電極構造が形成された表示パネルの廃棄物について、ガラスの種類別に選別する工程(ガラス選別工程)、選別した上記廃棄物を微粉砕する工程(粉砕工程)、上記微粉砕物を酸溶解して溶出した有価金属を回収する工程(酸溶解工程)、酸溶解後の固形分を比重選別によってガラス粉末と付着物とを分離する工程(分離工程)を有する処理方法において、王水、塩酸、または硝酸を加え、スラリーの水分濃度を25〜75%にして粉砕することによって破砕工程と酸溶解工程を同時に行うことを特徴とする表示パネル廃棄物の処理方法。
〔2〕 表示パネルが液晶パネル、またはプラズマディスプレイパネルである上記[1]に記載する表示パネル廃棄物の処理方法。
〔3〕 粉砕工程において、表示パネル廃棄物を200メッシュ以下に粉砕する上記[1]または上記[2]に記載する表示パネル廃棄物の処理方法。
〔4〕 分離工程において、固液分離した固形分に水を加えて懸濁液にし、これを僅かに傾斜している振動テーブルの上面に供給して比重差に応じてガラス粉末と付着物とに分離する上記[1]〜上記[3]の何れかに記載する表示パネル廃棄物の処理方法。
〔5〕 分離工程において、比重選別に代えて、微粉砕物を浮遊選別によってガラス粉末と付着物とを分離する上記[1]〜上記[4]の何れかに記載する表示パネル廃棄物の処理方法。
The present invention relates to a method for treating display panel waste, which solves the above problems by the following configuration.
[1] About the waste of the display panel in which the electrode structure is formed on the glass substrate, the step of sorting by glass type (glass sorting step), the step of finely grinding the sorted waste (grinding step), In the processing method which has the process (separation process) which isolate | separates glass powder and a deposit | attachment by the density | concentration selection of the solid content after acid dissolution , the process of collect | recovering the valuable metals which melt | dissolved by acid dissolving the ground material A method for treating display panel waste, wherein a crushing step and an acid dissolution step are simultaneously performed by adding aqua regia, hydrochloric acid, or nitric acid, and crushing the slurry with a water concentration of 25 to 75% .
[2] The method for treating display panel waste according to the above [1], wherein the display panel is a liquid crystal panel or a plasma display panel.
[3] The method for treating display panel waste according to [1] or [2] above, wherein the display panel waste is pulverized to 200 mesh or less in the pulverization step.
[4] In the separation step, water is added to the solid content separated into solid and liquid to form a suspension, which is supplied to the top surface of a slightly inclined vibration table, and the glass powder and the adhering matter are separated according to the specific gravity difference. The method for disposing of display panel waste according to any one of [1] to [3] above.
[5] Treatment of display panel waste according to any one of [1] to [4] above, wherein in the separation step, instead of specific gravity sorting, finely pulverized material is separated from glass powder and deposits by floating sorting. Method.
本発明の処理方法は、最初に表示パネル廃棄物をガラスの種類別に選別するので、単一種類のガラスカレットを得ることができ、ガラスを再利用するのに適する。また、表示パネルを微粉砕して酸溶解することによってITOなどの有価金属を溶出回収することができる。さらに、溶出金属を除去した微粉砕物を比重選別あるいは浮遊選別によって分離することによってガラス粉末を付着物から分離して回収することができる。また、分離工程は振動テーブルによる比重選別または浮遊選別を行うので、ガラス粉末と付着物との分離性が良く、蒸着金属などの付着物が非常に少ないガラス粉末を回収することができる。 The processing method of the present invention first sorts display panel wastes by glass type, so that a single type of glass cullet can be obtained, which is suitable for reusing glass. Also, valuable metals such as ITO can be eluted and recovered by finely pulverizing the display panel and dissolving it with an acid. Furthermore, the glass powder can be separated and collected from the deposit by separating the finely pulverized product from which the eluted metal has been removed by specific gravity sorting or floating sorting. In addition, since the separation step performs specific gravity sorting or floating sorting using a vibration table, the separation between the glass powder and the deposit is good, and the glass powder with very little deposit such as vapor deposition metal can be collected.
本発明の処理方法は、粉砕工程において、表示パネル廃棄物を200メッシュ以下に粉砕することによって、ガラス表面の蒸着物等の剥離効果を高めることができる。また、水分濃度25〜75%、好ましくは25〜50%で表示パネルを粉砕することによって、粉砕効果を高めることができる。 The processing method of this invention can heighten the peeling effect of the vapor deposition etc. of the glass surface by grind | pulverizing a display panel waste to 200 mesh or less in a grinding | pulverization process. Further, the pulverization effect can be enhanced by pulverizing the display panel at a moisture concentration of 25 to 75%, preferably 25 to 50%.
本発明の処理方法は、酸性溶液を粉砕工程に供給して粉砕を行うことによって、粉砕工程と酸溶解工程とを同時に行うことができ、粉砕工程後の溶解工程を省略することができるので、処理工程が簡略になり、処理時間を短縮することができる。 The treatment method of the present invention can perform the pulverization step and the acid dissolution step simultaneously by supplying the acidic solution to the pulverization step, and the dissolution step after the pulverization step can be omitted. The processing steps are simplified and the processing time can be shortened.
本発明の処理方法は、比重差を利用した分離装置、例えば、僅かに傾斜している振動テーブルの上面に微粉砕物を液体と共に供給し、粉砕物を比重差に応じて分離する薄流選別を行うことによって、ガラス粉末と付着物とが比重に応じて振動テーブル上に分散するので、ガラス粉末と付着物との高い分離効果を得ることができる。 The processing method of the present invention is a separation apparatus using a specific gravity difference, for example, a thin-flow sorting method in which finely pulverized material is supplied together with a liquid to the upper surface of a slightly inclined vibration table, and the pulverized material is separated according to the specific gravity difference. Since the glass powder and the deposit are dispersed on the vibration table according to the specific gravity, a high separation effect between the glass powder and the deposit can be obtained.
本発明の処理方法は、振動テーブルによる比重選別に代えて、微粉砕物を浮遊選別することによってガラス粉末と付着物とを効果的に分離し、付着物の少ないガラス粉末を回収することができる。また、分離したガラス付着物を重液選別によって更に有機物と金属粉とに分離することによって、有機物を除去して金属粉を回収することができる。 The treatment method of the present invention can effectively separate glass powder and deposits by floating sorting finely pulverized material instead of specific gravity sorting using a vibration table, and collect glass powder with less deposits. . Moreover, by separating the separated glass deposit into an organic substance and a metal powder by heavy liquid sorting, the organic substance can be removed and the metal powder can be recovered.
本発明の処理方法は液晶パネル、プラズマディスプレイパネルなどのガラス基板に金属や樹脂フィルム等が施されている表示パネルに広く適用することができる。 The treatment method of the present invention can be widely applied to display panels in which a metal substrate, a resin film, or the like is applied to a glass substrate such as a liquid crystal panel or a plasma display panel.
本発明の処理方法の概略を図1に示す。
図示するように、本発明の処理方法は、ガラス基板上に電極構造が形成された表示パネルの廃棄物について、ガラスの種類別に選別する工程(ガラス選別工程)、選別した表示パネル廃棄物を微粉砕する工程(粉砕工程)、上記微粉砕物を酸溶解して溶出した有価金属を回収する工程(酸溶解工程)、溶出金属を除去した微粉砕物を比重差を利用した分離装置に供給して比重選別によりガラス粉末と付着物とを分離する工程(分離工程)を有することを特徴とする表示パネル廃棄物の処理方法である。
An outline of the treatment method of the present invention is shown in FIG.
As shown in the figure, the processing method of the present invention is a process for sorting display panel waste having an electrode structure formed on a glass substrate according to the type of glass (glass sorting process). Supplying the pulverized step (pulverizing step), the step of recovering valuable metals eluted by dissolving the finely pulverized product in acid (acid dissolving step), and the finely pulverized product from which the eluted metals have been removed to a separator utilizing the specific gravity difference The display panel waste processing method further includes a step (separation step) of separating the glass powder and the deposit by specific gravity sorting.
〔ガラス選別工程〕
表示パネル廃棄物について、ガラスの種別を判定し、ガラスの種類ごとに分別する。ガラスの種別を判定する方法は蛍光X線分析等によることができる。X線分析によって得られる回折ピークによってガラス成分を把握し、種別を判定して組成の近いものにグループ分けする。
[Glass sorting process]
About display panel waste, the kind of glass is judged and classified according to the kind of glass. The method of determining the type of glass can be based on fluorescent X-ray analysis or the like. The glass component is grasped by the diffraction peak obtained by X-ray analysis, the type is determined, and the components are grouped into those having similar compositions.
〔粉砕工程〕
ガラスの種類に応じて分別した表示パネル廃棄物を切断し、破砕機に入れて微粉砕する。破砕機としてはボールミル或いはタワーミル等を用いることができる。好ましくは、粒径200メッシュ以下(74μm以下)に粉砕する。ガラス基板とその上に構成される付着物(金属、有機物フィルム等)とは、サブミクロンオーダーまで破砕すれば、両者の物性の違いによって接合界面近傍より分離することが期待される。しかし、このサイズまで破砕するのは容易ではない。
[Crushing process]
The display panel waste sorted according to the type of glass is cut, put into a crusher, and pulverized. As the crusher, a ball mill or a tower mill can be used. Preferably, it grind | pulverizes to a particle size of 200 mesh or less (74 micrometers or less). If the glass substrate and the deposits (metal, organic film, etc.) formed thereon are crushed to the submicron order, it is expected to be separated from the vicinity of the bonding interface due to the difference in physical properties between the two. However, crushing to this size is not easy.
本発明は、表示パネル廃棄物を粒径200メッシュ以下に粉砕すれば、粒径がサブミクロンまで至らないものの、破砕物どうしの相互摩擦によってガラス表面の付着物の剥離効果が高まり、分離性が向上し、付着物が大幅に少ないガラス粉末を得ることができる効果を得た。また、この粉砕と相互摩耗によって粉砕物の形状が球形に近づくことから、後工程の比重選別等での分離効果を高めることができる。 In the present invention, if the display panel waste is pulverized to a particle size of 200 mesh or less, the particle size does not reach submicron, but the effect of peeling off the adhered substance on the glass surface is enhanced by the mutual friction between the crushed materials. It was improved and the effect that the glass powder with much less deposits can be obtained was obtained. Moreover, since the shape of the pulverized product approaches a spherical shape due to this pulverization and mutual wear, the separation effect in the specific gravity selection in the subsequent process can be enhanced.
粉砕の途中で篩にかけて、有機分(フィルムなど)の大半を分離しておけば、後の微粉砕が効率的になりなお良い。更に粉砕物を重液選別することによって、有機分と金属粉とに分離することができる。重液としては硫酸などを用いるとよい。 If most of the organic components (film, etc.) are separated by sieving in the middle of pulverization, the subsequent fine pulverization becomes more efficient. Furthermore, the pulverized product can be separated into an organic component and a metal powder by heavy liquid sorting. As the heavy liquid, sulfuric acid or the like may be used.
粉砕工程において、粉砕物に液体(純水等)を添加することによって破砕効率を高めることができる。ただし、スラリー濃度が高くなると流動性が低下するために排鉱能力が低下する。効率のよい水分濃度は25〜75%であり、最適は25〜50%である。添加する液体は、純水、酸溶液などを用いることができる。 In the pulverization step, crushing efficiency can be increased by adding a liquid (pure water or the like) to the pulverized product. However, if the slurry concentration is increased, the fluidity is lowered, so that the ore discharging capacity is lowered. Efficient moisture concentration is 25-75%, optimal is 25-50%. As the liquid to be added, pure water, an acid solution, or the like can be used.
〔酸溶解工程〕
上記粉砕物を酸溶解して溶出した有価金属を回収する。粉砕物に王水や硝酸などを加えることによって、ガラス表面に付着しているインジウム等の有価金属が溶出する。これを固液分離し、溶出金属を含む濾液からインジウム等を回収する。なお、インジウムを回収する場合には、インジウムと錫との分離性が高まるので硝酸を用いるとよい。
[Acid dissolution step]
The pulverized product is acid-dissolved to recover valuable metals eluted. By adding aqua regia or nitric acid to the pulverized product, valuable metals such as indium adhering to the glass surface are eluted. This is subjected to solid-liquid separation, and indium and the like are recovered from the filtrate containing the eluted metal. In the case of recovering indium, nitric acid is preferably used because the separation between indium and tin is improved.
上記破砕工程において、王水や塩酸、硝酸を加えて破砕を行うことによって、破砕機内部で粉砕と同時に酸溶解が同時に進行するので、破砕工程と酸溶解工程とを同時に行うことができ、破砕工程後の酸溶解工程を省略することができる。この酸溶解工程の省略によって処理系全体の処理時間を短縮することができる。なお、王水や塩酸、硝酸を加えて破砕を行う場合にはスラリーの水分濃度は上記範囲が好ましい。 In the above crushing process, aqua regia, hydrochloric acid and nitric acid are added to crush, so that acid dissolution proceeds simultaneously with crushing inside the crusher, so that crushing process and acid dissolution process can be performed simultaneously, crushing The acid dissolution step after the step can be omitted. By omitting this acid dissolution step, the processing time of the entire processing system can be shortened. In addition, when crushing by adding aqua regia, hydrochloric acid and nitric acid, the water concentration of the slurry is preferably within the above range.
〔分離工程〕
溶出金属を濾過洗浄等で除去した粉砕物(ガラス粉末および付着粉砕物)を比重差を利用した分離装置に供給して比重選別によりガラスと付着粉砕物とを分離する。比重選別は、例えば、僅かに傾斜している振動テーブルの上面に粉砕物を液体と共に供給する薄流選別によって、微粉砕物を比重差に応じて分離すればよい。振動テーブルは、比重選鉱に用いられている揺動テーブル、選鉱テーブルと称される一般的な振動テーブルを用いることができる。振動の強さや振動テーブル上面に供給する粉砕物および液体の量は装置条件や処理条件に応じて適宜定めればよい。振動テーブル上面に供給された粉砕物は比重差による運動の違いが生じ、水の力によって、比重の小さい粉砕物は比重の大きい粉砕物よりも遠方に流されるので、テーブル上面で比重差に応じて分散し、ガラス粉末と付着粉砕物とが分離される。振動テーブルは一段から多段とすることで、分離効果を高めることができる。比重選別の装置には、振動テーブルのほかにジグ選別機、エアーテーブルなどもある。
[Separation process]
The pulverized product (glass powder and adhering pulverized product) from which the eluted metal has been removed by filtration washing or the like is supplied to a separator utilizing the specific gravity difference, and the glass and the adhering pulverized product are separated by specific gravity sorting. In the specific gravity sorting, for example, the finely pulverized material may be separated according to the specific gravity difference by thin flow sorting in which the pulverized material is supplied together with the liquid to the upper surface of the slightly tilted vibration table. As the vibration table, a general vibration table called a rocking table or a beneficiation table used for specific gravity beneficiation can be used. The intensity of vibration and the amount of pulverized material and liquid supplied to the upper surface of the vibration table may be appropriately determined according to apparatus conditions and processing conditions. The crushed material supplied to the upper surface of the vibration table has a difference in motion due to the difference in specific gravity, and the pulverized material having a lower specific gravity is caused to flow farther than the pulverized material having a higher specific gravity due to the force of water. And dispersed to separate the glass powder and the adhered pulverized product. The separation effect can be enhanced by changing the vibration table from one stage to multiple stages. Specific gravity sorting devices include jig sorters and air tables in addition to vibrating tables.
上記比重選別によれば、回収すべき基板ガラス粉末と、その他のガラス付着物(金属分の配向膜対向電極、液晶駆動電極、ゲートバスライン、ソースバスライン等、および有機分の配向膜等、フィルム等)とを比重差を利用して容易に分離することができる。また、比重選別に先立って粉砕工程を経ているので、粒径の影響が少なく、分離効果を高めることができる。 According to the above specific gravity sorting, the substrate glass powder to be recovered and other glass deposits (metal alignment film counter electrode, liquid crystal drive electrode, gate bus line, source bus line, etc., organic alignment film, etc., Film etc.) can be easily separated using the specific gravity difference. In addition, since the pulverization step is performed prior to the specific gravity selection, the influence of the particle size is small and the separation effect can be enhanced.
分離工程において、振動テーブルによる比重選別に代えて、微粉砕物を浮遊選別によってガラス粉末と付着粉砕物とを分離してもよい。ガラス粉末と付着粉砕物の濡れ性(親和力)の違いを利用し、適切な浮選剤を選択することによって、ガラス粉末と付着粉砕物を良好に分離することができる。 In the separation step, the glass powder and the adhered pulverized material may be separated from the finely pulverized product by floating sorting instead of the specific gravity sorting by the vibration table. By utilizing the difference in wettability (affinity) between the glass powder and the adhered pulverized material and selecting an appropriate flotation agent, the glass powder and the adhered pulverized material can be well separated.
以下、本発明の実施例を示す。
〔実施例1〕
偏向板付液晶パネル廃棄物を蛍光X線分析によってガラスの種類ごとに分別し、同種類のパネル廃棄物を切断し、粉砕器(ボールミル)に入れて200メッシュ以下に粉砕した。この粉砕物100gに7%濃度塩酸200mlを加えて2時間攪拌した。これを濾過して含水固形分を分離した。この含水固形分に水を加えて懸濁液にし、僅かに傾斜した振動テーブル上面に供給し、薄流選別を行い、ガラス粉末82gを回収した。回収したガラス粉末の成分を表1に示した。比較のため液晶パネルに使用されている基板ガラス(A種、B種、C種)の成分を表1に示した。回収したガラス粉末は基板ガラスCの組成と一致しており、付着物は検出限界以下であった。
Examples of the present invention will be described below.
[Example 1]
The liquid crystal panel waste with a deflector was separated according to the type of glass by fluorescent X-ray analysis, the panel waste of the same type was cut, put into a pulverizer (ball mill), and pulverized to 200 mesh or less. To 100 g of this pulverized product, 200 ml of 7% hydrochloric acid was added and stirred for 2 hours. This was filtered to separate the water-containing solid. Water was added to this water-containing solid content to form a suspension, which was supplied to the top surface of a slightly inclined vibration table, and subjected to thin-flow sorting to recover 82 g of glass powder. The components of the collected glass powder are shown in Table 1. Table 1 shows the components of the substrate glass (A type, B type, C type) used in the liquid crystal panel for comparison. The recovered glass powder was in agreement with the composition of the substrate glass C, and the deposits were below the detection limit.
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