JP2017209607A - Method of treating polarizer production waste liquid - Google Patents
Method of treating polarizer production waste liquid Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C01D3/12—Iodides
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
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- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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Abstract
Description
本発明は、偏光板製造廃液の処理方法に関し、より詳しくは、偏光板の製造工程で生じる廃液からヨウ化カリウム溶液を回収する偏光板製造廃液の処理方法に関する。 The present invention relates to a method for treating a polarizing plate production waste liquid, and more particularly to a method for treating a polarizing plate production waste liquid for recovering a potassium iodide solution from the waste liquid produced in the production process of a polarizing plate.
偏光板の製造工程で生じる廃液には、ヨウ素やホウ素、カリウム等の無機物成分や、ポリビニルアルコール(PVA)等の有機物成分が含まれており、このような偏光板製造廃液の処理方法が従来から検討されている。 The waste liquid produced in the manufacturing process of the polarizing plate contains inorganic components such as iodine, boron, and potassium, and organic components such as polyvinyl alcohol (PVA). It is being considered.
従来の偏光板製造廃液の処理方法としては、水酸化ナトリウム等のアルカリを添加して濃縮することが一般的であるが、ヨウ素の回収が煩雑になり易いことから、特許文献1には、廃液を電気透析することにより有機物成分を含む脱塩液と無機物成分を含む濃縮液とを分離し、濃縮液を更に処理することでヨウ素分等を回収することが開示されている。 As a conventional method for treating a polarizing plate production waste liquid, it is common to add and concentrate an alkali such as sodium hydroxide. However, since the recovery of iodine tends to be complicated, Patent Document 1 discloses a waste liquid. Is separated from a desalted solution containing an organic component and a concentrated solution containing an inorganic component by electrodialysis, and iodine is recovered by further processing the concentrated solution.
ところが、上記のように廃液を電気透析によって処理する方法は、メンテナンス上の問題が生じ易いと共に、装置コストが高くなるという問題があった。 However, the method of treating the waste liquid by electrodialysis as described above has a problem that maintenance problems are likely to occur and the cost of the apparatus is increased.
そこで、本発明は、偏光板製造廃液からヨウ化カリウム溶液を容易に効率良く回収することができる偏光板製造廃液の処理方法の提供を目的とする。 Then, this invention aims at provision of the processing method of the polarizing plate manufacturing waste liquid which can collect | recover potassium iodide solution easily from a polarizing plate manufacturing waste liquid efficiently.
本発明の前記目的は、偏光板製造廃液からヨウ化カリウム溶液を回収する偏光板製造廃液の処理方法であって、偏光板製造廃液のpHを3.5〜8.0に維持しながら蒸発濃縮し、ホウ酸およびポリビニルアルコールを含む析出物を生成する濃縮工程と、偏光板製造廃液から前記析出物を固液分離したろ液を回収する固液分離工程とを備える偏光板製造廃液の処理方法により達成される。 The object of the present invention is a method of treating a polarizing plate manufacturing waste liquid for recovering a potassium iodide solution from the polarizing plate manufacturing waste liquid, and evaporating and concentrating while maintaining the pH of the polarizing plate manufacturing waste liquid at 3.5 to 8.0. And a method for treating a polarizing plate manufacturing waste liquid comprising: a concentration step for producing a precipitate containing boric acid and polyvinyl alcohol; and a solid-liquid separation step for recovering a filtrate obtained by solid-liquid separation of the precipitate from the polarizing plate manufacturing waste liquid. Is achieved.
この偏光板製造廃液の処理方法は、前記濃縮工程と前記固液分離工程との間に、蒸発濃縮後の偏光板製造廃液を冷却晶析する冷却晶析工程を備えることが好ましい。 It is preferable that the processing method of this polarizing plate manufacturing waste liquid is equipped with the cooling crystallization process which cools and crystallizes the polarizing plate manufacturing waste liquid after evaporation concentration between the said concentration process and the said solid-liquid separation process.
また、前記濃縮工程で生成された蒸気をヨウ素ガスの回収後に凝縮させる凝縮工程を更に備えることが好ましい。 Moreover, it is preferable to further comprise a condensing step for condensing the vapor generated in the concentrating step after recovering iodine gas.
本発明によれば、偏光板製造廃液からヨウ化カリウム溶液を容易に効率良く回収することができる偏光板製造廃液の処理方法を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the processing method of the polarizing plate manufacturing waste liquid which can collect | recover potassium iodide solution from a polarizing plate manufacturing waste liquid easily and efficiently can be provided.
以下、本発明の一実施形態について添付図面を参照して説明する。図1は、本発明の一実施形態に係る偏光板製造廃液の処理方法の概略工程図である。図1に示すように、偏光板製造廃液の処理方法は、まず偏光板製造廃液を濃縮工程1において蒸発濃縮する。 Hereinafter, an embodiment of the present invention will be described with reference to the accompanying drawings. FIG. 1 is a schematic process diagram of a polarizing plate production waste liquid treatment method according to an embodiment of the present invention. As shown in FIG. 1, in the method for treating a polarizing plate production waste liquid, first, the polarizing plate production waste liquid is evaporated and concentrated in a concentration step 1.
偏光板製造廃液は、液晶ディスプレイ等に使用される偏光板の製造工程で生じる廃液である。偏光板の製造工程においては、一般に、ポリビニルアルコール(PVA)からなるフィルムをヨウ化カリウム(KI)溶液に浸漬させた後、ホウ酸(H3BO3)水溶液中で延伸させ、水洗および乾燥を経て偏光板が製造される。このため、偏光板製造廃液には、PVAが含まれており、更に、KIやH3BO3等が主にイオンの状態で含まれている。偏光板製造廃液のpHは、3.5〜8.0の範囲にあり、ホウ酸溶液を含むため通常は酸性であるが、中性付近の偏光板製造廃液であってもよい。 The polarizing plate production waste liquid is a waste liquid produced in the production process of a polarizing plate used for a liquid crystal display or the like. In the manufacturing process of a polarizing plate, generally, after a film made of polyvinyl alcohol (PVA) is immersed in a potassium iodide (KI) solution, it is stretched in an aqueous solution of boric acid (H 3 BO 3 ), washed with water and dried. After that, a polarizing plate is manufactured. For this reason, the polarizing plate production waste liquid contains PVA, and further contains KI, H 3 BO 3 and the like mainly in an ionic state. The pH of the polarizing plate production waste liquid is in the range of 3.5 to 8.0 and is usually acidic because it contains a boric acid solution, but it may be a neutral polarizing plate production waste liquid.
濃縮工程1は、従来のように水酸化ナトリウム等のアルカリを添加することなく、酸性から中性を維持しながら蒸発濃縮することにより行われる。濃縮工程1における蒸発濃縮方法は特に限定されないが、例えば、蒸発缶に供給した偏光板製造廃液を、蒸発缶内に配置された伝熱管群の表面に散布して蒸発させる方法や、偏光板製造廃液を加熱した後にフラッシュ缶に導入してフラッシュ蒸発させる方法等を挙げることができる。 The concentration step 1 is performed by evaporating and concentrating while maintaining neutrality from acidity without adding an alkali such as sodium hydroxide as in the prior art. The evaporation concentration method in the concentration step 1 is not particularly limited. For example, the polarizing plate manufacturing waste liquid supplied to the evaporator can be sprayed on the surface of the heat transfer tube group arranged in the evaporator and evaporated. An example is a method in which the waste liquid is heated and then introduced into a flash can for flash evaporation.
偏光板製造廃液が酸性の状態で濃縮される場合、蒸発缶やフラッシュ缶の接液部や接ガス部には、耐食性の高い樹脂材料等を使用することが好ましい。 When the polarizing plate production waste liquid is concentrated in an acidic state, it is preferable to use a highly corrosion-resistant resin material or the like for the liquid contact part or gas contact part of the evaporator or flash can.
濃縮工程1で生成された蒸気は、凝縮工程2において凝縮されて凝縮水が生成される。凝縮工程2は、例えば、濃縮工程1で使用した蒸発缶やフラッシュ缶から蒸気配管を介して凝縮器に蒸気を導入し、冷却水で冷却することにより行われる。蒸気に含まれるヨウ素ガス(I2ガス)は、還元剤の添加により発生を抑制することも可能であるが、還元剤を添加することなくI2ガスを回収することが好ましい。すなわち、蒸発缶またはフラッシュ缶と凝縮器との間にスクラバーを設置し、蒸気に同伴されるヨウ素を、スクラバー内でKOH等のアルカリ溶液に吸収させて回収することができる。KOHスクラバーの内部は、pHが11〜13となるように制御することが好ましい。I2ガスを吸収除去した後の蒸気は、凝縮器において凝縮することができるが、一部または全部を、蒸気圧縮機により昇温して濃縮工程1の加熱源として利用することもできる。KOHスクラバーにおいてI2ガスとの反応により生成されたKIは、濃縮工程1において偏光板製造廃液と共に更に濃縮してもよい。
The vapor generated in the concentration step 1 is condensed in the
一方、濃縮工程1で廃液が濃縮されると、廃液に含まれているホウ酸が析出する。図2は、ヨウ化カリウム(KI)およびホウ酸(H3BO3)の相互溶解度を溶液に対する重量%で示す図である。濃縮工程1を行う前の偏光板製造廃液に含まれるKIおよびH3BO3の濃度がA点で表される場合に、濃縮工程1において偏光板製造廃液を70℃で蒸発濃縮すると、KIおよびH3BO3の濃度はB点に移動する。KIおよびH3BO3は、A点からB点まで移動する間、偏光板製造廃液中に溶解された状態が維持される。 On the other hand, when the waste liquid is concentrated in the concentration step 1, boric acid contained in the waste liquid is precipitated. FIG. 2 is a graph showing the mutual solubility of potassium iodide (KI) and boric acid (H 3 BO 3 ) in weight% with respect to the solution. When the concentration of KI and H 3 BO 3 contained in the polarizing plate manufacturing waste liquid before concentration step 1 is represented by point A, when the polarizing plate manufacturing waste liquid is evaporated and concentrated at 70 ° C. in concentration step 1, KI and The concentration of H 3 BO 3 moves to point B. While KI and H 3 BO 3 move from point A to point B, the state of being dissolved in the polarizing plate production waste liquid is maintained.
この後、70℃に維持しながら偏光板製造廃液を更に蒸発濃縮するとH3BO3の析出が開始され、H3BO3の結晶を発生しながら、偏光板製造廃液中のKIおよびH3BO3の濃度が、溶解度線に沿ってB点からC点まで移動する。C点における濃縮後の偏光板製造廃液は、KIが高濃度(例えば20%以上)である一方、H3BO3は低濃度である。 Thereafter, when the polarizing plate manufacturing waste liquid is further evaporated and concentrated while maintaining at 70 ° C., precipitation of H 3 BO 3 starts, and crystals of H 3 BO 3 are generated, while KI and H 3 BO in the polarizing plate manufacturing waste liquid are generated. The concentration of 3 moves from point B to point C along the solubility line. The polarizing plate production waste liquid after concentration at point C has a high concentration (for example, 20% or more) of KI, while H 3 BO 3 has a low concentration.
また、偏光板製造廃液にはPVAが含まれていることから、上記のように偏光板製造廃液を高温で蒸発濃縮することにより、PVAが重合してコロイド状になる。一例として、濃縮工程1を行う前の偏光板製造廃液中にPVAが0.3重量%含まれている場合に、濃縮工程1を50℃以上で行うことにより、PVAの60%以上を分離可能にすることができる。 Moreover, since the polarizing plate production waste liquid contains PVA, the PVA is polymerized into a colloid by evaporating and concentrating the polarizing plate production waste liquid at a high temperature as described above. As an example, when 0.3% by weight of PVA is contained in the polarizing plate manufacturing waste liquid before performing concentration step 1, it is possible to separate 60% or more of PVA by performing concentration step 1 at 50 ° C. or higher. Can be.
こうして、濃縮工程1により濃縮された偏光板製造廃液は、この偏光板製造廃液に含まれていたホウ酸およびPVAの多くがスラッジとなる。このスラッジを含む偏光板製造廃液は、固液分離工程3において、KI溶液と析出物とに固液分離される。固液分離の方法は、特に限定されるものではないが、例えば、加圧ろ過(フィルタープレス)、真空ろ過、遠心ろ過などの各種ろ過や、デカンター型などの遠心分離など、公知の方法を使用することができる。
Thus, in the polarizing plate manufacturing waste liquid concentrated in the concentration step 1, most of boric acid and PVA contained in the polarizing plate manufacturing waste liquid becomes sludge. In the solid-
固液分離工程3により得られたKI溶液のろ液は、上記のように高濃度であることから偏光板の製造工程において再利用可能である。このろ液は、KIの純度を高めるために更に濃縮することにより、KI結晶を取得してもよい。一方、ホウ酸やPVA等の析出物は、適宜回収するか廃棄物処理される。
Since the filtrate of the KI solution obtained by the solid-
本実施形態の偏光板製造廃液の処理方法は、偏光板製造廃液に対してアルカリを添加することなく蒸発濃縮した後、ホウ酸やPVAなどの不純物の大部分を固液分離して除去することにより、偏光板の製造工程で再利用可能なレベルのKI溶液をオンサイトで容易に回収することができるので、偏光板の製造工程におけるKIの継ぎ足し量を削減することができる。 The processing method of the polarizing plate manufacturing waste liquid of this embodiment is to remove most of impurities such as boric acid and PVA by solid-liquid separation after evaporating and concentrating the polarizing plate manufacturing waste liquid without adding alkali. Thus, the KI solution at a level that can be reused in the manufacturing process of the polarizing plate can be easily collected on-site, so that the amount of KI added in the manufacturing process of the polarizing plate can be reduced.
以上、本発明の一実施形態について詳述したが、本発明の具体的な態様は上記実施形態に限定されない。例えば、図1に示す偏光板製造廃液の処理方法における濃縮工程1と固液分離工程3との間に、図3に示すように冷却晶析工程4を追加してもよい。冷却晶析工程4は、例えば、晶析槽の内部または外壁に沿って熱交換器を配置し、晶析槽に供給した偏光板製造廃液を撹拌翼により撹拌しながら冷却する装置を用いて行うことができる。熱交換器に供給する冷媒としては、冷却塔により冷却された冷却水を用いることが好ましいが、工業用水や海水等を冷媒として使用してもよい。冷却晶析工程4においては、偏光板製造廃液を、45℃以下、好ましくは40〜45℃、さらに好ましくは常温(具体例としては30℃以下)まで冷却することが好ましい。
As mentioned above, although one Embodiment of this invention was explained in full detail, the specific aspect of this invention is not limited to the said embodiment. For example, a cooling crystallization step 4 may be added as shown in FIG. 3 between the concentration step 1 and the solid-
この偏光板製造廃液の処理方法によれば、図1に示す偏光板製造廃液の処理方法と同様に、濃縮工程1によりホウ酸およびPVAをKI溶液から分離可能なスラッジにした後、冷却晶析工程4によりホウ酸を更に晶析することで、より純度の高いKI溶液を得ることができる。すなわち、図4に示すKIおよびH3BO3の相互溶解度を示す図において、濃縮工程1によりA点からB点を経てC点まで移動したKIおよびH3BO3の濃度が、冷却晶析工程4によりD点まで移動するため、濃縮後の偏光板製造廃液に含まれるH3BO3の濃度が更に低減される。 According to this polarizing plate manufacturing waste liquid treatment method, as with the polarizing plate manufacturing waste liquid processing method shown in FIG. By further crystallizing boric acid in step 4, a more pure KI solution can be obtained. That is, in the diagram showing the mutual solubility of KI and H 3 BO 3 shown in FIG. 4, the concentrations of KI and H 3 BO 3 that have moved from point A through point B to point C in concentration step 1 are the cooling crystallization step. 4 moves to point D, so that the concentration of H 3 BO 3 contained in the concentrated polarizing plate manufacturing waste liquid is further reduced.
1 濃縮工程
2 凝縮工程
3 固液分離工程
4 冷却晶析工程
DESCRIPTION OF SYMBOLS 1
Claims (3)
偏光板製造廃液のpHを3.5〜8.0に維持しながら蒸発濃縮し、ホウ酸およびポリビニルアルコールを含む析出物を生成する濃縮工程と、
偏光板製造廃液から前記析出物を固液分離したろ液を回収する固液分離工程とを備える偏光板製造廃液の処理方法。 A method for treating a polarizing plate manufacturing waste liquid for recovering a potassium iodide solution from a polarizing plate manufacturing waste liquid,
A concentration step of evaporating and concentrating while maintaining the pH of the polarizing plate production waste liquid at 3.5 to 8.0 to produce a precipitate containing boric acid and polyvinyl alcohol;
A method for treating a polarizing plate production waste liquid, comprising: a solid-liquid separation step of recovering a filtrate obtained by solid-liquid separation of the precipitate from the polarizing plate production waste liquid.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2016103022A JP6841481B2 (en) | 2016-05-24 | 2016-05-24 | Method for treating polarizing plate manufacturing waste liquid |
TW106109972A TWI750158B (en) | 2016-05-24 | 2017-03-24 | Treating method for polarizer manufacturing waste liquid |
KR1020170057953A KR102354481B1 (en) | 2016-05-24 | 2017-05-10 | Treating method for polarizer manufacturing waste liquid |
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Cited By (5)
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JP2019066835A (en) * | 2017-10-02 | 2019-04-25 | 住友化学株式会社 | Method of manufacturing polarizing film and manufacturing apparatus of polarizing film |
JP2019066681A (en) * | 2017-10-02 | 2019-04-25 | 住友化学株式会社 | Method of manufacturing polarizing film |
KR20190138737A (en) | 2018-06-06 | 2019-12-16 | 가부시키가이샤 사사꾸라 | Treating method and treating device for polarizer manufacturing waste liquid |
JP2021154214A (en) * | 2020-03-27 | 2021-10-07 | 日東電工株式会社 | Treatment method of polarizing plate production waste liquid |
CN116492999A (en) * | 2022-11-25 | 2023-07-28 | 住华科技股份有限公司 | Process waste treatment and recycling system, process waste treatment and recycling method, and method for manufacturing optical film material |
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CN107416866A (en) | 2017-12-01 |
KR102354481B1 (en) | 2022-01-20 |
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TW201741248A (en) | 2017-12-01 |
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