JP5699073B2 - Cleaning device - Google Patents

Cleaning device Download PDF

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JP5699073B2
JP5699073B2 JP2011287129A JP2011287129A JP5699073B2 JP 5699073 B2 JP5699073 B2 JP 5699073B2 JP 2011287129 A JP2011287129 A JP 2011287129A JP 2011287129 A JP2011287129 A JP 2011287129A JP 5699073 B2 JP5699073 B2 JP 5699073B2
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dye
cleaning
unit
removing means
foreign matter
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JP2013137869A (en
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圭介 中
圭介 中
臼井　弘紀
弘紀 臼井
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Fujikura 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
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    • Y02E10/542—Dye sensitized solar cells

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Description

本発明は、色素増感太陽電池に用いられる酸化物半導体を洗浄する装置に関する。より詳しくは、増感色素が吸着された酸化物半導体を洗浄した後の洗浄液を再生する再生部を備えた洗浄装置に関する。   The present invention relates to an apparatus for cleaning an oxide semiconductor used in a dye-sensitized solar cell. More specifically, the present invention relates to a cleaning apparatus including a regeneration unit that regenerates a cleaning liquid after cleaning an oxide semiconductor on which a sensitizing dye is adsorbed.

色素増感太陽電池モジュールの製造において、多孔質の酸化物半導体層が形成された基板を増感色素の溶液中に浸漬させた後、過剰に含浸された増感色素を洗浄する処理を行う。この洗浄処理で用いられる装置として、特許文献１のリンス装置が知られている。当該リンス装置は、増感色素を吸着させた酸化物半導体層にリンス液をミスト状に噴射することにより、過剰な増感色素を洗い流す装置である。   In the production of the dye-sensitized solar cell module, after the substrate on which the porous oxide semiconductor layer is formed is immersed in the sensitizing dye solution, a treatment for washing the excessively impregnated sensitizing dye is performed. As an apparatus used in this cleaning process, a rinsing apparatus of Patent Document 1 is known. The rinsing apparatus is an apparatus for washing away excess sensitizing dye by spraying a rinsing liquid in a mist form onto the oxide semiconductor layer on which the sensitizing dye is adsorbed.

特開２０１１−４８９３８号公報JP 2011-48938 A

酸化物半導体層から過剰な増感色素を洗い流すためには大量の洗浄液（リンス液）が必要となる。特許文献１の方法では、ミスト状の洗浄液を酸化物半導体層に吹き付けることにより、洗浄液中に酸化物半導体層を浸漬する場合よりも、洗浄液の使用量を減らすことができるとしている。しかしながら、洗浄処理を行うのに比例して使用済みの洗浄液（廃液）が生じてしまう問題がある。また、洗浄処理に比例して発生する大量の廃液を貯留するタンク（廃液タンク）のサイズが大きくなり、該廃液タンクを備えた洗浄装置が大型化してしまう問題がある。さらに、貯留した廃液を別途処理するために、装置外へ大量の廃液を搬送する手間も必要となる。   In order to wash away excess sensitizing dye from the oxide semiconductor layer, a large amount of cleaning liquid (rinsing liquid) is required. According to the method of Patent Document 1, the amount of the cleaning liquid used can be reduced by spraying a mist-like cleaning liquid on the oxide semiconductor layer, compared with the case where the oxide semiconductor layer is immersed in the cleaning liquid. However, there is a problem that a used cleaning liquid (waste liquid) is generated in proportion to the cleaning process. In addition, there is a problem that the size of a tank (waste liquid tank) for storing a large amount of waste liquid generated in proportion to the cleaning process is increased, and the cleaning apparatus including the waste liquid tank is increased in size. Furthermore, in order to separately process the stored waste liquid, it is necessary to carry a large amount of waste liquid outside the apparatus.

本発明は、上記事情に鑑みてなされたものであり、廃液量を低減することができる洗浄装置の提供を課題とする。   This invention is made | formed in view of the said situation, and makes it a subject to provide the washing | cleaning apparatus which can reduce the amount of waste liquids.

本発明の請求項１に記載の洗浄装置は、色素増感太陽電池用の色素が吸着された酸化物半導体を洗浄液で洗うための洗浄部と、前記洗浄部で使用された洗浄液中の色素を除去する再生部と、前記洗浄部と前記再生部の間で前記洗浄液を循環させる循環部と、を備え、前記再生部が前記色素を吸着又はろ過する色素除去手段を有し、前記色素除去手段が、前記色素を吸着又はろ過する担体が配されたプレカラム及びメインカラムを有することを特徴とする。 The cleaning apparatus according to claim 1 of the present invention includes a cleaning unit for cleaning an oxide semiconductor adsorbed with a dye for a dye-sensitized solar cell with a cleaning liquid, and a dye in the cleaning liquid used in the cleaning unit. A regeneration unit that removes, and a circulation unit that circulates the cleaning liquid between the cleaning unit and the regeneration unit, and the regeneration unit includes a pigment removal unit that adsorbs or filters the pigment, and the pigment removal unit Has a pre-column and a main column on which a carrier for adsorbing or filtering the dye is arranged .

この構成によれば、洗浄部で使用した洗浄液（廃液）を循環部を介して再生部に戻し、再生部において廃液に含まれる色素を除去することにより当該廃液を洗浄液として再生し、循環部を介して再び洗浄部へ送ることができる。したがって、一度使用した洗浄液を再生して再利用できるので廃液量を大幅に削減することができる。
また、洗浄処理を行うことに比例して廃液が増加してしまうことが無く、大きな廃液タンクを装置内に備える必要が無くなるので、洗浄装置を小型化することができる。
また、洗浄装置内に一定量の洗浄液が循環された状態となるため、洗浄処理を行う度に装置外部から装置内部に大量の洗浄液を供給し続ける必要及び廃液タンクから廃液を搬出する必要が無くなるので、洗浄液及び廃液の搬送にかかるコストを削減できる。 According to this configuration, the cleaning liquid (waste liquid) used in the cleaning section is returned to the regeneration section through the circulation section, and the waste liquid is regenerated as the cleaning liquid by removing the pigment contained in the waste liquid in the regeneration section. Through the cleaning section. Therefore, since the cleaning liquid once used can be regenerated and reused, the amount of waste liquid can be greatly reduced.
Further, the waste liquid does not increase in proportion to the cleaning process, and it is not necessary to provide a large waste liquid tank in the apparatus, so that the cleaning apparatus can be reduced in size.
In addition, since a certain amount of cleaning liquid is circulated in the cleaning apparatus, it is not necessary to continuously supply a large amount of cleaning liquid from the outside of the apparatus to the inside of the apparatus and to carry out the waste liquid from the waste liquid tank every time cleaning is performed. Therefore, the cost for transporting the cleaning liquid and the waste liquid can be reduced.

本発明の請求項１に記載の洗浄装置は、前記再生部が前記色素を吸着又はろ過する色素除去手段を有する。
この構成によれば、色素を吸着又はろ過する色素除去手段以外の手段、例えば蒸留塔、を有する場合よりも容易に低コストで、廃液を再生することができる。また、色素除去手段を回収した場合、色素を再利用することができる。 Cleaning apparatus according to claim 1 of the present invention has a depigmenting means of the reconstruction unit is adsorbed or filtering the dye.
According to this configuration, the waste liquid can be regenerated easily and at a lower cost than the case of having a means other than the dye removing means for adsorbing or filtering the dye, for example, a distillation column. Further, when the dye removing means is collected, the dye can be reused.

本発明の請求項１に記載の洗浄装置は、前記色素除去手段が、前記色素を吸着又はろ過する担体が配されたプレカラム及びメインカラムを有する。
この構成によれば、プレカラムとメインカラムとに分けて多段階で色素を吸着又はろ過することにより、カラムの目詰まりを防止して、一段階のカラムだけを有する場合よりも色素除去効率を高めることができる。 Cleaning apparatus according to claim 1 of the present invention, the pigment removal means comprises a pre-column and the main column carrier was arranged for adsorbing or filtering the dye.
According to this configuration, the dye is adsorbed or filtered in multiple stages separately in the pre-column and the main column, thereby preventing the clogging of the column and increasing the dye removal efficiency as compared with the case of having only one stage of the column. be able to.

本発明の請求項２に記載の洗浄装置は、色素増感太陽電池用の色素が吸着された酸化物半導体を洗浄液で洗うための洗浄部と、前記洗浄部で使用された洗浄液中の色素を除去する再生部と、前記洗浄部と前記再生部の間で前記洗浄液を循環させる循環部と、を備え、前記再生部が前記色素を吸着又はろ過する色素除去手段を有し、前記再生部において、複数の前記色素除去手段が並列に接続されていることを特徴とする。
この構成によれば、メンテナンスのために停止した一方の色素除去手段の機能を、並列に接続された他方の色素除去手段で補完する（代替する）ことができるため、洗浄装置の運転を継続したままで、色素除去手段のメンテナンスを行うことができる。 The cleaning apparatus according to claim 2 of the present invention includes a cleaning unit for cleaning an oxide semiconductor adsorbed with a dye for a dye-sensitized solar cell with a cleaning liquid, and a dye in the cleaning liquid used in the cleaning unit. A regeneration unit that removes, and a circulation unit that circulates the cleaning liquid between the cleaning unit and the regeneration unit, and the regeneration unit includes a pigment removal unit that adsorbs or filters the pigment, and the regeneration unit includes: A plurality of the dye removing means are connected in parallel.
According to this configuration, since the function of one of the dye removing means stopped for maintenance can be supplemented (substitute) by the other dye removing means connected in parallel, the operation of the cleaning device is continued. The maintenance of the dye removing means can be performed as it is.

本発明の請求項３に記載の洗浄装置は、請求項１又は２において、前記再生部が前記色素に該当しない異物を除去する異物除去手段を有することを特徴とする。
この構成によれば、洗浄能力を低下させたり、酸化物半導体層に混入したりする異物を使用済みの洗浄液から除去できるので、再生する洗浄液の品質を向上させることができる。また、異物が系内を循環して何度も色素除去手段に入ることを防止することができ、色素除去手段の性能の低下や故障を防止することができる。 A cleaning apparatus according to a third aspect of the present invention is characterized in that, in the first or second aspect , the regeneration unit includes a foreign matter removing unit that removes foreign matter not corresponding to the pigment.
According to this configuration, the foreign matter that decreases the cleaning ability or is mixed into the oxide semiconductor layer can be removed from the used cleaning liquid, so that the quality of the cleaning liquid to be regenerated can be improved. Further, it is possible to prevent the foreign matter from circulating in the system and entering the dye removing unit many times, and it is possible to prevent the performance and failure of the dye removing unit from being deteriorated.

本発明の請求項４に記載の洗浄装置は、色素増感太陽電池用の色素が吸着された酸化物半導体を洗浄液で洗うための洗浄部と、前記洗浄部で使用された洗浄液中の色素を除去する再生部と、前記洗浄部と前記再生部の間で前記洗浄液を循環させる循環部と、を備え、前記再生部が前記色素に該当しない異物を除去する異物除去手段を有し、前記再生部において、複数の前記異物除去手段が並列に接続されていることを特徴とする。
この構成によれば、メンテナンスのために停止した一方の異物除去手段の機能を、並列に接続された他方の異物除去手段で補完する（代替する）ことができるため、洗浄装置の運転を継続したままで、異物除去手段のメンテナンスを行うことができる。
本発明の請求項５に記載の洗浄装置は、請求項４において、前記再生部が前記色素を吸着又はろ過する色素除去手段を有することを特徴とする。 The cleaning apparatus according to claim 4 of the present invention includes a cleaning unit for cleaning an oxide semiconductor adsorbed with a dye for a dye-sensitized solar cell with a cleaning solution, and a dye in the cleaning solution used in the cleaning unit. A regeneration unit that removes, and a circulation unit that circulates the cleaning liquid between the cleaning unit and the regeneration unit, and the regeneration unit includes a foreign matter removing unit that removes foreign matter that does not correspond to the pigment, and the regeneration The plurality of foreign matter removing means are connected in parallel in the section.
According to this configuration, the function of the one foreign matter removing means stopped for maintenance can be supplemented (substitute) by the other foreign matter removing means connected in parallel, so that the operation of the cleaning device is continued. The maintenance of the foreign matter removing means can be performed as it is.
The cleaning apparatus according to claim 5 of the present invention is characterized in that, in claim 4, the regeneration unit has a dye removing means for adsorbing or filtering the dye.

本発明の請求項６に記載の洗浄装置は、請求項３又は５において、前記再生部において、前記異物除去手段が、前記色素除去手段の上流側に接続されたことを特徴とする。
この構成によれば、使用済みの洗浄液に含まれる異物を異物除去手段で予め除去したうえで、当該使用済み洗浄液を色素除去手段へ供給することができる。この結果、異物が色素除去手段の機能を低下させることを防止できる。 The cleaning apparatus according to a sixth aspect of the present invention is the cleaning apparatus according to the third or fifth aspect , wherein the foreign matter removing means is connected to an upstream side of the dye removing means in the regeneration unit.
According to this configuration, the foreign matter contained in the used cleaning liquid can be removed in advance by the foreign matter removing means, and then the used cleaning liquid can be supplied to the dye removing means. As a result, it is possible to prevent foreign matters from deteriorating the function of the dye removing means.

本発明の請求項７に記載の洗浄装置は、請求項１〜３及び５〜６のいずれか一項において、前記色素除去手段が、ゼオライト、金属酸化物又は炭素材料を含むことを特徴とする。
この構成によれば、色素を吸着又はろ過する機能に優れた材料であるゼオライト、金属酸化物又は炭素材料を用いるため、使用済みの洗浄液を効率よく再生することができるので、洗浄処理を高効率で行うことができる。

The cleaning apparatus according to a seventh aspect of the present invention is the cleaning apparatus according to any one of the first to third and fifth to sixth aspects, wherein the dye removing unit includes zeolite, a metal oxide, or a carbon material. .
According to this configuration, since the zeolite, metal oxide, or carbon material, which is a material excellent in the function of adsorbing or filtering the dye, is used, the used cleaning liquid can be efficiently regenerated, so that the cleaning process is highly efficient. Can be done.

本発明の洗浄装置によれば、装置内で洗浄液を再生して再利用するので、廃液量を低減することができる。   According to the cleaning apparatus of the present invention, since the cleaning liquid is regenerated and reused in the apparatus, the amount of waste liquid can be reduced.

本発明の第一実施形態の模式図である。It is a schematic diagram of 1st embodiment of this invention. 本発明の第二実施形態の模式図である。It is a schematic diagram of 2nd embodiment of this invention. 本発明の第三実施形態の模式図である。It is a schematic diagram of 3rd embodiment of this invention. 洗浄液の吸光度スペクトルが再生処理の前後で変化した様子を示す図である。It is a figure which shows a mode that the light absorbency spectrum of the washing | cleaning liquid changed before and after the reproduction | regeneration process. オーバーフロー方式による洗浄の一例を示す模式図である。It is a schematic diagram which shows an example of the washing | cleaning by an overflow system.

以下、図面を参照して本発明の実施形態を説明するが、本発明はかかる実施形態に限定されない。
＜第一実施形態＞
図１に示すように、第一実施形態の洗浄装置１は、増感色素が吸着された多孔質の酸化物半導体層２を備えた基板を洗浄液３で洗うための洗浄部４と、洗浄部４で使用された洗浄液３中の色素を除去する再生部５と、洗浄部４と再生部５の間で洗浄液３を循環させる循環部６と、を備える。 Hereinafter, although an embodiment of the present invention is described with reference to drawings, the present invention is not limited to such an embodiment.
<First embodiment>
As shown in FIG. 1, the cleaning apparatus 1 of the first embodiment includes a cleaning unit 4 for cleaning a substrate having a porous oxide semiconductor layer 2 on which a sensitizing dye is adsorbed, with a cleaning liquid 3, and a cleaning unit. 4 includes a regeneration unit 5 that removes the pigment in the cleaning liquid 3 used in 4, and a circulation unit 6 that circulates the cleaning liquid 3 between the cleaning unit 4 and the regeneration unit 5.

洗浄部４に搬入される酸化物半導体層２を備えた基板は、公知の色素増感太陽電池の製造に使用されるものであり、増感色素の吸着処理が行われた後のものである。色素の吸着処理では、吸着効率を高めるために高濃度の色素溶液に酸化物半導体層２を浸漬させる処理が通常行われる。酸化物半導体層２には色素が過剰に吸着するため、これを洗い落とす洗浄処理を洗浄装置１において行う。
本実施形態では洗浄部４が洗浄槽４である場合を説明するが、本発明はこれに限定されず、例えば特許文献１に記載されているように、洗浄部４を洗浄室として、該洗浄室において前記基板にミスト状の洗浄液３を噴射して、排液口から回収した使用済みの洗浄液３を再生部５へ戻す方式を採用しても構わない。 The board | substrate provided with the oxide semiconductor layer 2 carried in to the washing | cleaning part 4 is used for manufacture of a well-known dye-sensitized solar cell, and is a thing after the adsorption process of a sensitizing dye was performed. . In the dye adsorption treatment, a treatment of immersing the oxide semiconductor layer 2 in a high concentration dye solution is usually performed in order to increase adsorption efficiency. Since the dye is excessively adsorbed on the oxide semiconductor layer 2, the cleaning apparatus 1 performs a cleaning process to wash it off.
In this embodiment, the case where the cleaning unit 4 is the cleaning tank 4 will be described. However, the present invention is not limited to this, and for example, as described in Patent Document 1, the cleaning unit 4 is used as a cleaning chamber and the cleaning unit 4 is used. A system may be employed in which the mist-like cleaning liquid 3 is sprayed onto the substrate in the chamber, and the used cleaning liquid 3 recovered from the drainage port is returned to the regeneration unit 5.

洗浄液３は、過剰に吸着した色素を酸化物半導体層２から洗い落とすことができるものであれば特に制限されない。例えば１−プロパノール等のアルコールが使用できる。
洗浄部４が洗浄槽４である場合、洗浄槽４の形状および大きさは、搬入した前記基板を洗浄液３に浸漬できるものであれば特に制限されない。洗浄槽４を構成する材料は特に制限されず、洗浄液３に溶出しない材料であることが好ましく、例えば、チタン等の金属材料、チタンフッ素樹脂やポリプロピレン等の樹脂材料が挙げられる。金属材料で洗浄槽４を構成する場合は、金属材料の腐食や溶出を防止するために、洗浄液３に接する部分に樹脂コーティングを施すことが好ましい。 The cleaning liquid 3 is not particularly limited as long as it can wash off the excessively adsorbed dye from the oxide semiconductor layer 2. For example, alcohol such as 1-propanol can be used.
When the cleaning unit 4 is the cleaning tank 4, the shape and size of the cleaning tank 4 are not particularly limited as long as the carried substrate can be immersed in the cleaning liquid 3. The material constituting the cleaning tank 4 is not particularly limited, and is preferably a material that does not elute into the cleaning liquid 3, and examples thereof include metal materials such as titanium and resin materials such as titanium fluororesin and polypropylene. When the cleaning tank 4 is made of a metal material, it is preferable to apply a resin coating to a portion in contact with the cleaning liquid 3 in order to prevent corrosion or elution of the metal material.

再生部５は、異物除去手段７および色素除去手段８を有する。異物除去手段７と色素除去手段８とはバルブを設けた配管で接続されている。
再生部５における異物除去手段７の数および色素除去手段８の数は特に制限されない。図１に示すように、１ずつ配置しても良いし、後述する第二実施形態（図２）及び第三実施形態（図３）に示すように、各々複数を配置しても良い。 The reproducing unit 5 includes foreign matter removing means 7 and pigment removing means 8. The foreign matter removing means 7 and the pigment removing means 8 are connected by a pipe provided with a valve.
The number of foreign matter removing means 7 and the number of dye removing means 8 in the reproducing unit 5 are not particularly limited. As shown in FIG. 1, one may be arranged, or a plurality may be arranged as shown in a second embodiment (FIG. 2) and a third embodiment (FIG. 3) described later.

異物除去手段７は、使用済みの洗浄液３に含まれている可能性がある、色素以外の異物を除去するものである。異物除去手段７としては、洗浄液３に耐性を有する樹脂製フィルターが好ましく、例えばフッ素樹脂又はポリプロピレン製のフィルターが挙げられる。フィルターの目開き及び開孔率は、想定される異物の大きさに応じて適宜調整される。異物除去手段７を洗浄装置１に備えることによって、洗浄能力を低下させたり、酸化物半導体層２に混入したりする異物を使用済みの洗浄液３から除去できるので、再生する洗浄液３の品質を向上させることができる。   The foreign matter removing means 7 removes foreign matter other than the dye that may be contained in the used cleaning liquid 3. The foreign matter removing means 7 is preferably a resin filter having resistance to the cleaning liquid 3, and examples thereof include a fluororesin or polypropylene filter. The opening and the aperture ratio of the filter are appropriately adjusted according to the assumed size of the foreign matter. By providing the foreign substance removing means 7 in the cleaning device 1, it is possible to remove foreign substances from the used cleaning liquid 3 that deteriorate the cleaning capability or enter the oxide semiconductor layer 2, thereby improving the quality of the cleaning liquid 3 to be regenerated. Can be made.

異物除去手段７は、図１に示すように、色素除去手段８の上流側に接続することが好ましい。使用済みの洗浄液３に含まれる異物を異物除去手段７で予め除去したうえで、当該使用済み洗浄液３を色素除去手段８へ供給することができる。この結果、異物が色素除去手段８の機能を低下させることを防止できる。   The foreign matter removing means 7 is preferably connected to the upstream side of the dye removing means 8 as shown in FIG. The foreign matter contained in the used cleaning liquid 3 can be removed in advance by the foreign matter removing means 7 and then the used cleaning liquid 3 can be supplied to the dye removing means 8. As a result, it is possible to prevent foreign matters from deteriorating the function of the dye removing means 8.

色素除去手段８は、使用済みの洗浄液３に含まれる色素を除去できるものであれば特に制限されず、例えば、色素を吸着又はろ過する担体（フィルター）、或いは洗浄液３の溶媒を蒸留して色素から分留する蒸留器（蒸留塔）等が挙げられる。装置構成を簡単にすることができると共に、容易に低コストで使用済みの洗浄液を再生できることから、再生部５は色素を吸着又はろ過する色素除去手段８を有することが好ましい。   The dye removing means 8 is not particularly limited as long as it can remove the dye contained in the used cleaning liquid 3. For example, the dye removing means 8 is a dye that absorbs or filters a dye (filter) or the solvent of the cleaning liquid 3 to distill the dye. For example, a distiller (distillation tower) for fractional distillation. Since the apparatus configuration can be simplified and the used cleaning liquid can be easily regenerated at low cost, the regenerating unit 5 preferably has a dye removing means 8 for adsorbing or filtering the dye.

前記色素除去手段８は、色素の吸着又はろ過の効率が高い材料であるゼオライト、金属酸化物又は炭素材料を含むもの、例えば、これらの材料を含む担体（フィルター）であることが好ましい。
前記ゼオライトとしては、色素を吸着又はろ過できる公知のゼオライトが使用可能であり、例えばCa、Mg、Na、K、Alなどを含む珪酸塩、又はいわゆるモレキュラーシーブ等が挙げられる。
前記金属酸化物としては、色素を吸着又はろ過できる公知の金属酸化物が使用可能であり、例えば酸化チタン、酸化亜鉛等が挙げられる。
前記炭素材料としては、例えば活性炭、カーボンナノチューブ、フラーレン、アモルファスカーボン等が挙げられる。
これらの材料を含む色素除去手段８を用いると、使用済みの洗浄液３を効率よく再生することが可能であり、洗浄処理の効率を向上させることができる。
また、ゼオライト、金属酸化物又は炭素材料を含む色素除去手段８を用いると、使用後にアルコール等に浸すことによって、これらに吸着又はろ過した色素を、簡単に離脱させて、回収することができる。このため、使用後のゼオライト、金属酸化物又は炭素材料を回収すれば色素を再利用することもできる。
また、ゼオライト、金属酸化物又は炭素材料は、ハンドリングが容易であり、簡単に取替え作業をすることができる。 The dye removing means 8 is preferably a material containing zeolite, a metal oxide or a carbon material, which is a material with high efficiency of dye adsorption or filtration, for example, a carrier (filter) containing these materials.
As the zeolite, a known zeolite capable of adsorbing or filtering a dye can be used, and examples thereof include silicates containing Ca, Mg, Na, K, Al, etc., or so-called molecular sieves.
As said metal oxide, the well-known metal oxide which can adsorb | suck or filter a pigment | dye can be used, For example, a titanium oxide, a zinc oxide, etc. are mentioned.
Examples of the carbon material include activated carbon, carbon nanotube, fullerene, and amorphous carbon.
When the pigment removing means 8 containing these materials is used, the used cleaning liquid 3 can be efficiently regenerated, and the efficiency of the cleaning process can be improved.
In addition, when the dye removing means 8 containing zeolite, metal oxide, or carbon material is used, the dye adsorbed or filtered by these can be easily separated and recovered by being immersed in alcohol or the like after use. For this reason, if the zeolite, metal oxide, or carbon material after use is collect | recovered, a pigment | dye can also be reused.
In addition, the zeolite, metal oxide, or carbon material is easy to handle and can be easily replaced.

ここで実施例として、図４に、ゼオライトによる色素吸着を行った洗浄液の吸光度スペクトルを示す。色素としてブラックダイ（Ｎ７４９）が溶解された１−プロパノールを、使用済みの洗浄液３とした。これをゼオライト（ユニオン昭和株式会社製；製品名ＩＧＭＩＮＩ）２０ｇに接触させて、色素の吸着処理を行った。吸着処理前のスペクトルにおいて観測されていた、ブラックダイの特徴である４００ｎｍ付近のピーク及び６２０ｎｍ付近のピークが、吸着処理後には観測されなくなったことから、ゼオライトに色素が吸着することにより、洗浄液３を再生できたことが明らかである。吸着処理後のスペクトルは、溶媒だけのスペクトルと同等であることから、吸着処理によりほぼ完全に色素を除去することができる。よって、再生処理を繰り返すことにより、除去しきれない成分や色素が残留するようになるまで、洗浄液３を繰り返し再生して使用し続けることができる。   Here, as an example, FIG. 4 shows an absorbance spectrum of a cleaning solution that has been subjected to dye adsorption by zeolite. 1-propanol in which black dye (N749) was dissolved as a dye was used as the used cleaning liquid 3. This was brought into contact with 20 g of zeolite (manufactured by Union Showa Co., Ltd .; product name IGMINI) to carry out a dye adsorption treatment. Since the peak near 400 nm and the peak near 620 nm, which are the characteristics of the black die, observed in the spectrum before the adsorption treatment are not observed after the adsorption treatment, the dye is adsorbed on the zeolite, so that the washing liquid 3 It is clear that I was able to play. Since the spectrum after the adsorption treatment is equivalent to the spectrum of the solvent alone, the dye can be almost completely removed by the adsorption treatment. Therefore, by repeating the regeneration process, the cleaning liquid 3 can be repeatedly regenerated and used until components or pigments that cannot be removed remain.

色素除去手段８は、前記色素を吸着又はろ過する担体（フィルター）が配されたプレカラム及びメインカラムを有することが好ましい。この構成を採用した場合、プレカラムをいわゆるガードカラムとして機能させることができる。つまり、プレカラムにおいて、凝集等により比較的大きくなった色素粒子を除去して、メインカラムにおいて、より微細な色素粒子又は色素分子を除去する、という多段階方式を採用できる。この多段階方式であると、プレカラム及びメインカラムの目詰まりを抑制することが可能となり、一段階のメインカラムだけを有する場合よりも色素除去効率を高めることができる。なお、この多段階方式の場合、カラムの目詰まりを抑制するために、プレカラムのフィルターの目開き及び開孔率は、メインカラムのフィルターの目開き及び開孔率よりも大きくすることが好ましい。   The dye removing means 8 preferably has a pre-column and a main column on which a carrier (filter) for adsorbing or filtering the dye is arranged. When this configuration is employed, the precolumn can function as a so-called guard column. That is, it is possible to employ a multi-stage method in which pigment particles that have become relatively large due to aggregation or the like are removed in the precolumn, and finer pigment particles or pigment molecules are removed in the main column. With this multi-stage system, it becomes possible to suppress clogging of the pre-column and the main column, and the dye removal efficiency can be increased as compared with the case where only the single-stage main column is provided. In the case of this multi-stage system, in order to suppress clogging of the column, it is preferable that the opening and the opening ratio of the filter of the pre-column be larger than the opening and the opening ratio of the filter of the main column.

循環部６は、洗浄部４と再生部５との間で洗浄液３を循環させる配管を有することが好ましい。図１に示す第一実施形態には、洗浄部４で使用された洗浄液３を再生部５に戻す配管６ａ（戻し配管６ａ）と、再生部５で再生された洗浄液３を洗浄部４に送る配管６ｂ（送り配管６ｂ）とが備えられている。戻し配管６ａの途中には貯留タンク９が設置されていても構わない。貯留タンク９を設置することで、洗浄部４に流す洗浄液３の量を簡単に調整することができる。また、色素除去手段８の除去性能に合わせて、色素除去手段８に流す洗浄液の量を調整することができる。また、循環部６において、洗浄液３を送液するための送液ポンプ１０が設けられていることが好ましい。送液ポンプ１０は、有機系の洗浄液３の使用を考慮して、空圧駆動式であることが好ましい。洗浄液３を循環させる配管には、適宜バルブを設置することが好ましい。また、送液ポンプ１０は、少なくとも色素除去手段８の上流側に設けられることが好ましい。こうすることで、色素除去手段８の除去性能に合わせて、色素除去手段８に流れる流速をコントロールすることができる。   The circulation unit 6 preferably has a pipe for circulating the cleaning liquid 3 between the cleaning unit 4 and the regeneration unit 5. In the first embodiment shown in FIG. 1, a pipe 6 a (return pipe 6 a) for returning the cleaning liquid 3 used in the cleaning section 4 to the regeneration section 5 and a cleaning liquid 3 regenerated by the regeneration section 5 are sent to the cleaning section 4. A pipe 6b (feed pipe 6b) is provided. A storage tank 9 may be installed in the middle of the return pipe 6a. By installing the storage tank 9, it is possible to easily adjust the amount of the cleaning liquid 3 that flows to the cleaning unit 4. Further, the amount of the cleaning liquid that flows to the dye removing unit 8 can be adjusted according to the removal performance of the dye removing unit 8. Moreover, it is preferable that the circulation part 6 is provided with a liquid feed pump 10 for feeding the cleaning liquid 3. The liquid feed pump 10 is preferably a pneumatic drive type in consideration of the use of the organic cleaning liquid 3. It is preferable to appropriately install a valve in the pipe for circulating the cleaning liquid 3. Further, the liquid feed pump 10 is preferably provided at least upstream of the dye removing means 8. By doing so, it is possible to control the flow rate flowing through the dye removing means 8 in accordance with the removal performance of the dye removing means 8.

洗浄部４が洗浄槽４である場合、洗浄槽４における洗浄液３の流通方式は、オーバーフロー方式であることが好ましい。これを図５を参照して説明する。オーバーフロー方式は、洗浄する酸化物半導体層２を備えた基板を搬入した洗浄槽４の下部の流入口４ａから洗浄液３を流入させ、洗浄槽４の上方へ向けて洗浄液３を流通させる過程で酸化物半導体層２を洗浄し、洗浄槽４の上部の排出口４ｂから洗浄液３を溢れさせて排出する方式である。排出口４ｂの位置を、基板の上端よりも上方に設けることにより、基板の下端から上端まで余すことなく洗浄することができる。オーバーフロー方式であると、洗浄液３を流入させ続ける限り、洗浄槽４における洗浄液３の液面は排出口４ｂの高さで一定となるので、液面の高さの管理が容易となる。
また、排出口４ｂを設けずに、洗浄槽４の上端の縁全体から洗浄液３を溢れさせるように行っても良い。洗浄槽４内における洗浄液３の流れが偏らず、より均等に流れるので洗浄効率が向上する場合がある。溢れ出た洗浄液３は、洗浄槽４に隣接して設けられたオーバーフロー槽１１に回収して、戻し配管６ａへ流通させることができる（図１参照）。 When the cleaning unit 4 is the cleaning tank 4, the flow system of the cleaning liquid 3 in the cleaning tank 4 is preferably an overflow system. This will be described with reference to FIG. In the overflow method, the cleaning liquid 3 is introduced from the inlet 4a at the lower part of the cleaning tank 4 carrying the substrate having the oxide semiconductor layer 2 to be cleaned, and the cleaning liquid 3 is circulated upward of the cleaning tank 4 in the process. In this method, the physical semiconductor layer 2 is washed and the washing liquid 3 overflows from the discharge port 4b at the top of the washing tank 4 and is discharged. By providing the position of the discharge port 4b above the upper end of the substrate, cleaning can be performed without leaving the lower end to the upper end of the substrate. In the overflow method, as long as the cleaning liquid 3 continues to flow, the liquid level of the cleaning liquid 3 in the cleaning tank 4 is constant at the height of the discharge port 4b, so that the liquid level can be easily managed.
Moreover, you may carry out so that the washing | cleaning liquid 3 may overflow from the whole edge of the upper end of the washing tank 4, without providing the discharge port 4b. Since the flow of the cleaning liquid 3 in the cleaning tank 4 is not biased and flows more evenly, the cleaning efficiency may be improved. The overflowing cleaning liquid 3 can be collected in an overflow tank 11 provided adjacent to the cleaning tank 4 and circulated through the return pipe 6a (see FIG. 1).

＜第二実施形態＞
図２に示す第二実施形態の洗浄装置２１では、再生部５において、複数の異物除去手段７（第一の異物除去手段７ａ、第二の異物除去手段７ｂ）、および複数の色素除去手段８（第一の色素除去手段８ａ、第二の色素除去手段８ｂ）が備えられている。他の構成については、前述の第一実施形態の洗浄装置１と同じであるので、同じ符号を付して、その説明を省略する。 <Second embodiment>
In the cleaning device 21 of the second embodiment shown in FIG. 2, in the regeneration unit 5, a plurality of foreign matter removing means 7 (first foreign matter removing means 7 a, second foreign matter removing means 7 b) and a plurality of dye removing means 8. (First dye removing means 8a, second dye removing means 8b) are provided. Since other configurations are the same as those of the cleaning device 1 of the first embodiment described above, the same reference numerals are given and description thereof is omitted.

再生部５において、複数の異物除去手段７が並列に接続されているので、洗浄装置２１の運転を継続したままで、異物除去手段７のメンテナンスを行うことができる。例えば、第一の色素除去手段７ａをメンテナンスする場合、バルブ（三方弁）を制御して第二の色素除去手段７ｂのみに洗浄液３を流通させることによって、第一の異物除去手段７ａを循環経路から切り離すことができる。   Since the plurality of foreign matter removing means 7 are connected in parallel in the reproducing unit 5, the foreign matter removing means 7 can be maintained while the operation of the cleaning device 21 is continued. For example, when maintaining the first dye removing means 7a, the valve (three-way valve) is controlled so that the cleaning liquid 3 is circulated only through the second dye removing means 7b. Can be separated from.

再生部５において、複数の色素除去手段８が並列に接続されているので、洗浄装置２１の運転を継続したままで、色素除去手段８のメンテナンスを行うことができる。例えば、第一の色素除去手段８ａをメンテナンスする場合、バルブ（三方弁）を制御して第二の色素除去手段８ｂのみに洗浄液３を流通させることによって、第一の色素除去手段８ａを循環経路から切り離すことができる。   Since the plurality of dye removing means 8 are connected in parallel in the reproducing unit 5, the dye removing means 8 can be maintained while the operation of the cleaning device 21 is continued. For example, when maintaining the first dye removing means 8a, the valve (three-way valve) is controlled so that the cleaning liquid 3 is circulated only through the second dye removing means 8b, whereby the first dye removing means 8a is circulated. Can be separated from.

＜第三実施形態＞
図３に示す第三実施形態の洗浄装置３１では、再生部５において、異物除去手段７、第一の色素除去手段８ａ、第二の色素除去手段８ｂ、の順で直列に接続されている。他の構成については、前述の第一実施形態の洗浄装置１と同じであるので、同じ符号を付して、その説明を省略する。 <Third embodiment>
In the cleaning device 31 of the third embodiment shown in FIG. 3, the foreign matter removing means 7, the first dye removing means 8 a, and the second dye removing means 8 b are connected in series in the regeneration unit 5. Since other configurations are the same as those of the cleaning device 1 of the first embodiment described above, the same reference numerals are given and description thereof is omitted.

再生部５において、複数の色素除去手段８が直列に接続されているので、各色素除去手段８ａ，８ｂの使用可能期間を長くする（各色素除去手段を長寿命化する）ことができる。各色素除去手段８が前記フィルターである場合、第一のフィルター８ａの目開き及び開孔率は、第二のフィルター８ｂの目開き及び開孔率よりも大きくすることが好ましい。この構成にすると、各フィルターの目詰まりを防止して、各フィルターの使用可能期間をより一層長くすることができる。   In the reproducing unit 5, since the plurality of dye removing means 8 are connected in series, the usable period of each of the dye removing means 8a and 8b can be extended (the life of each dye removing means can be extended). When each pigment removing means 8 is the filter, it is preferable that the opening and the opening ratio of the first filter 8a are larger than the opening and the opening ratio of the second filter 8b. With this configuration, each filter can be prevented from being clogged, and the usable period of each filter can be further extended.

本発明は、上記実施形態には限定されない。
前述の第二実施形態では、色素除去手段８と異物除去手段７をそれぞれ個別に並列に接続している。この第二実施形態の変形例として、色素除去手段８と異物除去手段７を直列につないだ組を複数備え、これらの組同士を並列に接続した構成が挙げられる。具体例としては、図２に示す洗浄装置２１において、まず異物除去手段７と色素除去手段８の間にある２個のバルブを取り外し、次に異物除去手段７ａと色素除去手段８ａを直列に接続した組、及び異物除去手段７ｂと色素除去手段８ｂを直列に接続した組を準備し、続いてこれら２つの組を並列に接続した構成が挙げられる。この構成であると、第二実施形態よりもバルブの数を減らすことができる。また、並列に接続された２つの組のうち、どちらか一方の組で運転を継続したまま、他方の組を外して色素除去手段８と異物除去手段７を同時にメンテナンスすることができる。このように色素除去手段と異物除去手段の両方を同時にメンテナンスすることにより、当該運転期間中に除去した色素量と異物量の関係を簡単に測定することができる。 The present invention is not limited to the above embodiment.
In the second embodiment described above, the dye removing unit 8 and the foreign matter removing unit 7 are individually connected in parallel. As a modified example of the second embodiment, there is a configuration in which a plurality of sets in which the pigment removing unit 8 and the foreign matter removing unit 7 are connected in series are provided and these sets are connected in parallel. As a specific example, in the cleaning apparatus 21 shown in FIG. 2, first, two valves between the foreign matter removing means 7 and the dye removing means 8 are removed, and then the foreign matter removing means 7a and the dye removing means 8a are connected in series. And a set in which the foreign matter removing means 7b and the dye removing means 8b are connected in series, and then these two sets are connected in parallel. With this configuration, the number of valves can be reduced as compared with the second embodiment. In addition, while the operation is continued with one of the two sets connected in parallel, the other set can be removed and the pigment removing unit 8 and the foreign matter removing unit 7 can be maintained at the same time. Thus, by maintaining both the pigment removing unit and the foreign matter removing unit at the same time, the relationship between the amount of pigment removed during the operation period and the amount of foreign matter can be easily measured.

１，２１，３１…洗浄装置、２…酸化物半導体層（酸化物半導体層が形成された基板）、３…洗浄液（リンス液）、４…洗浄部、５…再生部、６…循環部、６ａ…戻し配管、６ｂ…送り配管、７…異物除去手段、８…色素除去手段、９…貯留タンク、１０…送液ポンプ、１１…オーバーフロー槽。 DESCRIPTION OF SYMBOLS 1, 21, 31 ... Cleaning apparatus, 2 ... Oxide semiconductor layer (substrate in which oxide semiconductor layer is formed), 3 ... Cleaning liquid (rinsing liquid), 4 ... Cleaning part, 5 ... Regeneration part, 6 ... Circulation part, 6a ... return pipe, 6b ... feed pipe, 7 ... foreign matter removing means, 8 ... dye removing means, 9 ... storage tank, 10 ... liquid feed pump, 11 ... overflow tank.

Claims (7)

色素増感太陽電池用の色素が吸着された酸化物半導体を洗浄液で洗うための洗浄部と、
前記洗浄部で使用された洗浄液中の色素を除去する再生部と、
前記洗浄部と前記再生部の間で前記洗浄液を循環させる循環部と、
を備え、前記再生部が前記色素を吸着又はろ過する色素除去手段を有し、
前記色素除去手段が、前記色素を吸着又はろ過する担体が配されたプレカラム及びメインカラムを有することを特徴とする洗浄装置。 A washing section for washing the oxide semiconductor adsorbed with the dye for a dye-sensitized solar cell with a washing liquid;
A regeneration unit for removing the dye in the cleaning liquid used in the cleaning unit;
A circulating unit for circulating the cleaning liquid between the cleaning unit and the regeneration unit;
Comprising a dye removing means for adsorbing or filtering the dye.
The washing apparatus , wherein the dye removing means has a pre-column and a main column on which a carrier for adsorbing or filtering the dye is arranged . 色素増感太陽電池用の色素が吸着された酸化物半導体を洗浄液で洗うための洗浄部と、
前記洗浄部で使用された洗浄液中の色素を除去する再生部と、
前記洗浄部と前記再生部の間で前記洗浄液を循環させる循環部と、
を備え、前記再生部が前記色素を吸着又はろ過する色素除去手段を有し、
前記再生部において、複数の前記色素除去手段が並列に接続されていることを特徴とする洗浄装置。 A washing section for washing the oxide semiconductor adsorbed with the dye for a dye-sensitized solar cell with a washing liquid;
A regeneration unit for removing the dye in the cleaning liquid used in the cleaning unit;
A circulating unit for circulating the cleaning liquid between the cleaning unit and the regeneration unit;
Comprising a dye removing means for adsorbing or filtering the dye.
A cleaning apparatus , wherein a plurality of the pigment removing means are connected in parallel in the regeneration unit . 前記再生部が前記色素に該当しない異物を除去する異物除去手段を有することを特徴とする請求項１又は２に記載の洗浄装置。 Cleaning apparatus according to claim 1 or 2, characterized in that it has a foreign substance removing means for removing foreign matter the playback unit does not correspond to the dye. 色素増感太陽電池用の色素が吸着された酸化物半導体を洗浄液で洗うための洗浄部と、
前記洗浄部で使用された洗浄液中の色素を除去する再生部と、
前記洗浄部と前記再生部の間で前記洗浄液を循環させる循環部と、
を備え、前記再生部が前記色素に該当しない異物を除去する異物除去手段を有し、
前記再生部において、複数の前記異物除去手段が並列に接続されていることを特徴とする洗浄装置。 A washing section for washing the oxide semiconductor adsorbed with the dye for a dye-sensitized solar cell with a washing liquid;
A regeneration unit for removing the dye in the cleaning liquid used in the cleaning unit;
A circulating unit for circulating the cleaning liquid between the cleaning unit and the regeneration unit;
A foreign matter removing means for removing the foreign matter that does not correspond to the pigment,
The cleaning apparatus , wherein the regeneration unit includes a plurality of the foreign matter removing means connected in parallel . 前記再生部が前記色素を吸着又はろ過する色素除去手段を有することを特徴とする請求項４に記載の洗浄装置。The cleaning apparatus according to claim 4, wherein the regeneration unit includes a dye removing unit that adsorbs or filters the dye. 前記再生部において、前記異物除去手段が、前記色素除去手段の上流側に接続されたことを特徴とする請求項３又は５に記載の洗浄装置。 The cleaning apparatus according to claim 3 or 5 , wherein, in the regeneration unit, the foreign matter removing unit is connected to an upstream side of the dye removing unit. 前記色素除去手段が、ゼオライト、金属酸化物又は炭素材料を含むことを特徴とする請求項１〜３及び５〜６のいずれか一項に記載の洗浄装置。 Said pigment removal means, zeolites, cleaning apparatus according to any one of claims 1-3 and 5-6 characterized in that it comprises a metal oxide or carbon material.
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