JP2016180592A - Method of determining absorption state of organic substances absorbed by resin particles, and method of managing water treatment system - Google Patents
Method of determining absorption state of organic substances absorbed by resin particles, and method of managing water treatment system Download PDFInfo
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本発明は、樹脂粒子に吸着した有機物の吸着状態判定方法に関する。また、本発明は、純水製造システムなどの水処理システムに使用されるイオン交換樹脂の汚染物質、特に処理水中に微量含まれる有機物汚染によるイオン交換樹脂の劣化状況を把握し、管理する方法に関する。 The present invention relates to an organic substance adsorption state determination method adsorbed on resin particles. The present invention also relates to a method for grasping and managing the deterioration state of ion exchange resin pollutants used in water treatment systems such as a pure water production system, in particular, ion exchange resin deterioration due to organic matter contamination contained in trace amounts in treated water. .
純水装置で使用するイオン交換樹脂が、処理原水中に含まれる有機物によって汚染され、薬品再生後の再生薬品の残留により採水開始までの時間が延長する事例がある。これまで有機物の構造に含まれるカルボン酸基に再生薬品のナトリウムが結合し、再生薬品の残留が高くなると考えられてきたが、原水に含まれる有機物は、フルボ酸やフミン酸といった土壌分解性の有機物であり、イオン交換樹脂の母体も有機物であるためイオン交換樹脂を直接分析し、有機物の特定や濃度を測定することは難しい。 There is a case where the ion exchange resin used in the pure water apparatus is contaminated by organic substances contained in the treated raw water, and the time until the start of water sampling is extended due to the residual of the regenerated chemical after chemical regeneration. So far, it has been thought that regenerative chemical sodium binds to the carboxylic acid group contained in the structure of organic matter, and the residual of the regenerative chemical becomes high. Since it is an organic substance and the base of the ion exchange resin is also an organic substance, it is difficult to directly analyze the ion exchange resin and to determine the concentration and the concentration of the organic substance.
構造がある程度予測される有機物の吸着に関しては、特許文献１には表面分析法により試料の表面部分に吸着した物質の試料深さ方向の分布を測定することを特徴とする試料表面に吸着した物質の吸着状態判定方法が開示され、表面分析法として電子線プローブマイクロアナライザー法、二次イオン質量分析法、光電子分光法、光音響分光法、赤外全反射分光法（ＡＴＲ法）、ラマン分光法が挙げられおり、特にＡＴＲ法を使用した判定方法が開示されている。 Regarding the adsorption of organic substances whose structure is predicted to some extent, Patent Document 1 discloses a substance adsorbed on the sample surface characterized by measuring the distribution in the sample depth direction of the substance adsorbed on the surface part of the sample by a surface analysis method. The method for determining the adsorption state of an electron beam is disclosed, and as a surface analysis method, an electron beam probe microanalyzer method, secondary ion mass spectrometry, photoelectron spectroscopy, photoacoustic spectroscopy, infrared total reflection spectroscopy (ATR method), Raman spectroscopy In particular, a determination method using the ATR method is disclosed.
しかしながら、特許文献１の方法は、原水中に含まれる有機物ではなく、多段に組み合わせた他のイオン交換樹脂からの溶出物に対して効果を奏するものである。そのため、フルボ酸やフミン酸といった土壌分解性の有機物、特にこれら酸性の無定形高分子有機物については十分な方法とはいえなかった。 However, the method of Patent Document 1 is effective not for organic substances contained in raw water but for eluates from other ion exchange resins combined in multiple stages. For this reason, it has not been a sufficient method for soil-decomposable organic substances such as fulvic acid and humic acid, especially these acidic amorphous polymer organic substances.
原水中に含まれる有機物濃度は、ＴＯＣとしては数十μｇ／ｌと低いが、処理の過程で徐々にイオン交換樹脂に有機物が蓄積されると考えられるため、安定した運転管理を行うには、イオン交換樹脂の有機物吸着状況を把握することは重要である。 The concentration of organic substances contained in the raw water is as low as several tens of μg / l as TOC, but it is considered that organic substances are gradually accumulated in the ion exchange resin during the treatment process. It is important to understand the organic matter adsorption status of ion exchange resins.
本発明では、有機物によるイオン交換樹脂の吸着状況を判定する方法及びそれに処理原水中に微量含まれる酸性の無定形高分子有機物汚染の状況をこの吸着状態の判定方法に基づいて把握し、イオン交換樹脂の交換時期を管理する水処理システムの管理方法を提供することを目的とする。 In the present invention, the method for determining the adsorption status of the ion exchange resin by the organic matter and the acidic amorphous polymer organic matter contamination status contained in a trace amount in the treated raw water are grasped based on this adsorption status determination method, and ion exchange is performed. It aims at providing the management method of the water treatment system which manages the exchange time of resin.
本発明者が鋭意検討した結果、イオン交換樹脂の性能低下を引き起こす酸性の無定形高分子有機物と同等の性能低下挙動を示す構造既知の有機物を見出し、その有機物を用いて、有機物の吸着状態を蛍光光度法にて評価する方法に到達したものである。 As a result of diligent study by the present inventor, the present inventors have found an organic substance having a known structure exhibiting a performance deterioration behavior equivalent to that of an acidic amorphous polymer organic substance that causes a decrease in the performance of the ion exchange resin, and the organic substance is used to determine the adsorption state of the organic substance. It has reached the method of evaluation by the fluorescence photometry.
すなわち、本発明の一形態によれば、樹脂粒子への有機物の吸着状態を判定する方法であって、有機物を吸着した樹脂粒子を粉砕して、粉砕した前記樹脂粒子に対して蛍光光度法により励起波長を走査して少なくとも２つの励起波長における蛍光ピークの強度を取得し、２つの前記蛍光ピークの強度の比に基づいて前記有機物の吸着量を予測する吸着状態判定方法が提供される。 That is, according to one aspect of the present invention, a method for determining an adsorption state of an organic substance on a resin particle, the resin particle adsorbing an organic substance is pulverized, and the pulverized resin particle is obtained by a fluorometric method. An adsorption state determination method is provided that scans excitation wavelengths to acquire fluorescence peak intensities at at least two excitation wavelengths, and predicts an adsorption amount of the organic substance based on a ratio of the two fluorescence peak intensities.
又、本発明の別の形態によれば、水処理システムに使用されるイオン交換樹脂に吸着した外来有機物の吸着状態について上記吸着状態判定方法により、イオン交換樹脂への外来有機物の吸着量を予測し、該吸着量からイオン交換樹脂の交換時期を決定する水処理システムの管理方法が提供される。 According to another aspect of the present invention, the amount of foreign organic matter adsorbed on the ion exchange resin is predicted by the adsorption state determination method for the state of adsorption of the foreign organic matter adsorbed on the ion exchange resin used in the water treatment system. And the management method of the water treatment system which determines the replacement | exchange time of ion exchange resin from this adsorption amount is provided.
本発明よれば、特定の有機物のイオン交換樹脂への吸着状態より、再生薬品の残留性を把握できるようになり、安定した水処理系の管理ができ、適切な交換時期の判断や決定ができるようになる。 According to the present invention, it becomes possible to grasp the persistence of regenerated chemicals from the adsorption state of a specific organic substance on an ion exchange resin, and it is possible to manage a stable water treatment system and to judge and determine an appropriate replacement time. It becomes like this.
フルボ酸やフミン酸といった土壌分解性の有機物は不定形であるため、これを直接用いて、イオン交換樹脂への吸着状況を確認することは極めて困難である。そこで、本発明ではこのような酸性の無定形高分子有機物と同等の性能低下挙動を示す構造既知の有機物を用いて、その吸着状況を把握し、それを実際の原水処理などの水処理システムに使用したイオン交換樹脂にも適用できることを見出した。 Since soil-decomposable organic substances such as fulvic acid and humic acid are indefinite, it is extremely difficult to directly check the adsorption state on the ion exchange resin. Therefore, in the present invention, using an organic substance with a known structure that exhibits the same performance degradation behavior as that of the acidic amorphous polymer organic substance, the adsorption state is grasped, and this is applied to a water treatment system such as actual raw water treatment. It was found that the present invention can also be applied to the ion exchange resin used.
ここで、指標となる構造既知の有機物としては、カルボン酸基含有芳香族化合物、特にカルボン酸基とフェノール性水酸基をそれぞれ１つ以上有する化合物が同等の性能低下挙動を示すことを見出した。中でも下記構造式に示す没食子酸鉄を指標化合物として用いるものである。 Here, it has been found that as an organic substance having a known structure serving as an index, a carboxylic acid group-containing aromatic compound, particularly a compound having at least one carboxylic acid group and one or more phenolic hydroxyl groups, exhibits equivalent performance-decreasing behavior. Among them, iron gallate shown in the following structural formula is used as an indicator compound.
没食子酸鉄（ビス（３，４，５−トリヒドロキシ安息香酸）鉄（ＩＩ））は、万年筆などの黒色インク成分として古くから知られており、容易に入手することができる。 Iron gallate (bis (3,4,5-trihydroxybenzoate) iron (II)) has been known for a long time as a black ink component such as a fountain pen and can be easily obtained.
本発明が適用されるイオン交換樹脂としては、陰イオン交換樹脂であり、特に弱塩基性の陰イオン交換樹脂である。また、イオン交換樹脂のベース樹脂としては、ポリアクリル系とポリスチレン系とがあるが、本発明ではポリスチレン系の弱塩基性の陰イオン交換樹脂に対して特に有効である。 The ion exchange resin to which the present invention is applied is an anion exchange resin, particularly a weakly basic anion exchange resin. In addition, as the base resin of the ion exchange resin, there are a polyacrylic type and a polystyrene type. In the present invention, it is particularly effective for a polystyrene type weakly basic anion exchange resin.
（測定方法およびイオン交換樹脂性能評価方法）
イオン交換樹脂の有機物吸着量の測定法としては、蛍光光度法を用いる。蛍光光度法とは、測定試料に光を照射することで試料に含まれる物質が励起状態になり、基底状態に戻る際に発する蛍光を測定する方法である。測定するイオン交換樹脂や有機物により励起波長や蛍光波長が異なるため、３次元の蛍光スペクトルのデータが収集できる機器が好ましい。測定するイオン交換樹脂を乾燥後粉砕し、プレート上に成型する。その際に正確な定量を実施するため成型の型や成型するイオン交換樹脂量は一定にする必要がある。成型したイオン交換樹脂に対して励起波長を走査し、蛍光波長を求め、３次元の蛍光スペクトルデータを取得する。波長範囲は励起波長、蛍光波長ともに２００ｎｍ〜６００ｎｍで測定を行う。
(Measurement method and ion exchange resin performance evaluation method)
As a method for measuring the organic substance adsorption amount of the ion exchange resin, a fluorometric method is used. The fluorescence photometry is a method for measuring fluorescence emitted when a substance contained in a sample is excited by irradiating the measurement sample with light and returns to the ground state. Since the excitation wavelength and fluorescence wavelength differ depending on the ion exchange resin or organic substance to be measured, an apparatus capable of collecting three-dimensional fluorescence spectrum data is preferable. The ion exchange resin to be measured is dried, pulverized, and molded on a plate. At that time, in order to carry out accurate quantification, it is necessary to make the mold and the amount of ion exchange resin to be molded constant. The excitation ion wavelength is scanned with respect to the molded ion exchange resin, the fluorescence wavelength is obtained, and three-dimensional fluorescence spectrum data is obtained. The wavelength range is measured at 200 nm to 600 nm for both excitation wavelength and fluorescence wavelength.
有機物が吸着していないイオン交換樹脂について、蛍光光度法による測定を行い、この時、異なる励起波長において少なくとも２つの蛍光ピークがあることを確認する。次に、有機物を吸着させると、蛍光ピークの強度が吸着量により減衰する。しかしながら、一つのピークのみの減衰傾向は有機物吸着以外の要因もあり、有機物の吸着量を正確に把握することはできない。そこで、本発明では２つのピークにおける強度比（蛍光強度比という）を求めることで、有機物吸着以外の要因は相殺され、有機物の吸着量に依存した減衰傾向が求められる。 The ion exchange resin to which no organic matter is adsorbed is measured by a fluorometric method, and at this time, it is confirmed that there are at least two fluorescent peaks at different excitation wavelengths. Next, when an organic substance is adsorbed, the intensity of the fluorescence peak is attenuated by the amount of adsorption. However, the decay tendency of only one peak is caused by factors other than organic matter adsorption, and the amount of organic matter adsorbed cannot be accurately grasped. Therefore, in the present invention, by obtaining the intensity ratio (referred to as fluorescence intensity ratio) at the two peaks, factors other than organic substance adsorption are offset, and an attenuation tendency depending on the amount of organic substance adsorption is obtained.
蛍光強度比は、蛍光ピーク強度の低いものを蛍光ピーク強度の高いもので除した値である。また、２つの蛍光ピークは、同じ波長であっても異なる波長であっても良いが、同じ蛍光波長であることが好ましい。 The fluorescence intensity ratio is a value obtained by dividing the low fluorescence peak intensity by the high fluorescence peak intensity. The two fluorescence peaks may be the same wavelength or different wavelengths, but are preferably the same fluorescence wavelength.
本発明では、構造既知の指標化合物の吸着量を蛍光光度法で測定される蛍光強度比から推定し、それに基づいて実機の有機物汚染状況を把握するものである。 In the present invention, the amount of adsorption of an index compound having a known structure is estimated from the fluorescence intensity ratio measured by the fluorometric method, and based on this, the actual state of organic contamination is grasped.
このように、本発明では指標有機物の選択と、有機物量による蛍光光度法における蛍光強度比の減衰傾向という２つの新たな知見により、再生薬品の残留性を予測できるようになり、安定した水処理系の管理ができ、適切な交換時期の判断や決定ができるようになる。 As described above, in the present invention, it is possible to predict the persistence of the regenerative chemical by the two new findings of the selection of the indicator organic substance and the decay tendency of the fluorescence intensity ratio in the fluorometric method based on the amount of organic substance, and stable water treatment The system can be managed, and it will be possible to judge and determine an appropriate replacement time.
以下、実施例を挙げて本発明を具体的に説明するが、本発明はこれらの実施例のみに限定されるものではない。 EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated concretely, this invention is not limited only to these Examples.
イオン交換樹脂として弱塩基性ポリスチレン系陰イオン交換樹脂（アンバーライトＩＲＡ９６ＳＢ、商品名、ダウ・ケミカル社製）を用いた。
乾燥した試料を粉砕し、ペレット状に成型したものを測定した。測定機器を以下に示す。
測定機器：Ｆ−７０００型 分光蛍光光度計 日立製
付属品 固体試料ホルダー
測定モード：３次元 データモード：蛍光
励起開始波長：２００．０ｎｍ 励起終了波長：６００．０ｎｍ 励起サンプリング間隔：５．０ｎｍ
蛍光開始波長：２００．０ｎｍ 蛍光終了波長：６００．０ｎｍ 蛍光サンプリング間隔：５．０ｎｍ
Weakly basic polystyrene anion exchange resin (Amberlite IRA 96SB, trade name, manufactured by Dow Chemical Company) was used as the ion exchange resin.
The dried sample was pulverized and measured into a pellet shape. The measuring equipment is shown below.
Measuring instrument: F-7000 type spectrofluorophotometer Hitachi accessory Solid sample holder measurement mode: 3D data mode: fluorescence excitation start wavelength: 200.0 nm excitation end wavelength: 600.0 nm excitation sampling interval: 5.0 nm
Fluorescence start wavelength: 200.0 nm Fluorescence end wavelength: 600.0 nm Fluorescence sampling interval: 5.0 nm
図１に３次元蛍光スペクトルの測定結果の一例を示す。３次元蛍光スペクトルは、励起波長（ｎｍ）、蛍光波長（ｎｍ）、蛍光強度の３軸から構成される。図１において測定対象とした試料は、有機物未吸着の陰イオン交換樹脂である。この蛍光スペクトルにおいて励起波長２８０ｎｍと励起波長３８０ｎｍともに蛍光波長４３０ｎｍに蛍光強度が高く検出されている。 FIG. 1 shows an example of the measurement result of the three-dimensional fluorescence spectrum. The three-dimensional fluorescence spectrum is composed of three axes: excitation wavelength (nm), fluorescence wavelength (nm), and fluorescence intensity. The sample to be measured in FIG. 1 is an anion exchange resin that does not adsorb organic matter. In this fluorescence spectrum, both the excitation wavelength 280 nm and the excitation wavelength 380 nm are detected with high fluorescence intensity at the fluorescence wavelength 430 nm.
次に、指標化合物として没食子酸鉄を用いて、有機物を上記のイオン交換樹脂に吸着させた。 Next, using iron gallate as an indicator compound, organic substances were adsorbed on the ion exchange resin.
イオン交換樹脂の没食子酸鉄の吸着量は、イオン交換樹脂一定量に没食子酸鉄を一定量添加した状態で、所定時間振とうし、没食子酸鉄を吸着させ、イオン交換樹脂と水溶液を分離した後にＴＯＣ濃度を測定し、添加量との差（没食子酸鉄の添加濃度−ＴＯＣ濃度）から算出したものである。 The amount of iron gallate adsorbed on the ion-exchange resin was shaken for a predetermined time with a certain amount of iron gallate added to a certain amount of ion-exchange resin to adsorb iron gallate and separate the ion exchange resin and aqueous solution. The TOC concentration was measured later and calculated from the difference from the addition amount (addition concentration of iron gallate-TOC concentration).
図２に蛍光波長４３０ｎｍにおける励起スペクトルの測定結果を示す。図２の横軸は励起波長を示し、図２の縦軸は蛍光強度を示す。図２においては、異なる有機物汚染濃度（０ｍｇ／Ｌ、２０ｍｇ／Ｌ、２００ｍｇ／Ｌ、８７０ｍｇ／Ｌ、４４００ｍｇ／Ｌ）のイオン交換樹脂のスペクトルを重ねている。蛍光波長４３０ｎｍにおける励起波長２８０ｎｍの蛍光強度と励起波長３８０ｎｍの蛍光強度の比を蛍光強度比と定義し、有機物濃度（有機物汚染濃度）と蛍光強度比をプロットした結果を図３に示す。 FIG. 2 shows the measurement results of the excitation spectrum at a fluorescence wavelength of 430 nm. The horizontal axis in FIG. 2 indicates the excitation wavelength, and the vertical axis in FIG. 2 indicates the fluorescence intensity. In FIG. 2, spectra of ion exchange resins having different organic contamination concentrations (0 mg / L, 20 mg / L, 200 mg / L, 870 mg / L, 4400 mg / L) are superimposed. The ratio of the fluorescence intensity at the excitation wavelength of 280 nm and the fluorescence intensity at the excitation wavelength of 380 nm at the fluorescence wavelength of 430 nm is defined as the fluorescence intensity ratio, and the result of plotting the organic substance concentration (organic matter contamination concentration) and the fluorescence intensity ratio is shown in FIG.
次に、イオン交換樹脂の再生薬品の残留性と有機物濃度の評価法を説明する。先ず、イオン交換樹脂に没食子酸鉄を一定量吸着させた樹脂（作成方法に関しては、上記の蛍光法による試料の作成法と同様）を樹脂搭に充填した後、その樹脂搭に再生薬品を樹脂の約５倍量通薬した。次に、樹脂搭に一定流速で純水を流し、充填された樹脂に対して純水洗浄を行った。そして、純水洗浄を開始してから６０分後に樹脂搭の出口から流れる水の電気伝導率を測定した。再生薬品を通薬する工程において、樹脂からの没食子酸鉄の脱離が考えられるため、樹脂を通過した薬液を回収し、その通過した薬液中のＴＯＣ量を測定することで樹脂の残留有機物量（有機物濃度）を算出した。
Next, the evaluation method of the persistence of the regenerative chemical of the ion exchange resin and the organic substance concentration will be described. First, the resin tower is filled with a resin in which a certain amount of iron gallate is adsorbed on an ion exchange resin (the preparation method is the same as the preparation method of the sample by the fluorescence method described above), and then a regenerative chemical is put on the resin tower. About 5 times the dose. Next, pure water was allowed to flow through the resin tower at a constant flow rate, and the filled resin was washed with pure water. And the electrical conductivity of the water which flows from the exit of a
図４に残留有機物濃度と、純水洗浄を開始してから６０分後のイオン交換樹脂塔出口から流れる水の電気伝導率の測定結果を示す。図４の横軸は、１回目の有機物吸着後の１回目の通液−純水洗浄後（１−１）、２回目の有機物吸着後の１回目の通液−純水洗浄後（２−１）、２回目の通液−純水洗浄後（２−２）、３回目の通液−純水洗浄後（２−３）等を意味する。図５は、図４の結果に基づき、イオン交換樹脂塔の出口から流れる水の電気伝導率を横軸に示し、樹脂の残留有機物量を縦軸に示したものである。図４及び図５を参照すると、樹脂の残留有機物量（有機物濃度）は、イオン交換樹脂塔の出口から流れる水の電気伝導率にほぼ正比例することが分かる。すなわち、この電気伝導率の変動は、フルボ酸やフミン酸といった土壌分解性の有機物に影響を受けており、このことから、没食子酸鉄が指標化合物として使用できることが確認された。
FIG. 4 shows the measurement results of the residual organic matter concentration and the electrical conductivity of water flowing from the ion exchange
例えば、イオン交換樹脂の性能が低下したと判断する電気伝導率基準値を、純水洗浄を開始してから６０分後に５０μＳ／ｃｍと設定すると、有機物濃度は２１００ｍｇ／Ｌ−樹脂となる。これは図５の出口電気伝導率と有機物濃度より計算できる。そして、この有機物濃度と蛍光光度法の結果を示す図３より、蛍光強度比が０．４５以下の時にイオン交換樹脂の性能が低下したと判断できる。
For example, if the electric conductivity reference value for determining that the performance of the ion exchange resin has deteriorated is set to 50 μS /
この指標を用いて、実際の原水処理においては、イオン交換樹脂の蛍光強度比が、指標化合物を用いて決定された性能低下の基準値に応じた所定値以下で確認された場合に性能低下と判断し、交換時期を管理することが可能となる。 With this index, in actual raw water treatment, when the fluorescence intensity ratio of the ion exchange resin is confirmed to be a predetermined value or less according to the reference value of the performance decrease determined using the index compound, the performance deterioration It is possible to judge and manage the replacement time.
本発明に係る吸着状態判定方法は、イオン交換樹脂に限定されず樹脂粒子全般に対して有機物の吸着状態の把握に利用することができる。 The adsorption state determination method according to the present invention is not limited to ion-exchange resins, and can be used for grasping the adsorption state of organic substances for all resin particles.
Claims (7)
前記イオン交換樹脂塔に再生薬品の通液し、
前記イオン交換樹脂に対して純水洗浄を行い、
前記純水洗浄を開始してから所定時間経過後の前記イオン交換樹脂塔の出口から流れる液の電気伝導率を測定し、
前記電気伝導率が基準値を超える際の前記イオン交換樹脂に残留する残留有機物濃度を求め、
前記指標化合物の濃度を変えて測定した蛍光光度法による蛍光ピークの強度比から前記残留有機物濃度に対応する強度比を決定し、この強度比以下に外来有機物の前記強度比が確認された場合に性能低下と判断し、イオン交換樹脂の交換を行う請求項６に記載の水処理システムの管理方法。 An ion-exchange resin tower in which an indicator organic substance having a known structure is adsorbed at a predetermined concentration is packed in an ion-exchange resin tower,
Regenerative chemicals are passed through the ion exchange resin tower,
Perform pure water cleaning on the ion exchange resin,
Measure the electrical conductivity of the liquid flowing from the outlet of the ion exchange resin tower after a predetermined time has elapsed since the start of the pure water cleaning,
Obtain the residual organic matter concentration remaining in the ion exchange resin when the electrical conductivity exceeds a reference value,
When the intensity ratio corresponding to the residual organic matter concentration is determined from the fluorescence peak intensity ratio measured by changing the concentration of the indicator compound, and when the intensity ratio of the exogenous organic matter is confirmed below this intensity ratio. The method of managing a water treatment system according to claim 6, wherein the ion exchange resin is replaced by judging that the performance is lowered.
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