JP2003094051A - Regeneration method of boron selective adsorption resin - Google Patents
Regeneration method of boron selective adsorption resinInfo
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- JP2003094051A JP2003094051A JP2001288777A JP2001288777A JP2003094051A JP 2003094051 A JP2003094051 A JP 2003094051A JP 2001288777 A JP2001288777 A JP 2001288777A JP 2001288777 A JP2001288777 A JP 2001288777A JP 2003094051 A JP2003094051 A JP 2003094051A
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- boron
- selective adsorption
- adsorption resin
- resin
- solution
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- Treatment Of Water By Ion Exchange (AREA)
Abstract
(57)【要約】
【課題】 ホウ素を吸着したホウ素選択吸着
樹脂から、鉱酸によってホウ素を溶離後、NaOH溶液を通
液して再生されたホウ素選択吸着樹脂を遊離型に変換し
た後、改めてホウ素含有排液を通液したとき通液当初の
処理液に塩酸や硫酸等の酸を添加するｐH調整を行わな
くてもよい樹脂再生方法を提案する。
【解決手段】 N-メチルグルカミン基を有するホ
ウ素選択吸着樹脂に吸着したホウ素を鉱酸により溶離
後、NaOH溶液を通液して、該ホウ素選択吸着樹脂を遊離
型に変換する再生処理を行うに際し、NaOH溶液の通液量
を、前記NaOH溶液の通液後、洗浄及び逆洗浄を行った状
態で前記ホウ素選択吸着樹脂を取り囲む溶液のpHが7.5
〜8.5になるように制御する。この際、前記NaOH溶液の
通液量を、前記ホウ素選択吸着樹脂を取り囲む溶液のpH
がほぼ処理排水のpHと同一となるように制御することが
より好ましい。
(57) [Summary] PROBLEM TO BE SOLVED: To elute boron with a mineral acid from a boron selective adsorption resin that has adsorbed boron, pass through a NaOH solution, convert the regenerated boron selective adsorption resin to a free form, and then renew it The present invention proposes a resin regeneration method that does not require pH adjustment by adding an acid such as hydrochloric acid or sulfuric acid to the treatment liquid at the beginning of the passage of the boron-containing waste liquid. SOLUTION: After eluted with a mineral acid, boron adsorbed on a boron selective adsorption resin having an N-methylglucamine group is passed through a NaOH solution to perform a regeneration treatment for converting the boron selective adsorption resin to a free form. When passing the NaOH solution, after passing the NaOH solution, the pH of the solution surrounding the boron selective adsorption resin in a state where washing and back washing have been performed is 7.5.
Control to be 8.5. At this time, the flow rate of the NaOH solution was adjusted to the pH of the solution surrounding the boron selective adsorption resin.
Is more preferably controlled to be substantially equal to the pH of the treated wastewater.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、N-メチルグルカミ
ン基を有するホウ素選択吸着樹脂の再生方法に係り、特
にホウ素を吸着したホウ素選択吸着樹脂に鉱酸を通液し
てホウ素を溶離後、NaOH溶液を通液して該ホウ素選択吸
着樹脂を遊離型に変換して再使用に供するN-メチルグル
カミン基を有するホウ素選択吸着樹脂の再生方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for regenerating a boron-selective adsorption resin having an N-methylglucamine group, and in particular, after a mineral acid is passed through the boron-selective adsorption resin having adsorbed boron to elute boron. The present invention relates to a method for regenerating a boron-selective adsorption resin having an N-methylglucamine group, which is passed through a NaOH solution to convert the boron-selective adsorption resin into a free form for reuse.
【０００２】[0002]
【従来の技術】一般にニッケルメッキ液あるいはアルミ
表面処理液中にはホウ素化合物（ホウ酸等）が含まれて
おり、これらを扱う工場ではホウ素を含有する洗浄排水
が発生する。また、ガラス、釉薬、アルミコンデンサー
等ホウ素を使用する工場においてもホウ素を含む工場排
水が発生する。さらにごみ焼却場、石炭火力発電所等に
おいてもホウ素を含む排水が発生する。2. Description of the Related Art Generally, a nickel plating solution or an aluminum surface treatment solution contains a boron compound (boric acid, etc.), and a cleaning waste water containing boron is generated in a factory handling these compounds. In addition, factories using boron such as glass, glaze, and aluminum capacitors also generate factory wastewater containing boron. Furthermore, wastewater containing boron is also generated in refuse incineration plants, coal-fired power plants, and the like.
【０００３】ホウ素は植物にとっては必須微量元素であ
り、海水には4〜5mg/l程度含まれていることは周知のこ
とである。一方、ホウ素はある濃度以上に存在すると、
植物の成長を阻害したり、動物に対して神経障害を起こ
すおそれがあるといわれている。さらに人体に与える影
響は必ずしも明確ではないものの低濃度の継続摂取にお
いて生殖機能の低下などの健康障害を起こす可能性が指
摘されている。平成11年2月、ホウ素の環境基準として1
mg/l以下が告示され、平成13年6月に排水基準も公布、7
月1日より施行されたため、これらのホウ素を含む工場
排水中のホウ素除去処理が必要となってきている。Boron is an essential trace element for plants, and it is well known that sea water contains about 4 to 5 mg / l. On the other hand, when boron is present at a certain concentration or higher,
It is said that it may inhibit the growth of plants or cause nerve damage to animals. Furthermore, although the effects on the human body are not always clear, it has been pointed out that continued ingestion of low concentrations may cause health problems such as reduced reproductive function. February 1999, 1 as an environmental standard for boron
Following notification of mg / l, promulgated drainage standard in June 2001, 7
Since it was carried out from the 1st of March, it is necessary to remove the boron in the wastewater from the factory that contains these boron.
【０００４】排水中のホウ素を除去する方法には種々の
方法があるが、ホウ素を含有する排水をホウ素選択吸着
樹脂に吸着させ、それにより排水を浄化するとともに、
樹脂に吸着したホウ素を酸やアルカリを用いて溶離し、
溶離液から陰イオンである酸根やアルカリを除いて純度
の高いホウ素含有水を得る方法が、使用薬剤が少なく、
かつ発生汚泥も少ない方法として注目を浴びている。There are various methods for removing boron in wastewater, but wastewater containing boron is adsorbed on a boron selective adsorption resin to purify the wastewater, and
Elute the boron adsorbed on the resin with acid or alkali,
The method of obtaining highly pure boron-containing water by removing the acid radicals and alkalis that are anions from the eluent is less chemicals used,
In addition, it is drawing attention as a method that produces less sludge.
【０００５】この方法では、ホウ素含有排水からホウ素
を除去する樹脂としてN-メチルグルカミン基を有するホ
ウ素選択吸着樹脂を用い、これに排水を通液してホウ素
を吸着させ、しかる後、鉱酸によるホウ素溶離を行い、
さらにNaOH溶液を通液して上記樹脂を遊離型に変換して
再使用できる状態に再生する。この際のNaOHの使用量
は、概ね40〜120g/l-R（g/l-Rは樹脂1l当たりのNaOHの
使用量）とされている。In this method, a boron selective adsorption resin having an N-methylglucamine group is used as a resin for removing boron from boron-containing wastewater, and the wastewater is passed through this resin to adsorb boron. Elute boron with
Further, a NaOH solution is passed through to convert the above resin into a free form and regenerate it for reuse. The amount of NaOH used at this time is generally 40 to 120 g / lR (g / lR is the amount of NaOH used per liter of resin).
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、このよ
うな量のNaOHを用いて樹脂の再生処理を行うと、樹脂は
遊離型に完全に再生され、再びホウ素を十分に吸着でき
るようになるが、この完全再生樹脂をホウ素除去工程に
供すると、通液開始当初の処理液のpHが大きくアルカリ
側にふれ、処理液をそのまま放流することができず、処
理液に塩酸や硫酸等の酸を添加してpH調整を行わなけれ
ばならないという問題がある。However, when the resin is regenerated by using such an amount of NaOH, the resin is completely regenerated into a free form, and boron can be sufficiently adsorbed again. When this completely regenerated resin is subjected to the boron removal step, the pH of the treatment liquid at the beginning of the passage is large and it touches the alkali side, and the treatment liquid cannot be discharged as it is, and acids such as hydrochloric acid and sulfuric acid are added to the treatment liquid. Then, there is a problem that the pH must be adjusted.
【０００７】本発明は、上記樹脂再生工程における問題
を解決することを目的としてなされたもので、ホウ素を
吸着したホウ素選択吸着樹脂から、鉱酸によってホウ素
を溶離後、NaOH溶液を通液して再生されたホウ素選択吸
着樹脂を遊離型に変換した後、改めてホウ素含有排液を
通液したとき通液当初の処理液に塩酸や硫酸等の酸を添
加するｐH調整を行わなくてもよいホウ素選択吸着樹脂
の再生方法を提案することを目的とする。The present invention has been made for the purpose of solving the problem in the above-mentioned resin regeneration step. After elution of boron with a mineral acid from a boron selective adsorption resin having adsorbed boron, a NaOH solution is passed through. After the regenerated boron selective adsorption resin is converted to the free type, when the boron-containing waste liquid is passed through again, it is not necessary to adjust the pH by adding an acid such as hydrochloric acid or sulfuric acid to the initial treatment liquid. The purpose is to propose a method for regenerating a selective adsorption resin.
【０００８】[0008]
【課題を解決するための手段】本発明のホウ素選択吸着
樹脂の再生方法では、N-メチルグルカミン基を有するホ
ウ素選択吸着樹脂に吸着したホウ素を鉱酸により溶離
後、NaOH溶液を通液して、該ホウ素選択吸着樹脂を遊離
型に変換する再生処理を行うに際し、NaOH溶液の通液量
を、前記NaOH溶液の通液後、洗浄及び逆洗浄を行った状
態で前記ホウ素選択吸着樹脂を取り囲む溶液のpHが7.5
〜8.5になるように制御する。この際、前記NaOH溶液の
通液量を、前記ホウ素選択吸着樹脂を取り囲む溶液のpH
がほぼ処理排水のpHと同一となるように制御することが
より好ましい。In the method for regenerating a boron selective adsorption resin of the present invention, the boron adsorbed on the boron selective adsorption resin having an N-methylglucamine group is eluted with a mineral acid, and then a NaOH solution is passed through. When performing a regeneration treatment for converting the boron selective adsorption resin to a free form, the passing amount of the NaOH solution is changed to the boron selective adsorption resin in a state where washing and back washing are performed after passing the NaOH solution. PH of surrounding solution is 7.5
Control to be ~ 8.5. At this time, the flow rate of the NaOH solution, the pH of the solution surrounding the boron selective adsorption resin
It is more preferable to control so that the pH is almost the same as the pH of the treated wastewater.
【０００９】[0009]
【発明の実施の形態】以下、実験例を参照して本発明の
実施形態を具体的に説明する。BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be specifically described below with reference to experimental examples.
【００１０】内径20mm、高さ500mmのアクリル製カラム
を１本用意し、N-メチルグルカミン基を有するホウ素選
択吸着樹脂に硫酸処理を309g as H2SO4/l-Rの条件で行
い、次いでNaOH溶液を用いた遊離型への変換を、11、3
3、77g as NaOH/l-Rの3水準で行って樹脂を遊離型に再
生した。この再生樹脂に、さらにイオン交換水を各々流
速500ml/hで1h通液して樹脂に残存する薬剤を抽出・洗浄
した後、カラムから樹脂を取りだし、全体を十分混合し
た上でカラムに戻し、各再生樹脂の50mlを充填した樹脂
床を作った。この樹脂床に表１に示す成分を含むホウ素
含有水を流速1,000ml/hで通液した。One acrylic column having an inner diameter of 20 mm and a height of 500 mm was prepared, and a boron selective adsorption resin having an N-methylglucamine group was treated with sulfuric acid under the condition of 309 g as H 2 SO 4 / lR, and then NaOH. Conversion to free form using solution
The resin was regenerated to the free form at three levels of 3,77 g as NaOH / lR. Ion-exchanged water was further passed through the regenerated resin for 1 h at a flow rate of 500 ml / h to extract and wash the drug remaining in the resin, and then the resin was taken out from the column, thoroughly mixed and returned to the column, A resin bed filled with 50 ml of each reclaimed resin was made. Boron-containing water containing the components shown in Table 1 was passed through this resin bed at a flow rate of 1,000 ml / h.
【００１１】[0011]
【表１】 [Table 1]
【００１２】図２は、このときのNaOH処理量とホウ素漏
出濃度が10mg/lとなった時点までに樹脂単位体積当たり
に吸着した積算ホウ素吸着量とのグラフであり、図１
は、通液量と処理液のpHの関係を示すグラフである。FIG. 2 is a graph showing the amount of NaOH treated and the cumulative amount of adsorbed boron adsorbed per unit volume of resin by the time when the boron leakage concentration reached 10 mg / l.
[Fig. 4] is a graph showing the relationship between the flow rate and the pH of the treatment liquid.
【００１３】図１から明らかなように、処理液のpHはNa
OH処理量によって異なり、NaOH処理量が11g/l-Rの樹脂
は通液初期の処理pHがほぼ原水pHに近い値（7.9近傍）
で始まったが、NaOH処理量がより多い樹脂の場合にはpH
が12付近となった。一方、ホウ素漏出濃度が10mg/lとな
った時点までに樹脂単位体積当たりに吸着した積算ホウ
素吸着量は、図２に示されているように、NaOH処理量が
33g/l-Rの場合および77g/l-Rには2.9g/l-Rであるのに対
して、NaOH処理量が11g/l-Rの場合には2.6g/l-Rとなっ
た。As is clear from FIG. 1, the pH of the treatment liquid is Na.
Depending on the OH treatment amount, the resin with a NaOH treatment amount of 11 g / lR has a treatment pH at the beginning of liquid flow that is close to the pH of raw water (near 7.9)
However, for resins with higher NaOH throughput, pH
Became around 12. On the other hand, the cumulative amount of adsorbed boron per unit volume of the resin by the time the boron leak concentration reached 10 mg / l, as shown in FIG.
In the case of 33 g / lR and 77 g / lR, it was 2.9 g / lR, whereas when the amount of NaOH treated was 11 g / lR, it was 2.6 g / lR.
【００１４】しかしながら、その減少量は完全に再生処
理された樹脂を用いた場合に比べて約10%であり、通液
開始後の処理液のpHがホウ素含有排水（原水）のpHとほ
ぼ同等であることを考慮すると、そのデメリットは十分
に補い得るものである。本発明はこのような知見に基づ
き、上記再生処理の際のNaOHの通液の終点を、ホウ素
含有排水の通液再開後の初期処理水が排水基準の要求す
るpHを満たすこと、再生ホウ素選択吸着樹脂の積算ホ
ウ素吸着量が大きく落ち込まないレベルに保つことがで
きる、という状態に制御するものである。このような樹
脂の再生状態の制御は、上記実験例のように事前に試験
を行ってその条件を定めて行うことができる。However, the reduction amount is about 10% as compared with the case where the completely regenerated resin is used, and the pH of the treatment liquid after the start of the passage is almost equal to the pH of the boron-containing wastewater (raw water). Considering that, the disadvantage can be sufficiently compensated. The present invention is based on such knowledge, the end point of the passing of NaOH during the regeneration treatment, that the initial treated water after restarting the passing of the boron-containing wastewater meets the pH required by the wastewater standard, regenerated boron selection It is controlled so that the accumulated boron adsorption amount of the adsorption resin can be maintained at a level at which it does not drop significantly. Such control of the regenerated state of the resin can be performed by conducting a test in advance and determining the condition as in the above-mentioned experimental example.
【００１５】図３は、本発明を実施するためのプラント
の一例を示す概念図である。以下、これを用いて樹脂の
再生処理を行った場合の具体例を示す。ホウ素選択吸着
塔2にホウ素を吸着したN-メチルグルカミン基を有する
ホウ素選択吸着樹脂を充填し、所定量の硫酸を通液して
ホウ素を溶離後、NaOH溶液を通液する。通液に当たって
は、予備実験により洗浄、逆洗浄後に樹脂を取り囲む溶
液のpHが7.5〜8.5の範囲内になるNaOH溶液の通液量を求
めておき、その条件が達成されるように通液量を制御す
る。具体的には11g as NaOH/l-Rの量を通液する。これ
により樹脂は大部分遊離型に変換される。その後、工業
用水により洗浄及び逆洗浄を行う。まずバルブV1とV4を
開放し、V2とV3を閉じた状態で通常の洗浄を行い、次い
でバルブV1とV4を閉じ、V2とV3を開放して逆洗浄を行
い、pH計4により排出される洗浄水のpHを測定し、樹脂
を取り囲む溶液のpHが7.5〜8.5の範囲内にあることを確
認する。FIG. 3 is a conceptual diagram showing an example of a plant for carrying out the present invention. Hereinafter, a specific example of the case where the resin is used for the regeneration treatment will be described. The boron selective adsorption tower 2 is filled with a boron selective adsorption resin having an N-methylglucamine group having adsorbed boron, and a predetermined amount of sulfuric acid is passed to elute boron, and then a NaOH solution is passed. When passing the solution, in a preliminary experiment, after the washing and backwashing, calculate the passing volume of the NaOH solution that makes the pH of the solution surrounding the resin within the range of 7.5 to 8.5, and then pass it so that the condition is achieved. To control. Specifically, the amount of 11 g as NaOH / lR is passed. This largely converts the resin to the free form. After that, washing and back washing with industrial water are performed. First, the valves V1 and V4 are opened, V2 and V3 are closed, and normal cleaning is performed.Next, the valves V1 and V4 are closed, V2 and V3 are opened, and reverse cleaning is performed. Measure the pH of the wash water and make sure that the pH of the solution surrounding the resin is within the 7.5-8.5 range.
【００１６】[0016]
【発明の効果】本発明は上記のように、ホウ素選択吸着
樹脂に吸着したホウ素を鉱酸により溶離後NaOH溶液を通
液して、該ホウ素選択吸着樹脂を遊離型に変換する再生
処理を行うに際し、NaOH溶液の通液量を前記NaOH溶液の
通液後、洗浄及び逆洗浄を行った状態で前記ホウ素選択
吸着樹脂を取り囲む溶液のpHが7.5〜8.5になるように制
御したので、ホウ素含有排水を再通水したとき、処理水
のpHが排水基準を満たすようにすることができる。した
がって、従来では必要であった処理水のpH調整工程、そ
の設備を省略することができる。As described above, according to the present invention, the boron adsorbed on the boron selective adsorption resin is eluted with a mineral acid, and then a NaOH solution is passed through to carry out a regeneration treatment for converting the boron selective adsorption resin into a free form. At this time, since the passing amount of the NaOH solution was controlled so that the pH of the solution surrounding the boron selective adsorption resin was 7.5 to 8.5 after the passing of the NaOH solution and the washing and the back washing were performed. When the wastewater is re-passed, the pH of the treated water can be adjusted to meet the wastewater standards. Therefore, it is possible to omit the pH adjusting step of the treated water and the equipment therefor which were conventionally required.
【図１】 NaOH処理量の異なる樹脂を用いて行ったカラ
ムテストの通液量と処理液のpHの関係を示すグラフであ
る。FIG. 1 is a graph showing the relationship between the flow rate of a column test conducted using resins having different NaOH treatment amounts and the pH of the treatment liquid.
【図２】 NaOH処理量と処理液中のホウ素リーク濃度10
mg/lにおけるホウ素吸着量の関係を示すグラフである。[Figure 2] Treatment amount of NaOH and boron leak concentration in the treatment solution 10
It is a graph which shows the relationship of the amount of adsorption of boron in mg / l.
【図３】 本発明を実施するためのプラントの一例を示
す概念図である。FIG. 3 is a conceptual diagram showing an example of a plant for carrying out the present invention.
１：ポンプ ２：ホウ素選択吸着樹脂塔 ３：処理水槽 ４：pH計 １１：H2SO4貯槽 １２：NaOH貯槽 １３：工業用水貯槽1: Pump 2: Boron selective adsorption resin tower 3: Treated water tank 4: pH meter 11: H 2 SO 4 storage tank 12: NaOH storage tank 13: Industrial water storage tank
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Claims (2)
択吸着樹脂に吸着したホウ素を鉱酸により溶離後、NaOH
溶液を通液して、該ホウ素選択吸着樹脂を遊離型に変換
する再生処理を行うに際し、 NaOH溶液の通液量を、前記NaOH溶液の通液後、洗浄及び
逆洗浄を行った状態で前記ホウ素選択吸着樹脂を取り囲
む溶液のpHが7.5〜8.5になるように制御することを特徴
とするホウ素選択吸着樹脂の再生方法。1. Boron adsorbed on a boron selective adsorption resin having an N-methylglucamine group is eluted with mineral acid and then NaOH is added.
When the solution is passed through and a regeneration treatment for converting the boron selective adsorption resin into a free form is performed, the passing amount of the NaOH solution is set to the above-mentioned state after washing and back washing after passing the NaOH solution. A method for regenerating a boron selective adsorption resin, characterized in that the pH of a solution surrounding the boron selective adsorption resin is controlled to be 7.5 to 8.5.
着樹脂を取り囲む溶液のpHがほぼ処理排水のpHと同一と
なるように制御することを特徴とする請求項１記載のホ
ウ素選択吸着樹脂の再生方法。2. The boron selective adsorption according to claim 1, wherein the passing amount of the NaOH solution is controlled so that the pH of the solution surrounding the boron selective adsorption resin is substantially the same as the pH of the treated wastewater. Resin regeneration method.
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| JP2001288777A JP2003094051A (en) | 2001-09-21 | 2001-09-21 | Regeneration method of boron selective adsorption resin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006110574A1 (en) * | 2005-04-08 | 2006-10-19 | Dow Global Technologies Inc. | Alkaline regeneration of n-methyl-d-glucamine functional resins |
| JP2011056465A (en) * | 2009-09-14 | 2011-03-24 | Toshiba Corp | Boron adsorbing composition, boron adsorbent, and system and using method thereof |
| CN115645983A (en) * | 2022-10-15 | 2023-01-31 | 湘南学院 | Process for directly recovering silver and copper from waste acid |
| CN116607010A (en) * | 2023-07-19 | 2023-08-18 | 长沙华时捷环保科技发展股份有限公司 | Method for removing and recovering lead from lead-containing solution |
-
2001
- 2001-09-21 JP JP2001288777A patent/JP2003094051A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006110574A1 (en) * | 2005-04-08 | 2006-10-19 | Dow Global Technologies Inc. | Alkaline regeneration of n-methyl-d-glucamine functional resins |
| AU2006235251B2 (en) * | 2005-04-08 | 2010-08-19 | Dow Global Technologies Inc. | Alkaline regeneration of N-Methyl-D-glucamine functional resins |
| US7811457B2 (en) | 2005-04-08 | 2010-10-12 | Dow Global Technologies Inc. | Alkaline regeneration of N-methyl-D-glucamine functional resins |
| JP2011056465A (en) * | 2009-09-14 | 2011-03-24 | Toshiba Corp | Boron adsorbing composition, boron adsorbent, and system and using method thereof |
| CN115645983A (en) * | 2022-10-15 | 2023-01-31 | 湘南学院 | Process for directly recovering silver and copper from waste acid |
| CN116607010A (en) * | 2023-07-19 | 2023-08-18 | 长沙华时捷环保科技发展股份有限公司 | Method for removing and recovering lead from lead-containing solution |
| CN116607010B (en) * | 2023-07-19 | 2023-10-17 | 长沙华时捷环保科技发展股份有限公司 | Method for removing and recovering lead from lead-containing solution |
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