【特許請求の範囲】
【請求項１】 ホウ素を吸着したイオン交換樹脂から酸根によりホウ素を溶離するに際し、ホウ素を吸着したイオン交換樹脂を充填したイオン交換塔と、ｎ個（ｎ≦２）の再生液タンクと、水タンクと、溶離液タンクとを備え、イオン交換塔内に充液する工程と、第１の再生液タンク内の再生液をこのイオン交換塔に通してホウ素を溶離させ、溶離した溶離液をタンクに収容する工程と、第ｎの再生液タンク内の再生液をイオン交換塔を通して、ホウ素を含む液を第ｎ−１の再生液タンクに収容する処理を順次おこなう工程と、第ｎの再生液タンクに酸根を加えて、再生液を作る工程と、水タンクに水を供給する工程とを具備したことを特徴とする、イオン交換樹脂に吸着したホウ素の回収方法。
【請求項２】 イオン交換樹脂に付着したスラッジ等を除去した後、請求項１に記載のホウ素を吸着したイオン交換樹脂の再生をおこなうことを特徴とする、イオン交換樹脂に吸着したホウ素の回収方法。
【請求項３】 イオン交換塔への充液を、再生液もしくはイオン交換樹脂の再生を行った後のホウ素濃度の薄い部分の液を用いて、溶離液中のホウ素濃度を高めることを特徴とする請求項１に記載の回収方法。
【請求項４】 ホウ素を吸着したイオン交換樹脂を充填したイオン交換塔と、このイオン交換塔内のイオン交換樹脂を再生するための再生液を充填した複数の第１〜第ｎ再生液タンクと、イオン交換塔内を洗浄する水を入れた水タンクと、イオン交換塔に再生液を通して溶離されたホウ素を入れる溶離液タンクと、このイオン交換塔に第１再生液タンクの再生液を通してホウ素を溶離し、溶離液をタンクに収容した後、第ｎの再生液タンク内の再生液をイオン交換塔を通して、第ｎ−１の再生液タンクに収容する処理をｎ＝２の再生液タンクから順番におこなう制御をする制御手段とを具備したホウ素の回収装置。
【請求項５】 ホウ素を吸着したイオン交換塔内のイオン交換樹脂に含まれる夾雑物を除去する装置を備えた請求項４に記載のホウ素の回収装置。
[Claims]
1. An ion-exchange column filled with an ion-exchange resin having boron adsorbed thereon, wherein n (n ≦ 2) regenerating solution tanks are used for eluting boron from an ion-exchange resin having adsorbed boron by an acid radical. A step of charging an ion exchange tower with a tank and an eluent tank, and eluted boron by passing the regenerated liquid in the first regenerated liquid tank through the ion exchange tower, And a step of sequentially performing a process of storing the boron-containing liquid in the (n-1) th regenerating liquid tank through the ion exchange tower and a step of storing the regenerating liquid in the n-th regenerating liquid tank. A method for recovering boron adsorbed on an ion exchange resin, comprising: a step of adding an acid group to a tank to form a regenerating solution; and a step of supplying water to a water tank.
2. A method for recovering boron adsorbed on an ion-exchange resin, the method comprising regenerating the ion-exchange resin adsorbed with boron according to claim 1, after removing sludge or the like adhering to the ion-exchange resin. Method.
3. The method according to claim 1, wherein the filling of the ion exchange column is carried out by using a regenerating solution or a portion of the solution having a low boron concentration after regenerating the ion exchange resin to increase the boron concentration in the eluent. The recovery method according to claim 1.
4. An ion exchange tower filled with an ion exchange resin adsorbed with boron, and a plurality of first to n-th regenerating liquid tanks filled with a regenerating liquid for regenerating the ion exchange resin in the ion exchange tower. A water tank containing water for washing the inside of the ion exchange tower, an eluent tank for containing boron eluted through the regenerating solution in the ion exchange tower, and a boron solution passing through the regenerating solution in the first regenerating solution tank through the ion exchange tower. After eluting and storing the eluent in the tank, the regenerating solution in the n-th regenerating solution tank is passed through the ion exchange tower, and the process of storing the regenerating solution in the (n-1) -th regenerating solution tank is started from the regenerating solution tank of n = 2 And a control means for controlling the recovery of the boron.
5. The boron recovery device according to claim 4, further comprising a device for removing impurities contained in the ion exchange resin in the ion exchange tower to which the boron has been adsorbed.
（４） ホウ素を吸着したイオン交換樹脂を充填したイオン交換塔と、このイオン交換塔内のイオン交換樹脂を再生するための再生液を充填した複数の第１〜第ｎ再生液タンクと、イオン交換塔内を洗浄する水を入れた水タンクと、イオン交換塔に再生液を通して溶離されたホウ素を入れる溶離液タンクと、このイオン交換塔に第１再生液タンクの再生液を通してホウ素を溶離し、溶離液をタンクに収容した後、第ｎの再生液タンク内の再生液をイオン交換塔を通して、第ｎ−１の再生液タンクに収容する処理をｎ＝２の再生液タンクから順番におこなう制御をする制御手段とを具備したホウ素の回収装置。
(4) an ion exchange tower filled with an ion exchange resin adsorbed with boron, a plurality of first to n-th regenerating liquid tanks filled with a regenerating liquid for regenerating the ion exchange resin in the ion exchange tower, A water tank containing water for washing the inside of the exchange tower, an eluent tank for containing boron eluted through the regenerating solution in the ion exchange tower, and boron eluted through the regenerating solution in the first regenerating solution tank into the ion exchange tower. After the eluent is stored in the tank, the process of storing the regenerated liquid in the n-th regenerated liquid tank in the (n-1) -th regenerated liquid tank through the ion exchange tower is performed in order from the regenerated liquid tank of n = 2. An apparatus for recovering boron, comprising: control means for controlling.
なお、本発明は上記実施の形態に限らず、レベル計ＬＣ１〜ＬＣ４はイオン交換塔への供給液を測定して制御できる積算流量計であっても構わない。また、第１再生液で処理されたものについてのみ、溶離液タンクに入れる例を説明したが、本発明はこれに限らず、第２〜第４再生液タンク２２、２３、２４での処理において、回収液中のホウ素濃度の高い部分をホウ素溶離液として系外に払い出すことも可能である。更に再生液タンク２４における硫酸の濃度制御は、硫酸濃度を検知し制御できるものであってもかまわない。
Note that the present invention is not limited to the above embodiment, and the level meters LC1 to LC4 may be integrating flow meters that can measure and control the liquid supplied to the ion exchange tower. Also, an example has been described in which only those treated with the first regenerating liquid are placed in the eluent tank, but the present invention is not limited to this, and the processing in the second to fourth regenerating liquid tanks 22, 23, and 24 is not limited thereto. Alternatively, a portion having a high boron concentration in the recovered liquid can be discharged out of the system as a boron eluent. Further, the control of the sulfuric acid concentration in the regenerating liquid tank 24 may be one that can detect and control the sulfuric acid concentration.
［実施例１］内径３４ｍｍ、高さ１、０００ｍｍのアクリル製カラムを用意し、ホウ素を３ｇ／Ｌ（イオン交換樹脂換算）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３００ｍＬを振動篩によりスラッジを除去した後充填する。イオン交換水１５０ｍＬをカラムに加えることによりイオン交換樹脂間の空気を追い出した後、５％硫酸溶液を６００ｍＬ／Ｈｒで通液して吸着したホウ素を溶離する。通液量（ＢＶ）によるホウ素、硫酸の漏出、及び処理液のＰＨを図４に示す。図より明らかなように通液して１ＢＶ以降でないとホウ素溶離は始まらず、ホウ素濃度が最高になるのは２．０ＢＶの時点であった。また溶離液中のホウ素濃度がホウ素の排水規制値に相当すると思われる１０ｍｇ／Ｌ以下になるためには、５％硫酸溶液通液量は４．１ＢＶであった。
[Example 1] An acrylic column having an inner diameter of 34 mm and a height of 1,000 mm was prepared, and 300 mL of a boron selective adsorption resin having an N-methylglucamine group adsorbing boron at 3 g / L (in terms of ion exchange resin) was vibrated through a vibrating sieve. After removing the sludge by the above, filling is performed. The air between the ion exchange resins is expelled by adding 150 mL of ion exchanged water to the column, and then the adsorbed boron is eluted by passing a 5% sulfuric acid solution at 600 mL / Hr. FIG. 4 shows the leakage of boron and sulfuric acid and the pH of the processing solution depending on the flow rate (BV). As is clear from the figure, the boron elution did not start until the liquid passed through and after 1 BV, and the maximum boron concentration was at 2.0 BV. Further, in order for the boron concentration in the eluent to be 10 mg / L or less, which is considered to correspond to the regulated value of boron wastewater, the flow rate of the 5% sulfuric acid solution was 4.1 BV.
［実施例２］内径３４ｍｍ、高さ１、０００ｍｍのアクリル製カラムを用意し、ホウ素を３ｇ／Ｌ（イオン交換樹脂換算）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３００ｍＬを振動篩によりスラッジを除去した後充填する。５％硫酸溶液１５０ｍＬをカラムに加えることによりイオン交換樹脂間の空気を追い出した後、５％硫酸溶液を６００ｍＬ／Ｈｒで通液して吸着したホウ素を溶離する。通液量（ＢＶ）によるホウ素、硫酸を漏出、及び処理液のＰＨを図５に示す。図より明らかなように通液当初からホウ素溶離は始まり、１．５ＢＶでホウ素濃度は最高になった。しかし溶離液中のホウ素濃度がホウ素の排水規制値に相当すると思われる１０ｍｇ／Ｌ以下になるためには、５％硫酸溶液通液量は３．７ＢＶであった。
[Example 2] An acrylic column having an inner diameter of 34 mm and a height of 1,000 mm was prepared, and 300 mL of a boron selective adsorption resin having an N-methylglucamine group adsorbing boron at 3 g / L (in terms of ion exchange resin) was vibrated through a sieve. After removing the sludge by the above, filling is performed. The air between the ion exchange resins is expelled by adding 150 mL of a 5% sulfuric acid solution to the column, and then the adsorbed boron is eluted by passing the 5% sulfuric acid solution at 600 mL / Hr. FIG. 5 shows the leakage of boron and sulfuric acid and the pH of the treatment liquid based on the flow rate (BV). As is clear from the figure, boron elution started from the beginning of the passage, and the boron concentration reached the highest at 1.5 BV. However, the flow rate of the 5% sulfuric acid solution was 3.7 BV so that the boron concentration in the eluent was 10 mg / L or less, which is considered to correspond to the regulation value of boron wastewater.