JP7184152B1 - Separation column for mixed ion exchange resin and method for separating mixed ion exchange resin using the same - Google Patents

Separation column for mixed ion exchange resin and method for separating mixed ion exchange resin using the same Download PDF

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JP7184152B1
JP7184152B1 JP2021209423A JP2021209423A JP7184152B1 JP 7184152 B1 JP7184152 B1 JP 7184152B1 JP 2021209423 A JP2021209423 A JP 2021209423A JP 2021209423 A JP2021209423 A JP 2021209423A JP 7184152 B1 JP7184152 B1 JP 7184152B1
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exchange resin
ion exchange
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JP2023094132A (en
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祐一 小川
みどり 宮地
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Kurita Water Industries Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/05—Regeneration or reactivation of ion-exchangers; Apparatus therefor of fixed beds
    • B01J49/09—Regeneration or reactivation of ion-exchangers; Apparatus therefor of fixed beds of mixed beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/60—Cleaning or rinsing ion-exchange beds
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange

Abstract

【課題】 混床式イオン交換装置などのイオン交換樹脂を高精度で分離することの可能なイオン交換樹脂の分離塔を提供する。【解決手段】 混合イオン交換樹脂の分離塔１は、円筒形の分離塔本体１Ａの底部に注水部としての給水管２及び複数の吐出ノズル２Ａを有し、頂部には排出部としての排出管３が接続している。この分離塔本体１Ａの吐出ノズル２Ａの上側には集水板４が配置されているとともに、分離塔本体１Ａの上端側にはスクリーン５は配置されている。このスクリーン５は、混合イオン交換樹脂のうち平均粒径が最も小さいイオン交換樹脂の平均粒径の９０％以下の網目を有する。【選択図】 図１[Problem] To provide an ion-exchange resin separation tower such as a mixed-bed ion-exchange apparatus capable of separating an ion-exchange resin with high accuracy. SOLUTION: A separation tower 1 for mixed ion exchange resin has a water supply pipe 2 as a water injection part and a plurality of discharge nozzles 2A at the bottom of a cylindrical separation tower main body 1A, and a discharge pipe as a discharge part at the top. 3 are connected. A water collecting plate 4 is arranged above the discharge nozzle 2A of the separation tower main body 1A, and a screen 5 is arranged on the upper end side of the separation tower main body 1A. This screen 5 has a mesh size of 90% or less of the average particle size of the ion exchange resin having the smallest average particle size among the mixed ion exchange resins. [Selection diagram] Fig. 1

Description

本発明は、純水製造装置などに用いる混床式イオン交換装置などで使用した混合イオン交換樹脂を分離する分離塔、およびこれを用いた混床式イオン交換装置などを構成する混合イオン交換樹脂の分離方法に関する。 The present invention relates to a separation tower for separating a mixed ion exchange resin used in a mixed bed ion exchange device used in a pure water production apparatus, etc., and a mixed ion exchange resin constituting a mixed bed ion exchange device using the same. It relates to the separation method of.

通常、純水製造装置では原水中の不純物を除去して清浄度を高めているが、イオン性の不純物、すなわちアニオン性の不純物とカチオン性の不純物を除去するためにアニオン交換樹脂とカチオン交換樹脂とを混合充填した混床式イオン交換装置が汎用的に用いられている。この混床式イオン交換装置では、イオン交換樹脂はイオン交換容量に相当する量のイオンを除去すると、それ以上のイオン性不純物は除去できずに破過する。そこで、ある程度の水量を処理したら、この混床式イオン交換装置からイオン交換樹脂を回収してそれぞれ分離し、カチオン交換樹脂再生塔、アニオン交換樹脂再生塔でそれぞれ硫酸や苛性ソーダなどにより再生して再度混床式イオン交換装置に充填して再利用することが行われている。 Normally, a pure water production system removes impurities in the raw water to improve cleanliness. A mixed-bed type ion exchange apparatus filled with a mixture of and is commonly used. In this mixed-bed type ion exchange apparatus, when the ion exchange resin removes ions in an amount corresponding to the ion exchange capacity, it breaks through without being able to remove any more ionic impurities. Therefore, after treating a certain amount of water, the ion exchange resin is recovered from this mixed bed ion exchange device, separated, and regenerated with sulfuric acid or caustic soda in the cation exchange resin regeneration tower and the anion exchange resin regeneration tower, respectively. Reuse is performed by filling a mixed-bed ion exchange device.

この混合イオン交換樹脂による処理水質はイオン交換樹脂の再生状態により決定されるが、樹脂の再生状態をより高度に維持するためには、逆再生をできるだけ生じさせない必要がある。逆再生とは、アニオン交換樹脂の混入したカチオン交換樹脂を塩酸や硫酸など酸溶液で再生する際、アニオン交換樹脂がＣｌ形やＳＯ４形などに再生され、またカチオン交換樹脂の混入したアニオン交換樹脂を水酸化ナトリウムなどのアルカリ溶液で再生する際、カチオン交換樹脂がＮａ形などに再生されることである。 The quality of water treated by this mixed ion exchange resin is determined by the state of regeneration of the ion exchange resin, and in order to maintain the state of regeneration of the resin at a higher level, it is necessary to prevent reverse regeneration as much as possible. In reverse regeneration, when the cation exchange resin mixed with the anion exchange resin is regenerated with an acid solution such as hydrochloric acid or sulfuric acid, the anion exchange resin is regenerated to the Cl type or SO 4 type, etc., and the anion exchange resin mixed with the cation exchange resin is regenerated. When the resin is regenerated with an alkaline solution such as sodium hydroxide, the cation exchange resin is regenerated to the Na form or the like.

この逆再生を生じさせないためには、２種以上のイオン交換樹脂の混合イオン交換樹脂を再生するとき、カチオン交換樹脂とアニオン交換樹脂とをできるだけ完全に近い状態に分離し、カチオン交換樹脂中へのアニオン交換樹脂の混入、およびアニオン交換樹脂中へのカチオン交換樹脂の混入を極力減少させる必要がある。 In order to prevent this reverse regeneration, when regenerating a mixed ion exchange resin of two or more kinds of ion exchange resins, the cation exchange resin and the anion exchange resin are separated in a state as close to complete as possible, and then transferred into the cation exchange resin. It is necessary to reduce the contamination of the anion exchange resin and the contamination of the anion exchange resin with the cation exchange resin as much as possible.

そこで、アニオン交換樹脂とカチオン交換樹脂とを精度よく分離する方法として、復水脱塩塔内で復水脱塩に使用されたイオン交換樹脂（アニオン交換樹脂とカチオン交換樹脂との混合樹脂）をカチオン交換樹脂再生塔内に導入し、下から逆洗水を上向流にて通水することにより、混合状態のイオン交換樹脂を比重差でアニオン交換樹脂とカチオン交換樹脂の上下２層に分離し、次いで上層を構成するアニオン交換樹脂を選択的に引き抜き、アニオン交換樹脂再生塔に移送し、アルカリにより再生を行う。そして、カチオン交換樹脂再生塔内に残ったカチオン交換樹脂は、該カチオン交換樹脂再生塔にて酸により再生することが提案されている（特許文献１，２）。 Therefore, as a method for accurately separating the anion exchange resin and the cation exchange resin, the ion exchange resin (mixed resin of the anion exchange resin and the cation exchange resin) used for condensate demineralization in the condensate demineralization tower is By introducing it into the cation exchange resin regeneration tower and passing backwash water from the bottom in an upward flow, the mixed ion exchange resin is separated into two upper and lower layers of anion exchange resin and cation exchange resin due to the difference in specific gravity. Then, the anion exchange resin constituting the upper layer is selectively extracted, transferred to an anion exchange resin regeneration tower, and regenerated with alkali. It has been proposed that the cation exchange resin remaining in the cation exchange resin regeneration tower be regenerated with an acid in the cation exchange resin regeneration tower (Patent Documents 1 and 2).

特開２０１９－１８１３６３号公報JP 2019-181363 A 特開２０２０－７５２２６号公報JP 2020-75226 A

しかしながら、近年、高純度の純水を製造する際に混合イオン交換樹脂を使用した場合に、より高度にアニオン交換樹脂とカチオン交換樹脂とを分離することが要望されているが、特許文献１，２などの従来の分離方法では限界があった。 However, in recent years, when a mixed ion exchange resin is used when producing high-purity pure water, it is desired to separate the anion exchange resin and the cation exchange resin to a higher degree. 2 and other conventional separation methods have limitations.

本発明は上記課題に鑑みてなされたものであり、混床式イオン交換装置などで使用した混合イオン交換樹脂分離塔を提供することを目的とする。また、本発明は、混床式イオン交換装置などを構成する混合イオン交換樹脂を高精度で分離することの可能な混合イオン交換樹脂の分離方法を提供することを目的とする。 The present invention has been made in view of the above problems, and an object of the present invention is to provide a mixed ion exchange resin separation column used in a mixed bed ion exchange apparatus or the like. Another object of the present invention is to provide a method for separating a mixed ion-exchange resin, which is capable of separating the mixed ion-exchange resin constituting a mixed-bed ion-exchange apparatus or the like with high accuracy.

上記目的に鑑み、本発明は第一に、２種以上のイオン交換樹脂の混合イオン交換樹脂を分離する混合イオン交換樹脂の分離塔であって、前記２種以上のイオン交換樹脂のうち平均粒径が最も小さいイオン交換樹脂の平均粒径の９０％以下の網目のスクリーンを分離塔の上部に設置し、該分離塔の底部に注水部を有するとともに前記スクリーンの上側に排出部を有する、混合イオン交換樹脂の分離塔を提供する（発明１）。 In view of the above object, the present invention firstly provides a mixed ion exchange resin separation column for separating a mixed ion exchange resin of two or more ion exchange resins, wherein the average particle size of the two or more ion exchange resins A mesh screen having an average particle size of 90% or less of the ion exchange resin with the smallest diameter is installed at the top of the separation tower, and a water inlet is provided at the bottom of the separation tower and an outlet is provided above the screen. Mixing A separation column for ion exchange resin is provided (Invention 1).

かかる発明（発明１）によれば、アニオン交換樹脂とカチオン交換樹脂などを混合した混合イオン交換樹脂における各イオン交換樹脂の分離精度を向上させることができる。これは以下のような作用による。すなわち、混合イオン交換樹脂の各イオン交換樹脂を比重分離しても分離精度に限界がある要因について本発明者らが検討した結果、混合イオン交換樹脂を再利用するためには、上向流で通水して比重差による沈降速度の違いを利用して分離するのが一般的であるが、破砕した樹脂が多く含まれる場合、破砕した樹脂は沈降速度が変化するため、必ずしも比重分離できないためであることがわかった。そこで、分離塔の上側に使用する樹脂よりも小さい孔径のスクリーンを設け、分離塔に上向流で通水することにより、破砕した細かな樹脂はスクリーンを抜けるが、通常の樹脂はスクリーンによりとどまるようにすることで、分離塔上部の排出部から破砕したイオン交換樹脂のみを排出することができ、これにより混合樹脂の分離精度を向上させることができる。 According to this invention (invention 1), it is possible to improve the separation accuracy of each ion exchange resin in a mixed ion exchange resin in which an anion exchange resin and a cation exchange resin are mixed. This is due to the following effects. That is, as a result of investigation by the present inventors on the factors that limit the separation accuracy even if each ion exchange resin of the mixed ion exchange resin is separated by specific gravity, it was found that in order to reuse the mixed ion exchange resin, an upward flow It is common to separate by passing water and using the difference in sedimentation speed due to the difference in specific gravity, but if there is a lot of crushed resin, the sedimentation speed of the crushed resin will change, so it is not always possible to separate by specific gravity. It turned out to be Therefore, by installing a screen with a pore size smaller than the resin used on the upper side of the separation tower and passing water through the separation tower in an upward flow, the finely crushed resin passes through the screen, but ordinary resin is retained by the screen. By doing so, it is possible to discharge only the crushed ion-exchange resin from the discharge section at the top of the separation tower, thereby improving the separation accuracy of the mixed resin.

上記発明（発明１）においては、前記２種以上のイオン交換樹脂の混合イオン交換樹脂が、少なくともアニオン交換樹脂及びカチオン交換樹脂をそれぞれ１種類以上含むことが好ましい（発明２）。 In the above invention (invention 1), the mixed ion exchange resin of two or more ion exchange resins preferably contains at least one kind of anion exchange resin and one kind or more of cation exchange resin (invention 2).

かかる発明（発明２）によれば、アニオン交換樹脂及びカチオン交換樹脂との混合樹脂は汎用的に用いられており、両者は比重の相違を利用して分離しやすいので発明１の分離塔を適用するのに好適である。 According to this invention (invention 2), mixed resins of anion exchange resin and cation exchange resin are used for general purposes, and the separation tower of invention 1 is applied because they are easy to separate by utilizing the difference in specific gravity. It is suitable for

上記発明（発明２）においては、前記混合イオン交換樹脂の分離塔が上部にアニオン交換樹脂抜出部を有するとともに該アニオン交換樹脂抜出部よりも下方にカチオン交換樹脂抜出部を有することが好ましい（発明３）。 In the above invention (Invention 2), the separation tower for the mixed ion exchange resin may have an anion exchange resin outlet at the top and a cation exchange resin outlet below the anion exchange resin outlet. Preferred (invention 3).

かかる発明（発明３）によれば、一般にアニオン交換樹脂とカチオン交換樹脂とでは、アニオン交換樹脂の方が比重は小さいので、破砕した樹脂を除去して比重分離した際にはアニオン交換樹脂は上側にカチオン交換樹脂は下側に沈降する。そこで、の後、上側のアニオン交換樹脂抜出部からアニオン交換樹脂を、下側のカチオン交換樹脂抜出部からカチオン交換樹脂をそれぞれ精度よく取り出すことができる。 According to this invention (invention 3), since the anion exchange resin generally has a smaller specific gravity than the cation exchange resin, when the crushed resin is removed and the specific gravity is separated, the anion exchange resin is on the upper side. The cation exchange resin settles to the bottom. Therefore, the anion-exchange resin can be taken out from the upper anion-exchange resin extraction part and the cation-exchange resin can be taken out from the lower cation-exchange resin extraction part with high accuracy.

また、本発明は第二に、２種以上のイオン交換樹脂の混合イオン交換樹脂を分離する混合イオン交換樹脂の分離塔の上部に該２種以上のイオン交換樹脂の混合イオン交換樹脂のうち平均粒径が最も小さいイオン交換樹脂の平均粒径の９０％以下の網目のスクリーンを設置し、該分離塔の底部に注水部を有するとともに前記スクリーンの上側に外部に連通した排出部を有する混合イオン交換樹脂の分離塔に使用済の前記２種以上のイオン交換樹脂の混合イオン交換樹脂を充填し、前記注水部より上向流で通水して破損した使用済のイオン交換樹脂を排出部より外部に排出した後、残存する複数の使用済のイオン交換樹脂を分離する、混合イオン交換樹脂の分離方法を提供する（発明４）。 Secondly, in the present invention, an average of the mixed ion exchange resins of two or more kinds of ion exchange resins is placed in the upper part of the mixed ion exchange resin separation tower for separating the mixed ion exchange resins of two or more kinds of ion exchange resins. A mixed ion having a screen having a mesh size of 90% or less of the average particle size of the ion exchange resin having the smallest particle size, having a water inlet at the bottom of the separation column and an outlet communicating with the outside above the screen. The exchange resin separation column is filled with the used mixed ion exchange resin of the above-mentioned two or more ion exchange resins, and the used ion exchange resin that has been damaged by passing water upward from the water injection part is removed from the discharge part. Provided is a method for separating a mixed ion exchange resin, which separates a plurality of remaining used ion exchange resins after being discharged to the outside (Invention 4).

かかる発明（発明４）によれば、分離塔の上側に使用する樹脂よりも小さい孔径のスクリーンを設け、上向流で通水することにより、破損していない通常の樹脂はスクリーン下部にとどまり、破砕した細かな樹脂のみがスクリーンを抜けるので、分離塔上部の排出部から破砕した樹脂を排出した後、複数種のイオン交換樹脂を比重分離することことで分離精度を向上させることができる。 According to this invention (invention 4), a screen having a pore size smaller than that of the resin used is provided on the upper side of the separation tower, and water is passed in an upward flow, so that the normal resin that is not damaged remains at the bottom of the screen, Since only the finely crushed resin passes through the screen, separation accuracy can be improved by discharging the crushed resin from the discharge section at the top of the separation tower and then separating the multiple types of ion exchange resins by specific gravity.

上記発明（発明４）においては、前記２種以上のイオン交換樹脂の混合イオン交換樹脂が、少なくともアニオン交換樹脂及びカチオン交換樹脂をそれぞれ１種類以上含むことが好ましい（発明５）。 In the above invention (invention 4), the mixed ion exchange resin of two or more ion exchange resins preferably contains at least one anion exchange resin and one or more cation exchange resins (invention 5).

かかる発明（発明５）によれば、アニオン交換樹脂及びカチオン交換樹脂との混合樹脂は汎用的に用いられており、両者は比重の相違を利用して分離しやすいので発明１の分離塔を適用するのに好適である。 According to this invention (invention 5), the mixed resin of an anion exchange resin and a cation exchange resin is used for general purposes, and the two are easily separated by utilizing the difference in specific gravity, so the separation tower of invention 1 is applied. It is suitable for

上記発明（発明４，５）においては、前記平均粒径が最も小さいイオン交換樹脂の平均粒径が５０～２０００μｍであることが好ましい（発明６）。特に上記発明（発明４～６）においては、前記２種以上のイオン交換樹脂の混合イオン交換樹脂が、ポーラス型イオン交換樹脂であることが好ましい（発明７）。 In the above inventions (Inventions 4 and 5), it is preferable that the ion exchange resin having the smallest average particle diameter has an average particle diameter of 50 to 2000 μm (Invention 6). In particular, in the above inventions (inventions 4 to 6), the mixed ion exchange resin of two or more ion exchange resins is preferably a porous ion exchange resin (invention 7).

かかる発明（発明６，７）によれば、平均粒径が最も小さいイオン交換樹脂の平均粒径をこのような範囲とすることで、破砕した樹脂を平均粒径９０％以下の網目のスクリーンから好適に分離することができる。 According to such inventions (inventions 6 and 7), by setting the average particle size of the ion exchange resin having the smallest average particle size in such a range, the crushed resin is separated from the mesh screen having an average particle size of 90% or less. can be preferably separated.

上記発明（発明４～７）においては、前記上向流での通水が、早い通水速度で所定時間通水する工程とそれより遅い通水速度で所定時間通水する工程とを１セットとして、その通水を１セット以上繰り返すことが好ましい（発明８）。 In the above inventions (inventions 4 to 7), the upward flow of water comprises a step of passing water at a high water passing speed for a predetermined time and a step of passing water at a slower water passing speed for a predetermined time. As such, it is preferable to repeat the water passage for one or more sets (Invention 8).

かかる発明（発明８）によれば、混合イオン交換樹脂の分離塔に上向流で通水する際の通水速度に緩急をつけることにより混合イオン交換樹脂の攪拌効果が生じ、この攪拌効果により破砕したイオン交換樹脂が上部に舞い上がるので、破砕した細かな樹脂を分離塔上部の排出部からより確実に効率よく排出することができる。 According to this invention (invention 8), the mixing effect of the mixed ion-exchange resin is produced by adjusting the speed of the water flow when the water is passed through the separation tower of the mixed ion-exchange resin in an upward flow. Since the crushed ion-exchange resin floats upward, the finely crushed resin can be more reliably and efficiently discharged from the discharge section at the top of the separation tower.

本発明の混合イオン交換樹脂の分離塔によれば、２種以上のイオン交換樹脂の混合イオン交換樹脂のうち平均粒径が最も小さいイオン交換樹脂の平均粒径の９０％以下の網目のスクリーンを分離塔の上部に設置しているので、破砕した細かな樹脂はスクリーンを抜けるが、通常の樹脂はスクリーン下部にとどまるようにすることで、分離塔上部の排出部から破砕した樹脂のみを排出することができ、これにより混合樹脂の分離精度を向上させることができる。 According to the mixed ion-exchange resin separation tower of the present invention, a mesh screen having an average particle size of 90% or less of the average particle size of the ion-exchange resin having the smallest average particle size among the mixed ion-exchange resins of two or more types of ion-exchange resins is used. Since it is installed at the top of the separation tower, finely crushed resin passes through the screen, but normal resin stays at the bottom of the screen, so that only the crushed resin is discharged from the discharge part at the top of the separation tower. Therefore, it is possible to improve the separation accuracy of the mixed resin.

本発明の一実施形態による混合イオン交換樹脂の分離塔を示す概略図である。1 is a schematic diagram illustrating a separation column for mixed ion exchange resins according to one embodiment of the present invention; FIG. 前記実施形態による混合イオン交換樹脂の分離塔による逆洗工程を示す概略図である。FIG. 4 is a schematic view showing a backwashing process by a separation tower for mixed ion exchange resins according to the embodiment; 前記実施形態による混合イオン交換樹脂の分離塔による逆洗工程を示す拡大図である。FIG. 4 is an enlarged view showing a backwashing process by a separation tower for mixed ion exchange resins according to the embodiment; 比較例１（従来）の混合イオン交換樹脂の分離塔を示す概略図である。It is a schematic diagram showing a separation tower of mixed ion exchange resin of Comparative Example 1 (conventional).

以下、本発明の混合イオン交換樹脂の分離塔の一実施形態について添付図面を参照にして詳細に説明する。 An embodiment of the mixed ion exchange resin separation column of the present invention will be described in detail below with reference to the accompanying drawings.

〔混合イオン交換樹脂の分離塔〕
図１は、本発明の一実施形態による混合イオン交換樹脂の分離塔を示している。図１において、混合イオン交換樹脂の分離塔１は、円筒形の分離塔本体１Ａの底部に注水部としての給水管２及び複数の吐出ノズル２Ａが設けられていて、頂部には排出部としての排出管３が接続している。この分離塔本体１Ａの吐出ノズル２Ａの上側には集水板４が配置されているとともに、分離塔本体１Ａの上端側にはスクリーン５が配置されている。なお、分離塔１内の上下方向の中間付近にはアニオン交換樹脂抜出部（図示せず）が設けられ、それよりも下方にカチオン交換樹脂抜出部（図示せず）が設けられている。また、分離塔１の底部には注排水口が設けられているとともに、側面上側には使用済みの混合樹脂の充填口や覗き窓などが設けられているが、これらは説明の便宜上省略する。 [Separation Tower for Mixed Ion Exchange Resin]
FIG. 1 shows a separation column for mixed ion exchange resins according to one embodiment of the present invention. In FIG. 1, a separation tower 1 for mixed ion exchange resin is provided with a water supply pipe 2 as a water injection part and a plurality of discharge nozzles 2A at the bottom of a cylindrical separation tower main body 1A, and a discharge part at the top. A discharge pipe 3 is connected. A water collecting plate 4 is arranged above the discharge nozzle 2A of the separation tower main body 1A, and a screen 5 is arranged on the upper end side of the separation tower main body 1A. An anion exchange resin extraction part (not shown) is provided near the middle of the separation tower 1 in the vertical direction, and a cation exchange resin extraction part (not shown) is provided below it. . The bottom of the separation tower 1 is provided with an inlet/outlet port, and the upper side of the separation tower 1 is provided with a filling port for used mixed resin, a viewing window, and the like, but these are omitted for convenience of explanation.

そして、分離塔本体１Ａの集水板４とスクリーン５との間の空間には、約４０～７０容積％を占める程度に使用済の混合イオン交換樹脂が充填される。本実施形態において混合イオン交換樹脂は、アニオン交換樹脂及びカチオン交換樹脂の混合樹脂である。この混合イオン交換樹脂におけるアニオン交換樹脂及びカチオン交換樹脂の割合（容積比）は、特に制限はないがアニオン交樹脂：カチオン交換樹脂＝３０：７０～７０：３０程度である。また、これらアニオン交樹脂及びカチオン交換樹脂の平均粒径は小さい方のイオン交換樹脂で平均粒径が５０～２０００μｍ（膨潤時基準）であることが好ましい。さらには、アニオン交樹脂及びカチオン交換樹脂は、ポーラス型イオン交換樹脂であることが好ましい。なお、前述したアニオン交換樹脂抜出部とカチオン交換樹脂抜出部とは、この混合イオン交換樹脂の充填量（容積）と、アニオン交換樹脂及びカチオン交換樹脂の割合と、安全率とに応じてそれぞれの樹脂抜出位置が設定される。 The space between the water collecting plate 4 and the screen 5 of the separation tower main body 1A is filled with the used mixed ion exchange resin to the extent that it occupies about 40 to 70% by volume. The mixed ion exchange resin in this embodiment is a mixed resin of an anion exchange resin and a cation exchange resin. The ratio (volume ratio) of the anion exchange resin and the cation exchange resin in this mixed ion exchange resin is not particularly limited, but the anion exchange resin: cation exchange resin is about 30:70 to 70:30. In addition, it is preferable that the average particle size of the smaller ion exchange resin of these anion exchange resin and cation exchange resin is 50 to 2000 μm (based on swelling). Furthermore, the anion exchange resin and the cation exchange resin are preferably porous ion exchange resins. The above-mentioned anion exchange resin extraction part and cation exchange resin extraction part are selected according to the filling amount (volume) of the mixed ion exchange resin, the ratio of the anion exchange resin and the cation exchange resin, and the safety factor. Each resin extraction position is set.

上述したような混合イオン交換樹脂の分離塔１において、スクリーン５は、アニオン交換樹脂及びカチオン交換樹脂のうち平均粒径が小さい方のイオン交換樹脂の平均粒径（膨潤時基準）の９０％以下の網目であり、特に７０～９０％である。スクリーン５の網目が平均粒径の９０％を超えると、後述する逆洗工程において、正常なイオン交換樹脂が排出されやすくなる一方、７０％より小さいと破砕した樹脂の除去率が十分でなくなる。 In the mixed ion exchange resin separation tower 1 as described above, the screen 5 is 90% or less of the average particle size (based on swelling) of the ion exchange resin having the smaller average particle size among the anion exchange resin and the cation exchange resin. mesh, especially 70-90%. If the mesh size of the screen 5 exceeds 90% of the average particle size, normal ion-exchange resin is likely to be discharged in the backwashing process described later.

〔混合イオン交換樹脂の分離方法〕
次に前述したような構成を有する本実施形態の混合イオン交換樹脂の分離塔１を用いた混合イオン交換樹脂の分離方法について説明する。 [Method for separating mixed ion exchange resin]
Next, a method for separating a mixed ion-exchange resin using the mixed ion-exchange resin separation tower 1 of the present embodiment having the above-described configuration will be described.

まず、混床式イオン交換装置内に充填されている使用済の混合イオン交換樹脂Ｒを取り出して、混合イオン交換樹脂の分離塔１に充填口から充填する。そして、分離塔１の底部の注排水口から水（純水）を注入して分離塔１内を水で満たす。 First, the used mixed ion exchange resin R packed in the mixed bed ion exchange apparatus is taken out, and the mixed ion exchange resin separation column 1 is filled from the packing port. Then, water (pure water) is injected from the inlet/outlet at the bottom of the separation tower 1 to fill the inside of the separation tower 1 with water.

次に逆洗工程として、複数の吐出ノズル２Ａから水（純水）を吐出して上向流で通水し、使用済みのイオン交換樹脂Ｒを逆洗する。このとき図２に示すように混合イオン交換樹脂Ｒは、集水板４とスクリーン５との間の空間の約４０～７０容積％を占めているので、集水板４とスクリーン５との間の空間全体に拡散する。このとき図３に示すように水の吐出圧により流動床化したアニオン交換樹脂Ａ及びカチオン交換樹脂Ｃがスクリーン５に向けて流動するが、スクリーン５は、平均粒径が小さい方のイオン交換樹脂の平均粒径（膨潤時基準）の９０％以下の網目であるので、正常なイオン交換樹脂はスクリーン５を透過せず、破損して短径が小さくなったイオン交換樹脂のみがスクリーン５を通過して排出管３から排出される。 Next, as a backwashing step, water (pure water) is discharged from a plurality of discharge nozzles 2A and passed upward to wash the used ion exchange resin R backwash. At this time, as shown in FIG. 2, the mixed ion exchange resin R occupies about 40 to 70% by volume of the space between the water collecting plate 4 and the screen 5, so that the space between the water collecting plate 4 and the screen 5 spread throughout the space. At this time, as shown in FIG. 3, the fluidized anion exchange resin A and cation exchange resin C flow toward the screen 5 due to the discharge pressure of water. Since the mesh size is 90% or less of the average particle size (standard when swollen), normal ion-exchange resin does not pass through the screen 5, and only the ion-exchange resin that has been damaged and has a smaller minor axis passes through the screen 5. Then, it is discharged from the discharge pipe 3.

この上向流での逆洗工程の時間は、長い方が破砕したイオン交換樹脂が除去できて好ましいが、長すぎるとかえって作業効率が低下するため、３０分～１２０分程度とするのが好ましい。特に、上述したような逆洗時間において、上向流での逆洗を例えばＬＶ１０ｍ／ｈ～２０ｍ／ｈ程度の早い通水速度と、例えばＬＶ３ｍ／ｈ～１０ｍ／ｈ未満の遅い通水速度とを１セットとして、その通水を１セット、特に２セット以上繰り返すことが好ましい。このように上向流で通水する際の通水速度に緩急をつけることにより、攪拌効果により破砕したイオン交換樹脂が上部に舞い上がるので、破砕した細かな樹脂を分離塔１の上部の排出管３からより確実に効率よく排出することができる。 The time of the backwashing step in this upward flow is preferably longer because the crushed ion exchange resin can be removed, but if it is too long, the work efficiency will rather decrease, so it is preferably about 30 to 120 minutes. . In particular, in the backwashing time as described above, the backwashing in the upward flow is performed at a high water flow rate of, for example, LV 10 m / h to 20 m / h and a slow water flow rate of, for example, LV 3 m / h to less than 10 m / h. is one set, and it is preferable to repeat the water passage for one set, particularly two or more sets. Since the crushed ion-exchange resin floats up due to the stirring effect by adjusting the speed of water passage when water is passed upward in this way, the crushed fine resin is discharged into the discharge pipe at the top of the separation tower 1. 3 can be more reliably and efficiently discharged.

このようにして、逆洗により破砕したイオン交換樹脂を排出したら、静置することで残存する正常なイオン交換樹脂Ｒは沈降する。このときアニオン交換樹脂とカチオン交換樹脂とは比重が異なるので比重分離することができる。一般にカチオン交換樹脂の方が比重は大きいので、アニオン交換樹脂が下側でカチオン交換樹脂が上側に沈降する。なお、逆洗後、底部に設けた注排水口から純水の排出、注入を行って、公知の方法によりイオン交換樹脂の分離工程を別途行ってもよい。そして、分離したアニオン交換樹脂及びカチオン交換樹脂は、アニオン交換樹脂抜出部とカチオン交換樹脂抜出部からそれぞれ抜き出して、それぞれの樹脂の再生塔により再生工程を行えばよい。なお、アニオン交換樹脂及びカチオン交換樹脂の分離精度の向上のために安全率を考慮してアニオン交換樹脂及びカチオン交換樹脂の分離境界から所定の範囲の樹脂は分離せず残存させるのが好ましいが。この残存させたイオン交換樹脂は、取り出して次回のアニオン交換樹脂とカチオン交換樹脂の混合樹脂の分離時に利用すればよい。 In this way, after the ion exchange resin crushed by backwashing is discharged, the remaining normal ion exchange resin R settles by allowing it to stand still. At this time, since the anion exchange resin and the cation exchange resin have different specific gravities, they can be separated by specific gravity. Since the cation exchange resin generally has a higher specific gravity, the anion exchange resin settles on the lower side and the cation exchange resin settles on the upper side. After backwashing, the ion exchange resin may be separated by a known method by discharging and injecting pure water from a water inlet provided at the bottom. Then, the separated anion-exchange resin and cation-exchange resin may be extracted from the anion-exchange resin extractor and the cation-exchange resin extractor, respectively, and subjected to the regeneration process in the respective resin regeneration towers. In order to improve the separation accuracy of the anion-exchange resin and the cation-exchange resin, it is preferable to leave the resin in a predetermined range from the separation boundary of the anion-exchange resin and the cation-exchange resin without separating in consideration of the safety factor. The remaining ion-exchange resin may be taken out and used for the next separation of the mixed resin of the anion-exchange resin and the cation-exchange resin.

以上、本発明について添付図面を参照にして前記実施形態に基づき説明してきたが、本発明は前記実施形態に限定されず、種々の変更実施が可能である。例えば、前記実施形態においては、アニオン交換樹脂とカチオン交換樹脂の２種類の樹脂の場合について説明したが、異なるグレードあるいは性状のアニオン交換樹脂とカチオン交換樹脂を複数種用いた場合にも適用可能である。さらに本発明において、イオン交換樹脂とは、アニオン交換樹脂及びカチオン交換樹脂に限らず、これらのイオン交換樹脂に触媒金属を担持させた触媒樹脂や、ホウ素選択制吸着樹脂なども含む。また、本発明は、複数種の混合イオン交換樹脂を分離するに際し、事前に破砕したイオン交換樹脂を排除することを特徴とするものであり、その後の分離工程については特に制限はなく、公知の種々の分離方法に適用できることはいうまでもない。 As described above, the present invention has been described based on the above-described embodiments with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments, and various modifications can be made. For example, in the above embodiment, two types of resins, an anion exchange resin and a cation exchange resin, are used, but the present invention can also be applied to a case where a plurality of anion exchange resins and cation exchange resins of different grades or properties are used. be. Furthermore, in the present invention, ion exchange resins are not limited to anion exchange resins and cation exchange resins, but also include catalyst resins in which catalyst metals are supported on these ion exchange resins, boron selective adsorption resins, and the like. In addition, the present invention is characterized in that the pre-crushed ion-exchange resin is excluded when separating a plurality of mixed ion-exchange resins, and the subsequent separation step is not particularly limited. Needless to say, it can be applied to various separation methods.

以下の具体的実施例により本発明をさらに詳細に説明する。 The following specific examples further illustrate the invention.

［実施例１］
図１に示すイオン交換樹脂の分離塔１に、アニオン交換樹脂とカチオン交換樹脂との混合樹脂（アニオン交換樹脂：カチオン交換樹脂＝５０：５０（容積比））を２ｍ３充填し、上向流でＬＶ１５ｍ／ｈで１時間通水した。通水停止後、分離したアニオン交換樹脂とカチオン交換樹脂をそれぞれ抜き取って他のイオン交換樹脂の混入率を測定した。その結果、アニオン交換樹脂中のカチオン交換樹脂およびカチオン交換樹脂中のアニオン交換樹脂の混入率はそれぞれ０．０１％であった。また、１時間の通水時に分離塔から排水槽に流入した健全な樹脂量を確認した結果、分離塔１からの健全な樹脂の損失割合は０％であった。これらの結果を逆洗条件とともに表１に示す。 [Example 1]
The ion exchange resin separation tower 1 shown in FIG. was passed at LV 15 m/h for 1 hour. After stopping the flow of water, the separated anion exchange resin and cation exchange resin were each taken out, and the mixing rate of other ion exchange resins was measured. As a result, the mixing rate of the cation exchange resin in the anion exchange resin and the anion exchange resin in the cation exchange resin was 0.01%, respectively. Also, as a result of checking the amount of healthy resin that flowed into the wastewater tank from the separation tower during one hour of water flow, the rate of loss of sound resin from the separation tower 1 was 0%. These results are shown in Table 1 together with the backwash conditions.

［実施例２］
図１に示すイオン交換樹脂の分離塔１に、アニオン交換樹脂とカチオン交換樹脂との混合樹脂（アニオン交換樹脂：カチオン交換樹脂＝５０：５０（容積比））を２ｍ３充填し、上向流でＬＶ１５ｍ／ｈで１５分通水し、その後ＬＶ５ｍ／ｈで１５分通水するサイクルを２回繰り返した。通水停止後、分離したアニオン交換樹脂とカチオン交換樹脂をそれぞれ抜き取って他のイオン交換樹脂の混入率を測定した。その結果、アニオン交換樹脂中のカチオン交換樹脂およびカチオン交換樹脂中のアニオン交換樹脂の混入率はそれぞれ０．００５％であった。また、１時間の通水時に分離塔１から排水槽に流入した健全な樹脂量を確認した結果、分離塔からの健全な樹脂の損失割合はお０％であった。これらの結果を逆洗条件とともに表１にあわせて示す。 [Example 2]
The ion exchange resin separation tower 1 shown in FIG. A cycle of passing water at LV 15 m/h for 15 minutes and then passing water at LV 5 m/h for 15 minutes was repeated twice. After stopping the flow of water, the separated anion exchange resin and cation exchange resin were each taken out, and the mixing rate of other ion exchange resins was measured. As a result, the mixing ratio of the cation exchange resin in the anion exchange resin and the anion exchange resin in the cation exchange resin was 0.005%, respectively. Also, as a result of checking the amount of healthy resin that flowed into the waste water tank from the separation tower 1 during one hour of water flow, the rate of loss of sound resin from the separation tower was 0%. These results are shown in Table 1 together with the backwashing conditions.

［比較例１］
図４に示すようにスクリーン５を有しない混合イオン交換樹脂の分離塔１に、アニオン交換樹脂とカチオン交換樹脂の混合樹脂（アニオン交換樹脂：カチオン交換樹脂＝５０：５０（容積比））を２ｍ３充填し、上向流でＬＶ５ｍ／ｈで１時間通水した。通水停止後、分離したアニオン交換樹脂とカチオン交換樹脂をそれぞれ抜き取って混入率を測定した。その結果、アニオン交換樹脂中のカチオン交換樹脂およびカチオン交換樹脂中のアニオン交換樹脂の混入率はそれぞれ０．１％であった。また、１時間の通水時に分離塔１から排水槽に流入した健全な樹脂量を確認した結果、分離塔からの健全な樹脂の損失割合は０％であった。 [Comparative Example 1]
As shown in FIG. 4, 2 m of a mixed resin of anion exchange resin and cation exchange resin (anion exchange resin: cation exchange resin = 50:50 (volume ratio)) is placed in a mixed ion exchange resin separation tower 1 without a screen 5. 3 , and water was passed for 1 hour at LV 5 m/h in an upward flow. After stopping the flow of water, the separated anion exchange resin and cation exchange resin were each taken out and the mixing rate was measured. As a result, the mixing rate of the cation exchange resin in the anion exchange resin and the anion exchange resin in the cation exchange resin were each 0.1%. As a result of confirming the amount of healthy resin that flowed into the waste water tank from the separation tower 1 during one hour of water flow, the rate of loss of sound resin from the separation tower was 0%.

［比較例２］
図４に示すようにスクリーン５を有しない混合イオン交換樹脂の分離塔１に、アニオン交換樹脂とカチオン交換樹脂との混合樹脂（アニオン交換樹脂：カチオン交換樹脂＝５０：５０（容積比））を２ｍ３充填し、上向流でＬＶ１５ｍ／ｈで１時間通水した。通水停止後、分離したアニオン交換樹脂とカチオン交換樹脂をそれぞれ抜き取って混入率を測定した。その結果、アニオン交換樹脂中のカチオン交換樹脂およびカチオン交換樹脂中のアニオン交換樹脂の混入率はそれぞれ０．２％であった。また、１時間の通水時に分離塔から排水槽に流入した健全な樹脂量を確認した結果、分離塔１からの健全な樹脂の損失割合は１０％であった
[Comparative Example 2]
As shown in FIG. 4, a mixed resin of an anion exchange resin and a cation exchange resin (anion exchange resin: cation exchange resin=50:50 (volume ratio)) is placed in a mixed ion exchange resin separation tower 1 that does not have a screen 5. It was filled with 2 m 3 and water was passed for 1 hour at LV 15 m/h in an upward flow. After stopping the flow of water, the separated anion exchange resin and cation exchange resin were each taken out and the mixing rate was measured. As a result, the mixing rate of the cation exchange resin in the anion exchange resin and the anion exchange resin in the cation exchange resin was 0.2%, respectively. In addition, as a result of confirming the amount of healthy resin that flowed into the waste water tank from the separation tower during one hour of water flow, the loss ratio of healthy resin from the separation tower 1 was 10%.

Figure 0007184152000002
Figure 0007184152000002

１ 混合イオン交換樹脂の分離塔１
１Ａ 分離塔本体
２ 給水管
２Ａ 吐出ノズル
３ 排出管
４ 集水板
５ スクリーン
Ｒ 混合イオン交換樹脂
Ａ アニオン交換樹脂
Ｃ カチオン交換樹脂 1 Mixed ion exchange resin separation tower 1
1A Separation tower main body 2 Water supply pipe 2A Discharge nozzle 3 Discharge pipe 4 Water collecting plate 5 Screen R Mixed ion exchange resin A Anion exchange resin C Cation exchange resin

Claims (8)

２種以上のイオン交換樹脂の混合イオン交換樹脂を分離する混合イオン交換樹脂の分離塔であって、
前記２種以上のイオン交換樹脂のうち平均粒径が最も小さいイオン交換樹脂の平均粒径の９０％以下の網目のスクリーンを分離塔の上部に設置し、
該分離塔の底部に注水部を有するとともに前記スクリーンの上側に排出部を有する、混合イオン交換樹脂の分離塔。 A mixed ion exchange resin separation column for separating a mixed ion exchange resin of two or more ion exchange resins,
A mesh screen having an average particle size of 90% or less of the average particle size of the ion exchange resin having the smallest average particle size among the two or more ion exchange resins is installed at the top of the separation tower,
A mixed ion exchange resin separation tower having a water inlet at the bottom of said separation tower and a discharge above said screen. 前記２種以上のイオン交換樹脂の混合イオン交換樹脂が、少なくともアニオン交換樹脂及びカチオン交換樹脂をそれぞれ１種類以上含む、請求項１に記載の混合イオン交換樹脂の分離塔。 2. The mixed ion exchange resin separation tower according to claim 1, wherein said mixed ion exchange resin of said two or more ion exchange resins contains at least one kind of anion exchange resin and one kind or more of cation exchange resin. 前記混合イオン交換樹脂の分離塔が上部にアニオン交換樹脂抜出部を有するとともに該アニオン交換樹脂抜出部よりも下方にカチオン交換樹脂抜出部を有する、請求項２に記載の混合イオン交換樹脂の分離塔。 3. The mixed ion exchange resin according to claim 2, wherein the mixed ion exchange resin separation tower has an anion exchange resin withdrawal at the top and a cation exchange resin withdrawal below the anion exchange resin withdrawal. separation tower. ２種以上のイオン交換樹脂の混合イオン交換樹脂を分離する混合イオン交換樹脂の分離塔の上部に該２種以上のイオン交換樹脂の混合イオン交換樹脂のうち平均粒径が最も小さいイオン交換樹脂の平均粒径の９０％以下の網目のスクリーンを設置し、該分離塔の底部に注水部を有するとともに前記スクリーンの上側に外部に連通した排出部を有する混合イオン交換樹脂の分離塔に使用済の前記２種以上のイオン交換樹脂の混合イオン交換樹脂を充填し、
前記注水部より上向流で通水して破損した使用済のイオン交換樹脂を排出部より外部に排出した後、残存する複数の使用済のイオン交換樹脂を分離する、混合イオン交換樹脂の分離方法。 An ion-exchange resin having the smallest average particle diameter among the mixed ion-exchange resins of two or more kinds of ion-exchange resins is placed in the upper part of the mixed ion-exchange resin separation tower for separating the mixed ion-exchange resin of two or more kinds of ion-exchange resins. A used mixed ion-exchange resin separation tower is equipped with a mesh screen having an average particle size of 90% or less, and has a water inlet at the bottom of the separation tower and an outlet communicating with the outside above the screen. Filling the mixed ion exchange resin of the two or more ion exchange resins,
Separation of mixed ion-exchange resin, wherein after the used ion-exchange resin that has been damaged by the upward flow of water from the water injection part is discharged to the outside from the discharge part, a plurality of remaining used ion-exchange resins are separated. Method. 前記２種以上のイオン交換樹脂の混合イオン交換樹脂が、少なくともアニオン交換樹脂及びカチオン交換樹脂をそれぞれ１種類以上含む、請求項４に記載の混合イオン交換樹脂の分離方法。 5. The method for separating a mixed ion exchange resin according to claim 4, wherein the mixed ion exchange resin of the two or more ion exchange resins contains at least one kind of anion exchange resin and one or more kinds of cation exchange resin. 前記平均粒径が最も小さいイオン交換樹脂の平均粒径が５０～２０００μｍである、請求項４又は５に記載の混合イオン交換樹脂の分離方法。 6. The method for separating mixed ion exchange resins according to claim 4 or 5, wherein the ion exchange resin having the smallest average particle size has an average particle size of 50 to 2000 μm. 前記２種以上のイオン交換樹脂の混合イオン交換樹脂が、ポーラス型イオン交換樹脂である、請求項４～６のいずれか１項に記載の混合イオン交換樹脂の分離方法。 The method for separating a mixed ion-exchange resin according to any one of claims 4 to 6, wherein the mixed ion-exchange resin of two or more ion-exchange resins is a porous ion-exchange resin. 前記上向流での通水が、早い通水速度で所定時間通水する工程とそれより遅い通水速度で所定時間通水する工程とを１セットとして、その通水を１セット以上繰り返す、請求項４～７のいずれか１項に記載の混合イオン交換樹脂の分離方法。 In the upward flow, a step of passing water at a high water passing speed for a predetermined time and a step of passing water at a slower water passing speed for a predetermined time are set as one set, and the water passing is repeated for one or more sets. The method for separating mixed ion exchange resins according to any one of claims 4 to 7.
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