JPS6142336A - Regeneration of powdery anion exchange resin - Google Patents

Regeneration of powdery anion exchange resin

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Publication number
JPS6142336A
JPS6142336A JP16552084A JP16552084A JPS6142336A JP S6142336 A JPS6142336 A JP S6142336A JP 16552084 A JP16552084 A JP 16552084A JP 16552084 A JP16552084 A JP 16552084A JP S6142336 A JPS6142336 A JP S6142336A
Authority
JP
Japan
Prior art keywords
anion exchange
exchange resin
resin
powdered
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP16552084A
Other languages
Japanese (ja)
Inventor
Koji Kawasaki
川崎 耕治
Fumio Maekawa
文男 前川
Mitsutoshi Hirasawa
平沢 光利
Mitsuru Nakano
満 中野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ITOCHU SEITO KK
Original Assignee
ITOCHU SEITO KK
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ITOCHU SEITO KK filed Critical ITOCHU SEITO KK
Priority to JP16552084A priority Critical patent/JPS6142336A/en
Publication of JPS6142336A publication Critical patent/JPS6142336A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To eliminate a problem such as the increase in running cost or the disposal of a used resin, by contacting a powdery anion exchange resin adsorbing a substance to be adsorbed with a heated aqueous acid solution to enable the reuse of the powdery anion exchange resin. CONSTITUTION:A powdery anion exchange resin with a particle size of 250mum or less, which was used in the purification of a solution containing a coloring matter component or suspended substance to adsrob a substance to be adsorbed, is contacted with a 0.1'5% aqueous acid solution (e.g., a hydrochloric acid solution) heated to 40 deg.C or more. At first, said anion exchange resin is contacted with the 0.1-5% aqueous acid solution heated to 40 deg.C or more while the treated resin is washed with a 0.1-1% alkaline aqueous solution (e.g., a NaOH solution). By this method, regeneration can be simply performed and the reuse of the powdery anion exchange resin is enabled and a problem such as the increase in running cost or the disposal of a used resin can be eliminated.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、コロイド物質及び懸濁物質等の濁質物を中心
とする不純物を含み高色価に着色される溶液の色素成分
並びに濁質物の除去に使用された粉末状陰イオン交換樹
脂の再生方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention is directed to the pigment components of solutions that are colored with high color values and which contain impurities mainly turbid substances such as colloidal substances and suspended solids, as well as the turbid substances. This invention relates to a method for regenerating powdered anion exchange resin used for removal.

〔従来の技術〕[Conventional technology]

従来、陰イオン交換樹脂が脱塩ばかりでなく脱色にも有
効であることが知られており、例えば精製糖工業におい
て脱色工程等で利用されている。
It has been known that anion exchange resins are effective not only for desalination but also for decolorization, and are used, for example, in the decolorization process in the sugar refining industry.

そして、その使用態様としては、一般に粒径が0.3〜
0.6mmの粒状陰イオン交換樹脂を吸着塔内に充填せ
しめ、当該充填層に被処理液を通液して溶液中の色素成
分を吸着せしめるというものが知られている。
In terms of usage, the particle size is generally 0.3~
It is known that an adsorption tower is filled with 0.6 mm granular anion exchange resin, and a liquid to be treated is passed through the packed bed to adsorb a dye component in the solution.

このような充填層に被処理液を通液する方法は単に充填
層に通液するだけであるから操作が比較的簡単であると
いう反面、吸着表面積が小さく吸着速度が遅いので、通
液速度をそれほど速くすることができないという欠点を
有する。このため吸着塔が比較的大きくなり易く、かつ
理論的吸着容量に対する利用率も比較的小さくなってし
まっている。また、被処理液中に濁質物が共存する場合
には、この濁質物が樹脂の母体網目構造を閉塞するため
予めこれを除去する操作が必要である。
This method of passing the liquid to be treated through the packed bed is relatively easy to operate because the liquid is simply passed through the packed bed, but on the other hand, the adsorption surface area is small and the adsorption rate is slow, so the rate of liquid passing must be reduced. It has the disadvantage that it cannot be made very fast. For this reason, the adsorption tower tends to be relatively large, and the utilization rate relative to the theoretical adsorption capacity is also relatively small. Furthermore, if a suspended substance coexists in the liquid to be treated, this suspended substance blocks the matrix network structure of the resin, and therefore it is necessary to remove it in advance.

このような欠点を解決するために、粒状陰イオン交換樹
脂を粉砕して粉末状にすることにより、その吸着表面積
を大きくしてこれを被処理腋と反応させれば、吸着速度
も大幅に増加し、かつ理論的吸着容量に対する利用率も
上昇し、わずかな樹脂量で効果的に脱色することができ
るものと考えた。
In order to solve these drawbacks, the granular anion exchange resin can be pulverized into powder to increase its adsorption surface area and react with the treated armpit, which will greatly increase the adsorption rate. Moreover, the utilization rate relative to the theoretical adsorption capacity increased, and it was thought that effective decolorization could be achieved with a small amount of resin.

本発明者等は、以上のような理由から、粉末状陰イオン
交換樹脂による色素成分の除去について鋭意検討を行な
った結果、上記の利点の外に、粒状陰イオン交換樹脂に
は認められなかった優れた吸着特性を新たに発現するこ
とを知見した。すなはち、低分子色素はもちろんのこと
、560〜720n+sの可視部高波長領域に吸光度特
性を有する高分子色素に対しても特異的に吸着できる能
力を有していること、さらにコロイド物質や懸濁物質等
の濁質物を吸着除去する能力が非常に優れており、粉末
活性炭以上の能力を有していることである。これらの吸
着特性は既存の吸着剤、例えば粉末活性炭、粒状炭、骨
炭、及び粒状陰イオン交換樹脂では見い出されないもの
であり、粉末状陰イオン交換樹脂の優位性を証明するも
のである。
For the reasons mentioned above, the present inventors conducted intensive studies on the removal of pigment components using powdered anion exchange resins, and as a result, in addition to the above advantages, granular anion exchange resins did not have any advantages. It was discovered that this product newly developed excellent adsorption properties. In other words, it has the ability to specifically adsorb not only low-molecular dyes, but also high-molecular dyes that have absorbance characteristics in the visible high wavelength region of 560 to 720 n+s, and it also has the ability to specifically adsorb to colloidal substances and It has an extremely excellent ability to adsorb and remove suspended matter such as suspended solids, and has an ability that exceeds that of powdered activated carbon. These adsorption properties are not found in existing adsorbents such as powdered activated carbon, granular carbon, bone char, and granular anion exchange resins, and prove the superiority of powdered anion exchange resins.

このような知見に基づいて、本願出願人等は、先に特願
昭58−47016号明細書において、粉末状陰イオン
交換樹脂を使用して色素成分を吸着させる液体の脱色方
法を提案した。
Based on such knowledge, the applicants of the present application previously proposed in Japanese Patent Application No. 58-47016 a method of decolorizing a liquid by using a powdered anion exchange resin to adsorb a pigment component.

ところで、一般に粉末状陰イオン交換樹脂に限らずイオ
ン交換樹脂を用いて溶液を脱色処理すると、上記溶液中
に含まれる色素成分等の被吸着物質が蓄積し上記イオン
交換樹脂の活性が低下するという現象が生ずる。そして
、特に上記脱色処理によって活性が低下したイオン交換
樹脂においては、例えば溶剤等で洗浄しても被吸着物質
をほとんど除去することができず活性が元の状態に回復
しないことが知られているので、上記脱色に用いられた
イオン交換樹脂は再利用が困難であるとして使い捨てに
されている。
By the way, it is generally said that when a solution is decolorized using an ion exchange resin, not just a powdered anion exchange resin, adsorbed substances such as pigment components contained in the solution accumulate and the activity of the ion exchange resin decreases. A phenomenon occurs. In particular, it is known that in ion exchange resins whose activity has been reduced by the above-mentioned decolorization treatment, the adsorbed substances can hardly be removed even if the resin is washed with a solvent or the like, and the activity does not return to its original state. Therefore, the ion exchange resin used for the above-mentioned decolorization is discarded because it is difficult to reuse it.

しかしながら、粉末状陰イオン交換樹脂は原材料である
陰イオン交換樹脂自体が高価であるので、非常に高価で
あり、したがって使い捨てで用いるとランニングコスト
が増大し、さらに産業廃棄物である使用済樹脂の処分が
問題となる。特に高色価溶液を処理する場合には上記樹
脂を頻繁に交換しなくてはならないので、上記問題が一
層顕著なものとなっている。
However, powdered anion exchange resins are very expensive because the anion exchange resin itself, which is the raw material, is expensive, and running costs increase when they are used as disposable materials. Disposal becomes an issue. In particular, when processing high color value solutions, the resin must be replaced frequently, making the above problem even more pronounced.

そこで、粉末状陰イオン交換樹脂を再生して使用するこ
とが要望されるが、この粉末状陰イオン交換樹脂の再生
に関してはB、Christina Goodacre
等がSugar Industry Technolo
gist Vol 41(1982) Paper 4
7+でわずかに触れているだけで、その他にはほとんど
見当らない、当報告では、10%塩化ナトリウム溶液を
用いて再生を行なっているが、高分子色素は脱着し難い
ので、予めこれを除去する処理、例えばタロフロック(
Talofloc)処理が必要であるとされており、こ
のため工程が煩雑なものとなってしまっている。
Therefore, it is desired to regenerate and use the powdered anion exchange resin, and regarding the regeneration of this powdered anion exchange resin, please refer to B.Christina Goodacre.
etc. are Sugar Industry Technolo
gist Vol 41 (1982) Paper 4
It is only slightly touched in 7+, and hardly seen in other cases.In this report, regeneration is performed using a 10% sodium chloride solution, but since polymer dyes are difficult to desorb, this must be removed in advance. processing, e.g. Talofloc (
Talofloc) treatment is required, which makes the process complicated.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

そこで本発明は、上述の従来の実情に鑑み提案されたも
のであって、簡単な操作で粉末状陰イオン交換樹脂の再
使用を可能とし、ランニングコストの増大や使用済樹脂
の処分等の問題を解消することが可能な粉末状陰イオン
交換樹脂の再生方法を提供することを目的とする。
Therefore, the present invention has been proposed in view of the above-mentioned conventional situation, and it makes it possible to reuse powdered anion exchange resin with a simple operation, and solves problems such as increased running costs and disposal of used resin. An object of the present invention is to provide a method for regenerating a powdered anion exchange resin that can solve the problem.

〔問題点を解決するための手段〕[Means for solving problems]

本発明者等は、濁質物に富む高色価液を処理して高分子
色素や濁質物等の難脱着性物質により活性が低下した粉
末状陰イオン交換樹脂について数多くの再生処理を試み
詳細に検討を加えた結果、新たな知見を発見し、本発明
を完成するに至ったものである。
The present inventors have attempted and detailed a number of regeneration treatments for powdered anion exchange resins whose activity has been reduced by difficult-to-detach substances such as polymeric dyes and turbid substances by processing high color value liquids rich in turbid substances. As a result of further investigation, new knowledge was discovered and the present invention was completed.

すなわち、本発明に係る粉末状陰イオン交換樹脂の再生
方法は、色素成分及び濁質物を含む溶液を精製し被吸着
物質を吸着した粒径250p以下の粉末状陰イオン交換
樹脂を、40℃以上に加温した0、1〜5%の酸水溶液
と接触させることを特徴とするものであり、さらに、4
0℃以上に加温した0、1〜5%の酸水溶液と接触させ
た後、0.1〜1%のアルカリ性水溶液で洗浄すること
を特徴とするものである。
That is, the method for regenerating a powdered anion exchange resin according to the present invention involves purifying a solution containing a pigment component and a turbid substance, and then purifying a powdered anion exchange resin having a particle size of 250p or less, which has adsorbed the adsorbed substance, at a temperature of 40°C or higher. It is characterized by contacting with a 0.1 to 5% acid aqueous solution heated to 4.
It is characterized in that it is brought into contact with a 0.1 to 5% acid aqueous solution heated to 0° C. or higher, and then washed with a 0.1 to 1% alkaline aqueous solution.

前述したように粉末状陰イオン交換樹脂は優れた吸着特
性として、コロイド物質や懸濁物質等の濁質物及び高分
子色素を吸着除去する能力が優れていることが知られて
いる。そして、粒状樹脂におけるこれまでの通念では、
これらの被吸着物質は樹脂の母体網目構造の内部に捕捉
される、いわゆる物理的吸着されているために、たとえ
再生工程で化学薬品処理されても、脱離され難いと言わ
れていた。
As mentioned above, powdered anion exchange resins are known to have excellent adsorption properties, such as the ability to adsorb and remove turbid substances such as colloidal substances and suspended substances, and polymeric dyes. The conventional wisdom regarding granular resin is that
Since these adsorbed substances are trapped inside the matrix network structure of the resin, so-called physically adsorbed, it is said that they are difficult to desorb even if they are treated with chemicals in the regeneration process.

しかしながら、本発明者等は40℃以上に加温した酸水
溶液を用いると、吸着されている粉末状陰イオン交換樹
脂から、色素成分はもちろんのこと、これまで脱着され
難いと言われていた濁質物さえも容易に脱着されること
を知見した。ここで重要なことは、40℃以上の高温下
でのみ脱着効果が著しく、常温では濁質物はほとんど脱
着されないことである。
However, the present inventors found that when using an acid aqueous solution heated to 40°C or higher, not only the dye component but also the turbidity, which had been said to be difficult to desorb, was removed from the adsorbed powdered anion exchange resin. It has been found that even pledged objects can be easily attached and detached. What is important here is that the desorption effect is significant only at high temperatures of 40° C. or higher, and that suspended matter is hardly desorbed at room temperature.

さらに、上記40℃以上の高温下では、酸濃度が低くて
も、脱着効果がそれほど低下せず、40°C以上に加温
されていれば0.1〜2%程度の稀薄溶液でも高分子色
素や濁質物の脱着が可能であるということも判明した。
Furthermore, at high temperatures above 40°C, even if the acid concentration is low, the desorption effect does not decrease significantly, and if heated above 40°C, even a dilute solution of about 0.1 to 2% can cause polymerization. It was also found that it is possible to desorb pigments and turbid substances.

このように稀薄溶液でも使用可能であるということは、
再生剤の使用量が少なくてすみ、経済的メリットは計り
知れないものがある。また、粒状イオン交換樹脂を用い
た脱色工程において、再生時に生じる稀薄な酸洗水も利
用可能であることは言うまでもない。
The fact that even dilute solutions can be used in this way means that
The amount of regenerating agent used is small, and the economic benefits are immeasurable. Furthermore, it goes without saying that in the decolorization process using a granular ion exchange resin, dilute pickling water generated during regeneration can also be used.

上記再生機構について、その詳細は不明であるが、粉末
状陰イオン交換樹脂による高分子色素や濁質物の吸着機
構がこれまで考えられていた粒状陰イオン交換樹脂によ
る吸着機構と様子を異にしており、酸水溶液との接触に
よって色素成分や濁質物等の被吸着物質が形態的な変化
を受は脱離しやすい形になり、温度を高くすることで促
進されると推測している。
Although the details of the above regeneration mechanism are unknown, the adsorption mechanism of polymeric dyes and suspended substances by powdered anion exchange resin is different from the adsorption mechanism by granular anion exchange resin that was previously thought. It is speculated that upon contact with the acid aqueous solution, adsorbed substances such as pigment components and turbid substances undergo morphological changes to a form in which they are more easily desorbed, and this is promoted by increasing the temperature.

ところで、本発明により再生される粉末状陰イオン交換
樹脂としては、新品の粉末状陰イオン交換樹脂ばかりで
なく、脱色工程や脱塩工程で多サイクル使用してその能
力が低下し使用できなくなり廃棄されるような使用済粉
末状陰イオン交換樹脂であってもよいが、この場合には
新品の樹脂では認められなかった現象が見出された。
By the way, the powdered anion exchange resin that can be recycled according to the present invention is not limited to new powdered anion exchange resins, but also those that have been used multiple times in the decolorization and desalination processes and become unusable and discarded. It is also possible to use a used powdered anion exchange resin such as the one described above, but in this case a phenomenon that was not observed with a new resin was discovered.

すなわち、酸水溶液で再生した粉末状陰イオン交換樹脂
を用いて糖液を処理したところ、上記使用済粉末状強塩
基性陰イオン交換樹脂を用いて処理すると処理糖液のp
Hが4〜5となるのに対して、新品の樹脂で処理すると
処理糖液のpHは7〜8となり、大きな相違が認められ
た。また、本発明者等の実験によれば、処理糖液のpH
と色価との関係を調べてみると、pHの低い処理糖液は
ど脱色率が低く着色が著しいことが分った。
That is, when a sugar solution was treated using a powdered anion exchange resin regenerated with an acid aqueous solution, the p of the treated sugar solution was
H was 4 to 5, whereas when treated with new resin, the pH of the treated sugar solution was 7 to 8, indicating a large difference. Furthermore, according to the experiments conducted by the present inventors, the pH of the treated sugar solution
When we investigated the relationship between sugar solution and color value, we found that treated sugar solutions with low pH had a low decolorization rate and significant coloration.

精製糖工場では、糖液のpHが低いと、その後の濃縮、
結晶工程における糖の加水分解が生じ、大きな問題とな
る。
In refined sugar factories, if the pH of the sugar solution is low, subsequent concentration,
Hydrolysis of sugars occurs during the crystallization process, which poses a major problem.

そこで、特に上記使用済粉末状強塩基性陰イオン交換樹
脂を用いた場合のpHの低下を解決するために種々検討
したところ、上記酸水溶液と接触した後に、稀薄なアル
カリ性水溶液、例えば00IN(0,4%)水酸化ナト
リウム水溶液で洗浄するだけで処理糖液のpHは8〜9
となり、色価も大幅に低くなり、再生効果が著しく向上
することが判明した。
Therefore, we conducted various studies in order to solve the problem of pH decrease especially when using the used powdered strong basic anion exchange resin, and found that after contacting with the acid aqueous solution, a dilute alkaline aqueous solution, for example 0IN (0IN), was used. , 4%) The pH of the treated sugar solution can be adjusted to 8-9 by simply washing with aqueous sodium hydroxide solution.
It was found that the color value was significantly lowered and the reproduction effect was significantly improved.

上記アルカリ洗浄によって処理糖液の品質が良くなる理
由としては、未だ明らかではないが、例えば使用済粉末
状強塩基性陰イオン交換樹脂は新品樹脂とは異なり強塩
基性及び弱塩基性交換基(強塩基性交換基が酸化を受は
弱塩基化したもの。
The reason why the above alkaline washing improves the quality of the treated sugar solution is not yet clear. A strongly basic exchange group that undergoes oxidation to become a weak base.

)が混在しているために、酸水溶液処理後、アルカリ洗
浄すると再生効率の良い弱塩基性交換基が優先的にOH
形になり、一部の強塩基性交換基もOH形になるために
、処理糖液のpHが上昇し色価も低くなることが考えら
れる。
), so when alkali washing is performed after acid aqueous solution treatment, weakly basic exchange groups with good regeneration efficiency are preferentially converted to OH.
It is thought that the pH of the treated sugar solution increases and the color value decreases because some of the strongly basic exchange groups also become OH-type.

このアルカリ洗浄処理は、同様に新品の粉末状陰イオン
交換樹脂並びに使用済粉末状中塩基性あるいは弱塩基性
陰イオン交換樹脂を酸水溶液で再生したあとに用いても
、再生効果は良くなり、処理糖液の色価も低くなる。
Even if this alkaline cleaning treatment is used after regenerating a new powdered anion exchange resin or a used powdered medium basic or weakly basic anion exchange resin with an acid aqueous solution, the regeneration effect will be improved. The color value of the treated sugar solution also becomes lower.

本発明に用いられる酸水溶液としては、通常0.1〜5
重量%程度の水溶液であり、40℃以上に加温されるこ
とが必要である。
The acid aqueous solution used in the present invention is usually 0.1 to 5
It is an aqueous solution of about 40% by weight, and needs to be heated to 40°C or higher.

上記酸水溶液に使用される酸としては、塩酸、硫酸、硝
酸、リン酸、蟻酸、酢酸等が挙げられるが、塩酸等の鉱
酸を用いた方が効果が高い。
Examples of acids used in the acid aqueous solution include hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid, and acetic acid, but the use of mineral acids such as hydrochloric acid is more effective.

最も好ましくは、先ず40℃以上に加温された低濃度(
例えば0.1〜2%)の酸水溶液と接触させ、続いて稀
薄(例えば0.1〜1%)なアルカリ性水溶液と接触さ
せることである。
Most preferably, the low concentration (
For example, 0.1-2%) is brought into contact with an acid aqueous solution, followed by contact with a dilute (for example 0.1-1%) alkaline aqueous solution.

上記アルカリ性水溶液に使用されるアルカリとしては、
水酸化ナトリウム、水酸化カリウム、水酸化リチウム、
アンモニア水等が挙げられ、さらにこのアルカリ性水溶
液には塩化ナトリウム等の塩類を加えてもよい。特に、
水酸化ナトリウム含有食塩が効果が高い。さらに、粒状
イオン交換樹脂を用いた脱色工程において、アルカリに
よる再生操作時に生じる稀薄なアルカリ廃水等も利用可
能である。
The alkalis used in the above alkaline aqueous solution include:
Sodium hydroxide, potassium hydroxide, lithium hydroxide,
Examples include aqueous ammonia, and salts such as sodium chloride may be added to this alkaline aqueous solution. especially,
Salt containing sodium hydroxide is highly effective. Furthermore, in the decolorization process using a granular ion exchange resin, dilute alkaline wastewater etc. generated during the regeneration operation with alkali can also be used.

本発明に用いられる粉末状陰イオン交換樹脂としては、
スチレンとジビニルベンゼンの共重合物あるいはアクリ
ルとジビニルベンゼンの共重合物などの母体に第4級ア
ンモニウム基、アルカノール基、第3級アミン基、第2
級アミン基、第1級アミン基、ポリアミン基などの強塩
基性基、中塩基性基、弱塩基性基などのイオン交換基を
有する強塩基性陰イオン交換樹脂、中塩基性陰イオン交
換樹脂、弱塩基性陰イオン交換樹脂などが挙げられ、そ
のイオン形もOH形の外、CI形、SO形などの各種の
塩形のものが挙げられるが、特に、精製糖工程の糖液に
対してはCI形強塩基性陰イオン交換樹脂が最も効果的
である。一方、上記弱塩基性陰イオン交換樹脂は、脱着
性に優れているので、例えば甘蔗糖液や甜菜糖液等の高
色価の溶液に対しての効果が大きい。
The powdered anion exchange resin used in the present invention includes:
Quaternary ammonium groups, alkanol groups, tertiary amine groups, secondary
Strong basic anion exchange resins and medium basic anion exchange resins having ion exchange groups such as strong basic groups such as primary amine groups, primary amine groups, and polyamine groups, medium basic groups, and weak basic groups. , weakly basic anion exchange resins, etc., and their ionic forms include various salt forms such as OH form, CI form, and SO form. CI type strongly basic anion exchange resin is the most effective. On the other hand, since the weakly basic anion exchange resin has excellent desorption properties, it is highly effective for solutions with high color values such as cane sugar solution and beet sugar solution.

上記粉末状陰イオン交換樹脂の粒径としては、250に
以下であることが好ましく、より好ましくは100弘以
下である。上記粒径が250p以上であると色素成分を
中心とする被吸着物質の脱離が難かしくなり、再生する
ことが困難なものとなる。また、上記粉末状陰イオン交
換樹脂の粒径が5pL以下、特にリークの危険性が大き
い1.5ル以下のものであるとる別が困難なものとなり
処理溶液中に樹脂が混入してしまう虞がある。
The particle size of the powdered anion exchange resin is preferably less than 250 mm, more preferably less than 100 mm. If the particle size is 250p or more, it becomes difficult to remove adsorbed substances, mainly dye components, and it becomes difficult to regenerate. In addition, if the particle size of the powdered anion exchange resin is 5 pL or less, especially 1.5 μL or less, which has a high risk of leakage, it will be difficult to separate, and there is a risk that the resin will be mixed into the processing solution. There is.

上記粉末状陰イオン交換樹脂の製法としては、粒状陰イ
オン交換樹脂を粉砕する方法や、工業的に合成する方法
等が挙げられるが、粉砕によるのが一般的である。また
、その粉砕方法としても、気流式粉砕法や凍結粉砕法、
機械的粉砕法等が挙げられるが、特に気流式粉砕法か凍
結粉砕法を用いることが好ましい。
Methods for producing the powdered anion exchange resin include a method of pulverizing a granular anion exchange resin and a method of industrial synthesis, but pulverization is generally used. In addition, the pulverization methods include air flow pulverization method, freeze pulverization method,
Mechanical pulverization methods may be used, but it is particularly preferable to use a pneumatic pulverization method or a freeze pulverization method.

上記気流式粉砕法は、空気の高速渦流による高周波な圧
力変動にともなう振動により原料である粒子状陰イオン
交換樹脂を自己破砕させ微粒子化させる方法であり、5
0#L以下に粉末化するのに要する時間が極めて短時間
(数秒程度)であるという特徴を有している。そしてこ
の粉砕方法によれば、粉砕時の温度上昇が40℃以下で
あるので熱による樹脂の劣化が生ずることがなく、さら
に特徴的なことは色素成分等の脱着性に優れ再生効果が
大きな粉末状陰イオン交換樹脂が得られることである。
The above-mentioned pneumatic pulverization method is a method in which the particulate anion exchange resin, which is a raw material, is self-pulverized into fine particles by vibrations caused by high-frequency pressure fluctuations caused by high-speed vortex flow of air.
It has the characteristic that the time required to powder it to 0 #L or less is extremely short (about several seconds). According to this pulverization method, the temperature rise during pulverization is 40°C or less, so there is no deterioration of the resin due to heat.What is more distinctive is that the powder has excellent desorption properties for pigment components and has a large regeneration effect. An anion exchange resin having a similar shape can be obtained.

また、上記凍結粉砕法は、粒状の陰イオン交換樹脂に、
例えば液体窒素を直接接触させて一100′C以下に冷
却せしめ、次いで冷却した当該陰イオン交換樹脂をただ
ちにハンマーミル等で粉末化するものである。なお、上
記冷却に使用できる冷媒としては、上記液体窒素の外に
液体炭酸ガス、液体酸素、液化プロパン等各種の低沸点
液化ガスが挙げられるが、冷却温度が低いことおよび安
全性、経済性の面で液体窒素を用いることが好ましい。
In addition, the above-mentioned freeze-pulverization method uses granular anion exchange resin to
For example, the resin is cooled to below -100'C by direct contact with liquid nitrogen, and then the cooled anion exchange resin is immediately pulverized using a hammer mill or the like. In addition to the above-mentioned liquid nitrogen, refrigerants that can be used for the above-mentioned cooling include various low-boiling point liquefied gases such as liquid carbon dioxide, liquid oxygen, and liquefied propane. Preferably, liquid nitrogen is used on the surface.

この場合にも熱劣化の生じることがなく細かい粒度で、
かつ粒子径が比較的揃った粉末状陰イオン交換樹脂が得
られる。
In this case too, there is no thermal deterioration and the particle size is fine.
Moreover, a powdered anion exchange resin having a relatively uniform particle size can be obtained.

これに対し、ボールミルやハンマーミルを用いた機械的
粉砕方法では、粉砕物の粒度を揃えることが難かしく、
得られた粉末状陰イオン交換樹脂を使用するにあたって
は、ふるい等で5〜250終のものを選別して用いるこ
とが好ましい、さらに、上記機械的粉砕方法では粉砕に
要する時間が長く温度上昇も大きいので、当該粉末状陰
イオン交換樹脂の脱色性能が低下する虞れもある。
On the other hand, with mechanical grinding methods using ball mills or hammer mills, it is difficult to make the particle size of the ground material uniform.
When using the obtained powdered anion exchange resin, it is preferable to use a sieve or the like to select those with a particle size of 5 to 250.Furthermore, the mechanical pulverization method described above takes a long time to pulverize and causes a rise in temperature. Since it is large, there is a possibility that the decolorizing performance of the powdered anion exchange resin may be reduced.

陰イオン交換樹脂はその耐熱温度が比較的低く、例えば
4級アンモニウム基をイオン交換基とするOH形強塩基
性陰イオン交換樹脂の最高操作温度は60℃とされてお
り、当該温度を越えると急速にイオン交換基の熱分解が
生じる。陰イオン交換樹脂による色素成分の吸着機構の
詳細については不明であるが、陰イオン交換樹脂粒子表
面の極性が大いに関与しているものと考えられるので、
その粉砕時に熱が加わるのは好ましくない。
Anion exchange resins have a relatively low heat resistance temperature. For example, the maximum operating temperature of OH type strongly basic anion exchange resins with quaternary ammonium groups as ion exchange groups is 60°C, and if this temperature is exceeded, Thermal decomposition of the ion exchange groups occurs rapidly. Although the details of the adsorption mechanism of dye components by anion exchange resin are unknown, it is thought that the polarity of the anion exchange resin particle surface is largely involved.
It is undesirable that heat is applied during the grinding.

本発明に用いられる粉末状陰イオン交換樹脂の使用態様
としては、バッチ方式、カラム方式ともに適用できる。
The powdered anion exchange resin used in the present invention can be used in both a batch method and a column method.

さらに多段接触方式または粉末樹脂層方式を採用するこ
とにより、使用量を大幅に減少することができるととも
に、処理液は極めて清澄なものを得ることができる等、
非常に効果的である。
Furthermore, by adopting a multi-stage contact method or a powder resin layer method, the amount used can be significantly reduced, and the processing liquid can be extremely clear.
Very effective.

多段接触方式とは、例えば第1図に示すように、粉末状
陰イオン交換樹脂を充填した粉末樹脂カラムを複数、こ
の例では4系列作成し、うち3系列は3段脱色システム
とするとともに1系列は再生塔とし順次再生操作を実施
する、いわゆるメリーゴーランド方式のようなものであ
り、効率的な処理が可能である。
For example, as shown in Fig. 1, the multi-stage contact system means that a plurality of powder resin columns filled with powdered anion exchange resin, four series in this example, are created, three of which are a three-stage decolorization system, and one The series is like a so-called merry-go-round system in which regeneration towers are used to sequentially perform regeneration operations, and efficient processing is possible.

粉末樹脂層方式とは、粉末状陰イオン交換樹脂とケイソ
ウ士、繊維状ろ過助剤(例えば、ガラス繊維、セルロー
ス繊維、活性炭繊維等)等とを混合使用して、通常のろ
過機にプレコート層を形成するような、あるいはろ過板
のように成型したものを用いるような方式である。この
粉末樹脂層方式によれば、圧力損失や水力学的性能等を
大幅に改善することが可能で、精製操作が著しく容易に
なり、そのうえ使用した粉末状陰イオン交換樹脂が漏出
する危険が全くなくなる。
The powdered resin layer method uses a mixture of powdered anion exchange resin, diatomaceous material, fibrous filter aids (e.g., glass fiber, cellulose fiber, activated carbon fiber, etc.), and adds a precoat layer to a regular filter. This method uses a molded filter plate, or a molded filter plate. According to this powder resin layer method, it is possible to significantly improve pressure drop and hydraulic performance, etc., and the purification operation is significantly easier. Moreover, there is no risk of leakage of the powdered anion exchange resin used. It disappears.

本発明は、コロイド物質や懸濁物質等の濁質物及び色素
成分を含む溶液の精製に使用した粉末状陰イオン交換樹
脂であれば如何なるものであっても適用可能であるが、
特に甘蔗糖液や甜菜糖液等の各種糖液、各種植物搾汁、
パルブ工場廃液、食品工場排水等の脱色及び脱コロイド
に使用した粉末状陰イオン交換樹脂に適用した場合に効
果が大きい。
The present invention can be applied to any powdered anion exchange resin used for purifying solutions containing turbid substances such as colloidal substances and suspended substances and pigment components.
In particular, various sugar solutions such as cane sugar solution and beet sugar solution, various plant juices,
It is highly effective when applied to powdered anion exchange resins used for decolorizing and decolloiding pulp factory wastewater, food factory wastewater, etc.

〔作用〕[Effect]

以上述べたように、色素成分や濁質物の除去により吸着
能力が低下した粉末状陰イオン交換樹脂を、40℃に加
温した酸水溶液で処理することにより、あるいは先ず4
0℃に加温した酸水溶液で処理し続いてアルカリ性水溶
液で洗浄することにより、上記粉末状陰イオン交換樹脂
に吸着される色素成分や濁質物が速やかに除去され再生
される。
As mentioned above, powdered anion exchange resin whose adsorption capacity has decreased due to the removal of pigment components and turbid substances can be treated with an acid aqueous solution heated to 40°C or
By treating with an acid aqueous solution heated to 0° C. and then washing with an alkaline aqueous solution, the pigment components and suspended matter adsorbed on the powdered anion exchange resin are quickly removed and regenerated.

〔実施例〕〔Example〕

以下、具体的な実施例により本発明を説明するが、本発
明がこれら実施例に限定されるものでないことは言うま
でもないことである。
The present invention will be explained below with reference to specific examples, but it goes without saying that the present invention is not limited to these examples.

実施例1゜ 粉末状強塩基性陰イオン交換樹脂(ローム・アンドφハ
ース社製、商品名アンバーライ)IRA−401)を気
流粉砕法にて粒径50弘以下(平均粒径18.5g)に
粉砕した粉末状陰イオン交換樹脂1g(乾燥重量)を精
製糖工場の炭酸飽充工程終了後の精製中間糖液(転化糖
0.15%。
Example 1 Powdered strongly basic anion exchange resin (manufactured by Rohm & φ Haas Co., Ltd., trade name Amberly IRA-401) was crushed to a particle size of 50 hiro or less (average particle size 18.5 g) by air pulverization method. 1 g (dry weight) of powdered anion exchange resin pulverized into a refined intermediate sugar solution (0.15% invert sugar) after the carbonation process at a refined sugar factory.

Bx61.O,pH8,0,透過度T二88.1%9色
価指数A、I 、750)300mlに加え60°Cで
60分間混合攪拌し、色素成分や11AI!I物を吸着
させた。吸着終了後、メンブランフィルタ−(東洋ろ紙
製 3ル)を用いて上記粉末状陰イオン交換樹脂をろ別
し、水洗後回収してジャケット付カラム内に移した。
Bx61. O, pH 8.0, transmittance T2 88.1% 9 Color value index A, I, 750) 300 ml and mixed and stirred at 60°C for 60 minutes to remove pigment components and 11AI! I was adsorbed. After the adsorption was completed, the powdered anion exchange resin was filtered using a membrane filter (Toyo Roshi Co., Ltd. 3L), washed with water, collected, and transferred into a jacketed column.

この色素成分等を吸着した粉末状陰イオン交換樹脂カラ
ムを各種温度に保温した後、1%塩酸水溶液200m1
を通薬し、流出してくる再生排液をpH7に中和して3
001に希釈した。
After keeping the powdered anion exchange resin column adsorbed with this dye component etc. at various temperatures, 200ml of 1% aqueous hydrochloric acid solution was added.
Pass the medicine through, neutralize the regenerated wastewater that flows out to pH 7, and
It was diluted to 0.001.

この排液について420〜720nmの吸光度を測定し
各波長における吸着色素量に対する色素脱着率を求めた
。結果を第1表に示す。
The absorbance of this waste liquid was measured at 420 to 720 nm, and the dye desorption rate relative to the amount of adsorbed dye at each wavelength was determined. The results are shown in Table 1.

なお、上記色素脱着率は次式より求めた。The above dye desorption rate was determined from the following formula.

0.0.、、:粉末樹脂被処理糖液の吸光度0.0−:
粉末樹脂処理糖液の吸光度 0.0:再生排液の吸光度 ■、:再生排液の量(■1) ■、:粉末樹脂処理糖液量(1) W  :粉末樹脂乾燥重量(g) b  =セルの長さくcm) 第1表 この第1表より、塩醜水溶液処理温度が40℃を越える
と、420〜720nmの広範囲で色素脱着率が大幅に
向上していることが分る。
0.0. ,,: Absorbance of sugar solution to be treated with powder resin 0.0-:
Absorbance of powdered resin-treated sugar solution 0.0: Absorbance of regenerated effluent ■,: Amount of regenerated effluent (■1) ■,: Amount of powdered resin-treated sugar solution (1) W: Dry weight of powdered resin (g) b =Cell length cm) Table 1 From Table 1, it can be seen that when the salt aqueous solution treatment temperature exceeds 40°C, the dye desorption rate is significantly improved over a wide range of 420 to 720 nm.

実施例2゜ 先の実施例1と同様に調製した粉末状強塩基性陰イオン
交換樹脂1g(乾燥重量)を用い、実施例1と同様の方
法により精製中間糖液を脱色した後、第2表に示す再生
剤を2001用いて60℃の温度条件で再生した。各再
生剤による色素脱着率を第2表に示す。
Example 2 Using 1 g (dry weight) of a powdered strongly basic anion exchange resin prepared in the same manner as in Example 1, a purified intermediate sugar solution was decolorized in the same manner as in Example 1, and then a second Regeneration was performed at a temperature of 60° C. using the regenerant 2001 shown in the table. Table 2 shows the dye desorption rate by each regenerant.

第2表 この第2表より、塩酸水溶液及び塩酸含有水溶液を用い
ることにより、560〜720nmの可視部高波長領域
での色素脱着率が著しく高くなることが分る。
Table 2 From this Table 2, it can be seen that by using an aqueous hydrochloric acid solution or an aqueous solution containing hydrochloric acid, the dye desorption rate in the visible high wavelength region of 560 to 720 nm is significantly increased.

実施例3゜ 粒状強塩基性陰イオン交換樹脂(ローム・アンド争ハー
ス社製、商品名アンバーライトI RA−401)をボ
ールミルにて粉砕し第3表に示すような粒度分布を有す
る粉末状陰イオン交換樹脂を篩分法により調製した。
Example 3 A granular strongly basic anion exchange resin (manufactured by Rohm & Haas Co., Ltd., trade name Amberlite I RA-401) was ground in a ball mill to obtain a powdery anion having a particle size distribution as shown in Table 3. Ion exchange resin was prepared by sieving method.

これら各粒度分布を有する粉末状陰イオン交換樹脂1g
(乾燥重量)を、先の実施例1と同様に精製中間糖液を
脱色した後、1%塩酸水溶液を200m1用いて60℃
の温度条件で再生した。
1g of powdered anion exchange resin having each of these particle size distributions
(dry weight), after decolorizing the purified intermediate sugar solution in the same manner as in Example 1, using 200 ml of 1% aqueous hydrochloric acid solution at 60°C.
It was regenerated under the following temperature conditions.

再生剤による色素脱着率並びに処理糖液の脱色率及び透
過度を第3表に示す。
Table 3 shows the dye desorption rate by the regenerant and the decolorization rate and transmittance of the treated sugar solution.

なお、色価指数及び脱色率はそれぞれ下記の式から求め
た。
Note that the color value index and decolorization rate were determined from the following formulas.

Xc ” D4%g、’被検試料(1) p Hを7.0 ±
0.1 ニ調整後、4201層における吸光度 b  =セルの長さくcm) C・被検試料中の固形物重量(g/ml)また、透過度
(濁度)は、被検試料のpHを7.0±0.1に調整し
たのち5cmのセルを用いて720nmにおける透過率
(T%)で表わした。
Xc ” D4%g, 'Test sample (1) pH 7.0 ±
0.1 After adjustment, absorbance b in the 4201 layer = cell length cm) C. Weight of solids in the test sample (g/ml) In addition, the transmittance (turbidity) depends on the pH of the test sample. After adjusting to 7.0±0.1, it was expressed as transmittance (T%) at 720 nm using a 5 cm cell.

この第3表より、粒径分布が250pm以下、特に21
0μm以下では、処理糖液の脱色率及び透過度が良好で
あるとともに、再生処理による色素脱着率が420nm
〜720r+mの広範囲で高いことが分る。
From Table 3, it is clear that the particle size distribution is 250 pm or less, especially 21
At 0 μm or less, the decolorization rate and transmittance of the treated sugar solution are good, and the dye desorption rate by regeneration treatment is 420 nm.
It can be seen that it is high over a wide range of ~720r+m.

実施例4゜ 甘蔗糖液の精製イオン交換樹脂工程に使用して能力の低
下した使用済粒状強塩基性陰イオン交換樹脂(三菱化成
社製、商品名FA−308)を気流粉砕法にて粒径50
膳以下(平均粒径19.3μ)に粉砕して得られた使用
済粉末状陰イオン交換樹脂(強塩基交換容量1 、 O
meq/g 、弱塩基交換容量0.7meq/g) 2
g (乾燥重量)と実施例1で調製した新品粉末状陰イ
オン交換樹脂(強塩基交換容量0 、7meq/呂)I
g(乾燥重量)とを用いて先の実施例1と同様に精製中
間糖液を脱色した後、各樹脂について1%塩酸水溶液2
001を用いて60℃の温度条件で再生した。さらに、
必要に応じてl/1 ON水酸化ナトリウム水溶液を5
01通薬した。
Example 4: Purification of cane sugar liquid A used granular strongly basic anion exchange resin (manufactured by Mitsubishi Kasei Corporation, trade name FA-308), whose capacity has decreased due to use in the ion exchange resin process, is granulated by an air flow pulverization method. Diameter 50
Used powdered anion exchange resin (strong base exchange capacity 1,000
meq/g, weak base exchange capacity 0.7 meq/g) 2
g (dry weight) and the new powdered anion exchange resin prepared in Example 1 (strong base exchange capacity 0, 7 meq/lot) I
g (dry weight) to decolorize the purified intermediate sugar solution in the same manner as in Example 1, and then add 1% aqueous hydrochloric acid solution to each resin.
001 at a temperature of 60°C. moreover,
If necessary, add 5 l/1 ON sodium hydroxide aqueous solution.
I took 01 medicines.

2に れらの再生後の粉末状陰イオン交換樹脂に対して、原料
糖(タイ産50%、キューバ産50%、還元糖0.82
%、灰分0.37%、色価指数A、l5270)を木に
溶解後、炭酸飽充法を実施し、ろ過した清澄液(Bx6
3、pH7,7、転化糖0.71%、透過度T″’TI
Dpm79’ 3%1色価指数A、I2380)を30
01添加し、60℃で60分間混合攪拌した後、ガラス
ファイバーフィルタ(GBlooR)を用いてろ過した
。
2. Raw sugar (50% from Thailand, 50% from Cuba, reducing sugar 0.82%) was added to the regenerated powdered anion exchange resin.
%, ash content 0.37%, color index A, 15270) was dissolved in wood, the carbonation method was carried out, and the filtered clear liquid (Bx6
3, pH 7.7, invert sugar 0.71%, permeability T''TI
Dpm79' 3%1 Color value index A, I2380) 30
After mixing and stirring at 60° C. for 60 minutes, the mixture was filtered using a glass fiber filter (GBlooR).

処理糖液の品質を第4表に示す。The quality of the treated sugar solution is shown in Table 4.

この第4表より、NaOH洗浄を行なうと、処理糖液の
色価が無処理に比べて新品樹脂で30%、使用済樹脂で
は45%程度低下することが分る。
From Table 4, it can be seen that when NaOH washing is performed, the color value of the treated sugar solution decreases by about 30% for new resin and 45% for used resin, compared to when no treatment is performed.

実施例5゜ 粒状強塩基性陰イオン交換樹脂(IRA−401)、粒
状弱塩基性陰イオン交換樹脂(WA−30、三菱化成社
製)及び粒状弱酸性陽イオン交換樹脂(WK−11,三
菱化成社製)の各樹脂を気流粉砕法にて粒径50p、以
下に粉砕して粉末状イオン交換樹脂を調製した。
Example 5 Particulate strongly basic anion exchange resin (IRA-401), particulate weakly basic anion exchange resin (WA-30, manufactured by Mitsubishi Chemical Corporation), and particulate weakly acidic cation exchange resin (WK-11, Mitsubishi Chemical Corporation) Powdered ion exchange resins were prepared by pulverizing each resin (manufactured by Kasei Co., Ltd.) to a particle size of 50p or less using an air flow pulverization method.

沖縄より入荷した砂糖さび(収穫後約7日間経過)を試
験用圧搾機で搾り、得られた搾汁を100℃に加熱した
後石灰乳を加えてpH7,0〜7.2とするホットライ
ミング法で清浄した後、ろ過して清澄液(Bxll、8
、pH7,6、透過度T”l″79.7%1色価指数A
、117000、見掛純糖率84 、4)を得た。
Hot liming: Sugar cane imported from Okinawa (approximately 7 days after harvest) is squeezed using a test press, the resulting squeezed juice is heated to 100°C, and then milk of lime is added to adjust the pH to 7.0 to 7.2. After cleaning by method, filter and clear liquid (Bxll, 8
, pH 7.6, Transmittance T"l" 79.7%1 Color value index A
, 117,000 and an apparent pure sugar rate of 84.4).

一方、第5表に示すように粉末状イオン交換樹脂者1g
(乾燥重量)にガラス繊維及びケイソウ土を混合してジ
ャケット付カラム(2c+mφXIOcm)に充填し、
また粒状イオン交換樹脂は湿潤状態で各41(乾燥重量
1gに相当する)を同様に充填した。
On the other hand, as shown in Table 5, 1 g of powdered ion exchange resin
(dry weight) mixed with glass fiber and diatomaceous earth and packed into a jacketed column (2c+mφXIOcm),
Further, 41 pieces of granular ion exchange resin (corresponding to 1 g of dry weight) each were filled in the same manner in a wet state.

これらの樹脂カラムを70℃に保温して上記清澄液20
01を1時間当り301のスピードで通液した。水洗後
、1%塩酸水溶液を200m1通薬して流出してくる再
生排液をpH7に中和して400m1に希釈した。処理
糖液の品質及び再生剤による色素脱着率を第5表に示す
。
These resin columns were kept warm at 70°C and the clarified liquid 20
01 was passed at a rate of 301 per hour. After washing with water, 200 ml of 1% aqueous hydrochloric acid solution was passed through to neutralize the regenerated effluent that flowed out to pH 7 and dilute it to 400 ml. Table 5 shows the quality of the treated sugar solution and the dye desorption rate by the regenerant.

この第5表において、560nIl〜720n11の高
波長領域での色素脱着率が粉末樹脂では100%以上と
なっていることは、被処理糖液中の可溶性非糖分が粉末
樹脂により吸着されて純情率が上昇し、本発明による再
生方法によって脱着することを示している。
In Table 5, the fact that the dye desorption rate in the high wavelength region of 560nIl to 720n11 is more than 100% for the powdered resin means that the soluble non-sugar content in the sugar solution to be treated is adsorbed by the powdered resin. increases, indicating that it is desorbed by the regeneration method according to the present invention.

実施例6゜ 実施例4で調製した使用済粉末状陰イオン交換樹脂を実
施例1で用いた精製中間糖液に懸濁させ1%懸濁糖液(
10g乾燥重量/l糖液)を調製した。
Example 6゜The used powdered anion exchange resin prepared in Example 4 was suspended in the purified intermediate sugar solution used in Example 1 to make a 1% suspended sugar solution (
10g dry weight/l sugar solution) was prepared.

さらに、必要に応じてケイソウ±(中央シリカ社製、シ
リカ−600H)及びガラスtal& (富士ファイバ
ーグラス社製、ガラスチョツプドストランドカット長6
■、フィラメント径to、5g)を0.2〜0.5%添
加した。
Furthermore, if necessary, diatomaceous material ± (manufactured by Chuo Silica Co., Ltd., Silica-600H) and glass tal& (manufactured by Fuji Fiberglass Co., Ltd., glass chopped strand cut length 6
2, filament diameter to, 5 g) was added in an amount of 0.2 to 0.5%.

ろ材として東洋ろ紙No、2を装着したミリポア製ろ過
器(ろ過面積10c■、容量340 ml)に、上記懸
濁糖液2501を混合しながら注ぎ込んだ後、70℃の
恒温槽内に浸漬し、I Kg/cmの圧空で加圧し、定
圧ろ過を行なった。
The suspended sugar solution 2501 was mixed and poured into a Millipore filter (filtration area 10 cm, capacity 340 ml) equipped with Toyo Filter Paper No. 2 as a filter medium, and then immersed in a constant temperature bath at 70°C. Constant pressure filtration was performed under pressure of I kg/cm.

ろ過量とろ適時間を測定し、さらに清澄ろ液について7
20nmにおける透過率を求めた。結果を¥p6表に示
す。
Measure the filtration amount and appropriate filtration time, and also check the clear filtrate.
Transmittance at 20 nm was determined. The results are shown in Table ¥p6.

〔発明の効果〕〔Effect of the invention〕

上述の説明からも明らかなように、本発明によれば、色
素成分や濁質物の除去により吸着能力が低下した粉末状
陰イオン交換樹脂を、40℃に加温した酸水溶液で処理
することにより、あるいは先ず40℃に加温した酸水溶
液で処理し続いてアルカリ性水溶液で洗浄することによ
り簡単に再生することが可能となり、したがってこの粉
末状陰イオン交換樹脂を繰り返し使用することが可能と
なるので、経済的メリットは極めて大きく、また産業廃
棄物の量が著しく減少するので処理労力や公害等の観点
からも好ましい。
As is clear from the above description, according to the present invention, a powdered anion exchange resin whose adsorption capacity has been reduced due to the removal of pigment components and turbid substances is treated with an acid aqueous solution heated to 40°C. Alternatively, it can be easily regenerated by first treating with an acid aqueous solution heated to 40°C and then washing with an alkaline aqueous solution, thus making it possible to use this powdered anion exchange resin repeatedly. , the economic merit is extremely large, and the amount of industrial waste is significantly reduced, which is preferable from the viewpoint of processing labor and pollution.

特に、40℃以上に加温した低濃度の酸水溶液(例えば
061〜2%塩酸溶液)処理、続いて稀薄なアルカリ性
水溶液(例えばO,lN水酸化ナトリウム溶液)による
洗浄により、使用済みの粒状陰イオン交換樹脂より調製
した使用済粉末状陰イオン交換樹脂、そのなかでも特に
粉末状弱塩基性陰イオン交換樹脂を繰り返し使用でき、
且つ従来適用不可能な甘蔗糖汁及び甜菜糖汁に代表され
る高色価、高コロイド及び懸濁物質含有溶液の精製にま
で粉末状陰イオン交換樹脂の応用範囲が拡大したことに
よる効果は甚大である。
In particular, used granular anhydride is treated with a low concentration acid aqueous solution (e.g. 061-2% hydrochloric acid solution) heated to 40°C or above, followed by washing with a dilute alkaline aqueous solution (e.g. O, IN sodium hydroxide solution). Used powdered anion exchange resins prepared from ion exchange resins, especially powdered weakly basic anion exchange resins, can be used repeatedly.
Furthermore, the scope of application of powdered anion exchange resins has expanded to include the purification of solutions with high color values, high colloids, and suspended solids, such as cane sugar juice and sugar beet juice, which were previously unapplicable. It is.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は多段接触方式の具体的構成の一例を示す模式図
である。
FIG. 1 is a schematic diagram showing an example of a specific configuration of the multi-stage contact method.

Claims (2)

【特許請求の範囲】[Claims] (1)色素成分及び濁質物を含む溶液を精製し被吸着物
質を吸着した粒径250μ以下の粉末状陰イオン交換樹
脂を、40℃以上に加温した0.1〜5%の酸水溶液と
接触させることを特徴とする粉末状陰イオン交換樹脂の
再生方法。
(1) A powdered anion exchange resin with a particle size of 250μ or less, which has been purified from a solution containing a pigment component and a suspended substance and has adsorbed the adsorbed substance, is mixed with a 0.1 to 5% acid aqueous solution heated to 40°C or higher. A method for regenerating a powdered anion exchange resin, the method comprising contacting the resin.
(2)色素成分及び濁質物を含む溶液を精製し被吸着物
質を吸着した粒径250μ以下の粉末状陰イオン交換樹
脂を、40℃以上に加温した0.1〜5%の酸水溶液と
接触させた後、0.1〜1%のアルカリ性水溶液で洗浄
することを特徴とする粉末状陰イオン交換樹脂の再生方
法。
(2) A powdered anion exchange resin with a particle size of 250μ or less, which has been purified from a solution containing a pigment component and a suspended substance and has adsorbed the adsorbed substance, is mixed with a 0.1 to 5% acid aqueous solution heated to 40°C or higher. A method for regenerating a powdered anion exchange resin, which comprises washing with a 0.1 to 1% alkaline aqueous solution after contacting the resin.
JP16552084A 1984-08-07 1984-08-07 Regeneration of powdery anion exchange resin Pending JPS6142336A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP16552084A JPS6142336A (en) 1984-08-07 1984-08-07 Regeneration of powdery anion exchange resin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP16552084A JPS6142336A (en) 1984-08-07 1984-08-07 Regeneration of powdery anion exchange resin

Publications (1)

Publication Number Publication Date
JPS6142336A true JPS6142336A (en) 1986-02-28

Family

ID=15813950

Family Applications (1)

Application Number Title Priority Date Filing Date
JP16552084A Pending JPS6142336A (en) 1984-08-07 1984-08-07 Regeneration of powdery anion exchange resin

Country Status (1)

Country Link
JP (1) JPS6142336A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54136576A (en) * 1978-04-14 1979-10-23 Itochu Seito Kk Solution treatment
JPS5546218A (en) * 1978-09-25 1980-03-31 Sony Corp Manufacturing method of image pick-up device
JPS577263A (en) * 1980-06-13 1982-01-14 Res Inst For Prod Dev Regeneration of basic anion exchange resin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54136576A (en) * 1978-04-14 1979-10-23 Itochu Seito Kk Solution treatment
JPS5546218A (en) * 1978-09-25 1980-03-31 Sony Corp Manufacturing method of image pick-up device
JPS577263A (en) * 1980-06-13 1982-01-14 Res Inst For Prod Dev Regeneration of basic anion exchange resin

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