JPS605280A - Treatment of waste water containing lead ion - Google Patents

Treatment of waste water containing lead ion

Info

Publication number
JPS605280A
JPS605280A JP58110100A JP11010083A JPS605280A JP S605280 A JPS605280 A JP S605280A JP 58110100 A JP58110100 A JP 58110100A JP 11010083 A JP11010083 A JP 11010083A JP S605280 A JPS605280 A JP S605280A
Authority
JP
Japan
Prior art keywords
cation exchange
lead
waste water
exchange resin
lead ion
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.)
Granted
Application number
JP58110100A
Other languages
Japanese (ja)
Other versions
JPH0368756B2 (en
Inventor
Sadao Yukimasa
行政 定夫
Yukihiro Kitamura
北村 幸弘
Yuji Hayashi
佑二 林
Shiyuichi Komatsu
小松 脩一
Norio Kuramoto
倉元 紀夫
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.)
Organo Corp
Original Assignee
Organo Corp
Japan Organo Co Ltd
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 Organo Corp, Japan Organo Co Ltd filed Critical Organo Corp
Priority to JP58110100A priority Critical patent/JPS605280A/en
Publication of JPS605280A publication Critical patent/JPS605280A/en
Publication of JPH0368756B2 publication Critical patent/JPH0368756B2/ja
Granted legal-status Critical Current

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  • Manufacture And Refinement Of Metals (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

PURPOSE:To treat waste water containing a lead ion easily, inexpensively and effectively to a dischargeable degree, by adsorbing the lead ions contained in waste water with a cation exchange resin while passing an aqueous nitrate solution through said lead ion adsorbed resin to desorb the lead ion. CONSTITUTION:Waste water 2 containing a lead ion is passed through an ion exchange tower 5 from a waste water tank 1 by a pump 3 and the lead ion is adsorbed with a strong acidic cation exchange resin 4 such as an Na-form one to obtain dischargeable treated water 6. The passing amount of the above mentioned waste water 2 is pref. about LV20m/H on the basis of the strong acidic cation exchanger resin 4 having a resin layer height of about 1,000mm.. When the above mentioned strong acidic cation exchange resin 4 reaches the flow-through point of the lead ion, the passing of water is stopped while an aqueous nitrate solution 7 such as about 5% aqueous sodium nitrate solution is passed through the cation exchange resin to desorb the lead ion to easily re-activate said resin. The desorbed liquid 8 is received in a desorbed liquid tank 9 where alkali is added to make it possible to recover lead as hydroxide by filtering.

Description

【発明の詳細な説明】 本発明は鉛イオンを含有する廃水をカチオン交換樹脂で
処理する方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for treating wastewater containing lead ions with a cation exchange resin.

従来から鉛イオンを含有する廃水を処理するにあたりヌ
当該廃水に石灰・ソーダ灰yか性ソーダなどのアルカリ
を添加し・廃水中の鉛イオンを水酸化鉛とし・これを固
液分離する・いわゆる沈殿処理をすることが普通に行な
われている。しかしながらこの方法は反応させるpHが
11以上となると水酸化錯イオンが生成して鉛化合物の
再溶解が起こるので・pHの制御を厳密にせねばならず
・また廃水中の鉛イオン濃度が変化しやすい場合は・当
該濃度に追随してアルカリの添加量も変化させねばなら
ず・運転管理が比較的煩雑であるという欠点を有してい
る。寸だ鉛イオン濃度が比較的薄い場合などは特に十記
沈殿処理が適用しにくいという欠点もある。
Conventionally, when treating wastewater containing lead ions, alkali such as lime or soda ash or caustic soda is added to the wastewater, the lead ions in the wastewater are converted to lead hydroxide, and this is separated into solid-liquid. Precipitation treatment is commonly used. However, in this method, when the pH of the reaction exceeds 11, hydroxide complex ions are generated and the lead compound is redissolved, so the pH must be strictly controlled, and the lead ion concentration in the wastewater is likely to change. In this case, the amount of alkali added must be changed according to the concentration, and operation management is relatively complicated. Another disadvantage is that it is difficult to apply the precipitation treatment especially when the lead ion concentration is relatively low.

一方鉛イオンはカチオン交換樹脂に吸着するので・上記
廃水をカチオン交換樹脂層に通水することにより廃水中
の鉛イオンを除去することができる。しかしながら当該
カチオン交換樹脂に吸着した鉛イオンを脱着する際に・
従来では以下のようが障害が生じていた。すなわち鉛イ
オンを吸着したカチオン交換樹脂に通常の脱着剤・たと
えば塩化ナトリウム水溶液や塩酸を通液すると・脱着に
より液中に移行した塩化鉛がカチオン交換樹脂層中で直
ちに析出し・脱着剤の通液が困難となったり・あるいは
カチオン交換樹脂を汚染し・さらには次回の通水中に当
該析出した塩化鉛が徐々に溶解して処理水中に鉛イオン
が漏出するなどの障害が生じていた。このように従来で
はカチオン交換樹脂に吸着した鉛イオンを効果的に脱着
することが困難であったので・鉛イオンを含有する廃水
の処理にカチオン交換樹脂が用いられなかったが・本発
明者等はこの点に鑑みて・種々の検討を行なった結果・
脱着剤として硝酸塩の水溶液を用いることにより・前述
した脱着の際の障害が全て解決できることを知見した。
On the other hand, since lead ions are adsorbed on the cation exchange resin, the lead ions in the waste water can be removed by passing the waste water through the cation exchange resin layer. However, when desorbing lead ions adsorbed on the cation exchange resin,
Previously, the following problems occurred. In other words, when a normal desorbent such as an aqueous sodium chloride solution or hydrochloric acid is passed through a cation exchange resin that has adsorbed lead ions, the lead chloride transferred into the liquid due to desorption will immediately precipitate in the cation exchange resin layer and the desorbent will pass through. Problems such as the liquid becoming difficult to clean, contaminating the cation exchange resin, and furthermore, the precipitated lead chloride gradually dissolving during the next water flow, causing lead ions to leak into the treated water. In this way, in the past, it was difficult to effectively desorb lead ions adsorbed on cation exchange resins, so cation exchange resins were not used to treat wastewater containing lead ions.The present inventors et al. In view of this point, as a result of various studies,
It has been found that by using an aqueous solution of nitrate as a desorbent, all of the above-mentioned problems during desorption can be overcome.

本発明は上記知見に基づくものであり・鉛イオンを含有
する廃水をカチオン交換樹脂に通水して該廃水中の鉛イ
オンをカチオン交換樹脂に吸着させ・ついで鉛イオンを
吸着した該カチオン交換樹脂に硝酸塩の水溶液を通液し
て該カチオン交換樹脂から鉛イオンを脱着することを特
徴とする鉛イオンを含有する廃水の処理方法に関するも
のである。
The present invention is based on the above findings. Waste water containing lead ions is passed through a cation exchange resin, and the lead ions in the waste water are adsorbed onto the cation exchange resin.Then, the cation exchange resin adsorbs the lead ions. The present invention relates to a method for treating wastewater containing lead ions, characterized in that lead ions are desorbed from the cation exchange resin by passing an aqueous solution of nitrate through the resin.

以下に本発明を図面を参照して詳細に説明する。The present invention will be explained in detail below with reference to the drawings.

図面は本発明を半導体製造工程から発生するハンダディ
ップ廃水の処理に適用した場合のフローの説明図である
The drawing is an explanatory diagram of a flow when the present invention is applied to treatment of solder dip wastewater generated from a semiconductor manufacturing process.

半導体製造工程において基板に各種の半導体を固定し・
これらを結線するためにハンダづけが行なわれているが
、最終製品を得る際にこれらの基板を薄い酸で洗浄する
ため鉛が約5mg7を前後を含有する半導体ハンダディ
ップ廃水が発生する。このような鉛イオン含有計が少な
い廃水においては前述したような沈殿処理法では生成す
るフロックの量が少なすぎ・その適用が困難であるが・
後述するようにカチオン交換樹脂を用いると良好に処理
することができる。
In the semiconductor manufacturing process, various semiconductors are fixed to the substrate.
Soldering is performed to connect these wires, but when the final product is obtained, these boards are cleaned with dilute acid, which generates semiconductor solder dip wastewater containing around 5 mg of lead. For such wastewater with low lead ion content, the precipitation treatment method described above produces too few flocs and is difficult to apply.
As described below, the treatment can be performed satisfactorily by using a cation exchange resin.

すなわち廃水槽lの鉛イオンを含む廃水2をポンプ3を
用いて・塩形たとえばNa形の強酸性カチオン交換樹脂
4が充填されているイオン交換塔5に通水し、廃水2中
の鉛イオンおよび共存する多価カチオンを強酸性カチオ
ン交換樹脂4に吸着させる。なお廃水2に懸濁物が含寸
れている場合は適当な濾過機を用いてあらかじめ懸濁物
を除去するとよい。このような操作により鉛イオンがo
 、 l mg7を以下に減少された処理水6が得られ
るので・当該処理水6をそのまま放流することができる
That is, the waste water 2 containing lead ions in the waste water tank 1 is passed through the ion exchange tower 5 filled with a strongly acidic cation exchange resin 4 in the salt form, for example, the Na form, using the pump 3, and the lead ions in the waste water 2 are removed. and the coexisting polyvalent cations are adsorbed onto the strongly acidic cation exchange resin 4. If the wastewater 2 contains suspended matter, it is advisable to remove the suspended matter in advance using a suitable filter. This operation removes lead ions.
Since the treated water 6 is obtained in which the amount of the treated water 6 is reduced to less than 1 mg7, the treated water 6 can be discharged as it is.

なお強酸性カチオン交換樹脂4の樹脂層高としては通常
1・000mm前後とし・すくなくとも600mmより
高くするとよい。また廃水2の通水流量はLV20m/
H前後が適当であるが・これ以下の流量でもまたこれ以
上の流量でもさしつかえない。
Note that the resin layer height of the strongly acidic cation exchange resin 4 is usually around 1.000 mm, and is preferably higher than at least 600 mm. In addition, the water flow rate of wastewater 2 is LV20m/
A flow rate of around H is appropriate, but a flow rate lower or higher than this is also acceptable.

このような通水を続行すると強酸性カチオン交換樹脂4
が鉛イオンなどの多価カチオンによって貫流点に達し・
処理水6中に鉛イオンがリークしはじめてくる。したが
って通水を中断し。
If this water flow continues, the strongly acidic cation exchange resin 4
reaches the flow-through point due to polyvalent cations such as lead ions.
Lead ions begin to leak into the treated water 6. Therefore, water flow was interrupted.

以下の脱着操作を行なう。Perform the following attachment/detachment operations.

す彦わち常法により強酸性カチオン交換樹脂4を逆洗し
て当該樹脂層中の懸濁物を除くとともに樹脂層をほぐし
・沈整した後脱着剤である硝酸塩水溶液7を通液する。
After backwashing the strongly acidic cation exchange resin 4 to remove suspended matter in the resin layer and loosening and settling the resin layer, a nitrate aqueous solution 7 as a desorbent is passed through the resin layer using a conventional method.

本発明に用いる硝酸塩としては硝酸す) IJウム・硝
酸カリウム!硝酸アンモニウムなどが用いられるが・通
常は硝酸ナトリウムの5条(距骨%)水溶液を用いるこ
とが好ましい3゜このような硝酸塩水溶液7を強酸性カ
チオン交換樹脂4に通液すると・該カチオン交換樹脂4
に吸着されていた鉛イオンは脱着され、該カチオン交換
樹脂4のイオン形を次の通水に適したNa形とするとと
もにt鉛イオンを多−計に含有する脱着液8が得られる
。当該脱着液8と押出し水および洗浄廃水を脱着液槽9
に受け、前述した沈殿処理を行なう。すなわち脱着液に
アルカリを添加して鉛を水酸化物となし・これを濾別し
て水酸化物のケーキを得る。なお本沈殿処理においては
鉛イオンが濃縮された脱着液が対象となり・かつバッチ
処理することができるので当該処理が比較的容易に実施
できる。
The nitrate used in the present invention is nitric acid) potassium nitrate! Although ammonium nitrate etc. are used, it is usually preferable to use a 5-filament (talus %) aqueous solution of sodium nitrate3. When such a nitrate aqueous solution 7 is passed through the strongly acidic cation exchange resin 4, the cation exchange resin 4
The lead ions adsorbed on the cation exchange resin 4 are desorbed, and the ion exchange resin 4 is changed into the Na type suitable for the next water passage, and a desorption liquid 8 containing a large amount of lead ions is obtained. The desorption liquid 8, extrusion water and washing waste water are transferred to a desorption liquid tank 9.
and undergo the precipitation treatment described above. That is, an alkali is added to the desorption solution to convert lead into hydroxide, which is filtered to obtain a hydroxide cake. In this precipitation process, the desorption liquid in which lead ions are concentrated is targeted, and since batch processing can be performed, the process can be carried out relatively easily.

また本発明の脱着操作においては強酸性カチオン交換樹
脂中に鉛塩が析出することなく良好に脱着することがで
きるが・これは脱着剤として硝酸塩の水溶液を用いるこ
とによる効果であり、従来から用いられているたとえば
塩化ナトリウムの水溶液・塩酸では本発明のような効果
は全く望むことができない。しだがって脱着後の通水に
おいて・従来見られていたような析出鉛が徐々に溶解す
ることによる鉛イオンの漏出が全く生じることがない。
In addition, in the desorption operation of the present invention, lead salts can be successfully desorbed into the strongly acidic cation exchange resin without precipitation. This is an effect of using an aqueous solution of nitrate as a desorbent, and is not used conventionally. For example, with an aqueous solution of sodium chloride or hydrochloric acid, the effects of the present invention cannot be expected at all. Therefore, during water passage after desorption, leakage of lead ions due to gradual dissolution of precipitated lead, which has been observed in the past, does not occur at all.

なお脱着剤としては硝酸塩の他に硝酸を用いても鉛塩の
析出を防止して脱着するという目的は達成できるが・硝
酸の場合はイオン交換塔その他の装置を耐酸性にせねば
ならず設備費が増加し・また処理水が酸性となるので放
流するにあたり中和する必要があり・さらに脱着液も強
酸性となるので・脱着液を沈殿処理して鉛を水酸化物と
して分離する際に多量のアルカリを必要とするなど種々
の欠点を有しており好ましくない。
Note that the purpose of preventing and desorbing lead salts can be achieved by using nitric acid instead of nitrate as a desorbent; however, in the case of nitric acid, the ion exchange tower and other equipment must be made acid-resistant, which increases equipment costs.・Also, the treated water becomes acidic, so it needs to be neutralized before being discharged. Furthermore, the desorption solution is also strongly acidic. ・When the desorption solution is precipitated to separate lead as hydroxide, a large amount It is not preferred because it has various drawbacks such as requiring alkali.

す」二説明したごとく本発明はイオン交換塔に単に廃水
を通水するのみで放流可能な処理水が得られ・また廃水
中の鉛イオンの量が変動しても全く問題なく処理するこ
とができるので運転管理が容易であり・かつ処理設備も
安価であり設置面積も小さい。さらにカチオン交換樹脂
に吸着した鉛イオンを脱着する際において・カチオン交
換樹脂層に鉛塩が全く析出することなく効果的に脱着す
ることができる。
As explained above, the present invention can obtain treated water that can be discharged by simply passing wastewater through an ion exchange tower, and can be treated without any problem even if the amount of lead ions in the wastewater fluctuates. This makes operation management easy, and the processing equipment is inexpensive and requires a small installation area. Furthermore, when desorbing lead ions adsorbed on the cation exchange resin, lead salts can be effectively desorbed without any precipitation on the cation exchange resin layer.

以下に本発明の効果を明確とするために実施例を説明す
る。
Examples will be described below to clarify the effects of the present invention.

実施例 内径32.5mm+長さl+000mmのアクリル製の
カラムにNa形の強酸性カチオン交換樹脂アンバーライ
ト(登録商標) IR−120Bを500m1充填し1
当該カラムにカルシウムイオン!マグネシウムイオンな
どの多価カチオン20■as Ca、GO3/lと鉛イ
オン5■aSPb/lを含む半導体製造工程から発生す
る一ノ・ンダデイツプ廃水を2517Hで通水した。そ
の結果鉛イオンo、1mg/IJソ下の処理水が得られ
た。処理量が約1.1m:’に達した点で貫流点となっ
たので通水を止め・以下の脱着を行なった。
Example: An acrylic column with an inner diameter of 32.5 mm + length l + 000 mm was filled with 500 ml of Na-type strongly acidic cation exchange resin Amberlite (registered trademark) IR-120B.
Calcium ions in the column! Ichino-Daip wastewater generated from a semiconductor manufacturing process containing polyvalent cations such as magnesium ions (20 as Ca, GO3/l) and lead ions (5 as SPb/l) was passed through at 2517H. As a result, treated water containing 1 mg/IJ of lead ions was obtained. When the throughput reached approximately 1.1 m:', the flow reached the point where water flow was stopped and the following desorption was performed.

すなわち常法により逆洗・沈整を行ガつた後・1507
の硝酸ナトリウム(再生レベル300S’NaNO3/
lRに相当する)を用いて5チ(重量係)の硝酸ナトリ
ウム水溶液を調整し・当該水溶液をSV4で通液し・常
法により押出水洗を行なった。
In other words, after backwashing and settling by conventional methods, 1507
of sodium nitrate (regeneration level 300S'NaNO3/
A sodium nitrate aqueous solution of 5 cm (by weight) was prepared using a 1R (corresponding to 1R), the aqueous solution was passed through an SV4, and extrusion was washed with water using a conventional method.

またその脱着液の鉛を分析したところカチオン交換樹脂
に吸着した鉛イオンのほぼ100係が脱着されているこ
とが確認された。
Furthermore, when the lead content of the desorption solution was analyzed, it was confirmed that approximately 100% of the lead ions adsorbed on the cation exchange resin were desorbed.

なお比較のために脱着剤として5チ(垂部、チ)の塩化
ナトリウム水溶液を用いたところ・通液中にカチオン交
換樹脂層に塩化鉛が析出し脱着が良好に行なわれなかっ
た。
For comparison, when a 5 liter aqueous solution of sodium chloride was used as a desorbent, lead chloride precipitated on the cation exchange resin layer during the passage of the solution, and desorption was not carried out well.

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

図面は本発明の実施態様の一例のフローの説明図であり
・1は廃水槽・2は廃水・3はポンプ・4は強酸性カチ
オン交換樹脂・5はイオン交換塔・6は処理水・7は硝
酸塩水溶液・8は脱着液、9は脱着液槽を示す。
The drawing is an explanatory diagram of the flow of an example of an embodiment of the present invention. 1 is a waste water tank, 2 is waste water, 3 is a pump, 4 is a strong acid cation exchange resin, 5 is an ion exchange tower, 6 is treated water, and 7 indicates a nitrate aqueous solution, 8 indicates a desorption liquid, and 9 indicates a desorption liquid tank.

Claims (1)

【特許請求の範囲】[Claims] 鉛イオンを含有する廃水をカチオン交換樹脂に通水して
該廃水中の鉛イオンをカチオン交換樹脂に吸着させ・つ
いで鉛イオンを吸着したカチオン交換樹脂に硝酸塩の水
溶液を通液して該カチオン交換樹脂から鉛イオンを脱着
することを特徴とする鉛イオンを含有する廃水の処理方
Wastewater containing lead ions is passed through a cation exchange resin to adsorb the lead ions in the wastewater onto the cation exchange resin, and then an aqueous solution of nitrate is passed through the cation exchange resin that has adsorbed lead ions to exchange the cations. A method for treating wastewater containing lead ions, characterized by desorbing lead ions from a resin.
JP58110100A 1983-06-21 1983-06-21 Treatment of waste water containing lead ion Granted JPS605280A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP58110100A JPS605280A (en) 1983-06-21 1983-06-21 Treatment of waste water containing lead ion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP58110100A JPS605280A (en) 1983-06-21 1983-06-21 Treatment of waste water containing lead ion

Publications (2)

Publication Number Publication Date
JPS605280A true JPS605280A (en) 1985-01-11
JPH0368756B2 JPH0368756B2 (en) 1991-10-29

Family

ID=14527032

Family Applications (1)

Application Number Title Priority Date Filing Date
JP58110100A Granted JPS605280A (en) 1983-06-21 1983-06-21 Treatment of waste water containing lead ion

Country Status (1)

Country Link
JP (1) JPS605280A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116607010A (en) * 2023-07-19 2023-08-18 长沙华时捷环保科技发展股份有限公司 Method for removing and recovering lead from lead-containing solution

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116607010A (en) * 2023-07-19 2023-08-18 长沙华时捷环保科技发展股份有限公司 Method for removing and recovering lead from lead-containing solution
CN116607010B (en) * 2023-07-19 2023-10-17 长沙华时捷环保科技发展股份有限公司 Method for removing and recovering lead from lead-containing solution

Also Published As

Publication number Publication date
JPH0368756B2 (en) 1991-10-29

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