JPS63134639A - Treatment of waste liquor for electroless precipitation of metallic copper - Google Patents
Treatment of waste liquor for electroless precipitation of metallic copperInfo
- Publication number
- JPS63134639A JPS63134639A JP61279351A JP27935186A JPS63134639A JP S63134639 A JPS63134639 A JP S63134639A JP 61279351 A JP61279351 A JP 61279351A JP 27935186 A JP27935186 A JP 27935186A JP S63134639 A JPS63134639 A JP S63134639A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- metallic copper
- waste liquor
- waste liquid
- precipitate
- 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
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 45
- 239000010949 copper Substances 0.000 title claims abstract description 45
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 238000001556 precipitation Methods 0.000 title abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 9
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical class [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 24
- 230000008021 deposition Effects 0.000 claims description 10
- 239000005416 organic matter Substances 0.000 claims description 6
- 239000005751 Copper oxide Substances 0.000 claims 1
- 229910000431 copper oxide Inorganic materials 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000004042 decolorization Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Removal Of Specific Substances (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、金属銅の無電解析出用廃液の処理方法に関し
、更に詳しくは、金属銅の無電解析出法（特公昭５６−
３１３５３号）において用いられる溶液の使用済廃液か
ら銅を分離回収する技術に関する。Detailed Description of the Invention (Industrial Field of Application) The present invention relates to a method for treating waste liquid for electroless deposition of metallic copper, and more specifically to a method for electroless deposition of metallic copper (Japanese Patent Publication No.
The present invention relates to a technology for separating and recovering copper from a spent solution waste solution used in (No. 31353).
（従来の技術）
前記金属銅の無電解析出法は、水溶液中のテトラアンミ
ノ第二銅錯イオンを、含窒素化合物の添加により迅速に
還元することによって得られた水溶液中のジアンミノ第
一銅錯イオンを、賦活性剤を有効量添加して自己酸化還
元させることにより、触媒活性化表面上に金属銅を王と
して析出させるようにしだものである。(Prior art) The electroless deposition method of metallic copper is based on diammino cuprous complex ions in an aqueous solution obtained by rapidly reducing tetraamino cupric complex ions in an aqueous solution by adding a nitrogen-containing compound. By adding an effective amount of an activator and causing self-redox, metallic copper is precipitated as a king on the catalyst-activated surface.
即ち、この析出法では、水溶液中のシアンミノ第一・銅
錯イオンを自己酸化還元させることによって金属銅の他
に第二銅錯イオンか生成され、このため、金属銅の析出
のために用いられた使用済廃液中には金属銅の残部と第
二銅錯イオンの他に、含窒素化合物、賦活性剤等が含有
されていることになる。That is, in this precipitation method, cupric complex ions are generated in addition to metallic copper by self-oxidation-reduction of cyamino-copper complex ions in an aqueous solution. The spent waste liquid contains nitrogen-containing compounds, activators, etc. in addition to the remainder of metallic copper and cupric complex ions.
以りのような使用済廃液から、排水基準に適合するよう
に銅を回収するための従来の廃液処理方法としては、イ
オン交換樹脂法か知られている。An ion exchange resin method is known as a conventional waste liquid treatment method for recovering copper from such used waste liquid in a manner that meets wastewater standards.
（発明か解決しようとする問題点）
しかしながら、従来のイオン交換樹脂法では装置か複雑
かつ大型化し、設備費及びランニンクコストか高くつく
と八に、一定使用頻度ごとにイオン交換樹脂のイオン交
換作用を活性化するための再生作業か必要であり、しか
も再生時の廃液中には樹脂中の銅のほぼ全量が含まれる
ことになり、例えば再生甲府に硫酸を用いた場合には樹
脂中の銅分は硫酸銅液として排出されることになるので
、更にこの液の処理回収か必要となる等工程か複雑化す
るという問題点があった。(Problem to be solved by the invention) However, in the conventional ion exchange resin method, the equipment is complicated and large, and the equipment cost and running cost are high. Regeneration work is required to activate the action, and the waste liquid during regeneration will contain almost all of the copper in the resin. For example, if sulfuric acid is used in the regenerated Kofu, Since the copper content is discharged as a copper sulfate solution, there is a further problem in that the process of processing and recovery of this solution becomes complicated.
尚、使用済廃液から銅を回収する方法としては、他に’
＝ｋ ％剤や沈澱剤を用いる方法か考えられるか、疑集
剤による場合は回収率か悪く、大量添加が必要であると
いう問題点かあるし、沈澱剤による場合は処理済液か着
色状態のままで別に脱色処理が必要になるという問題点
かある。There are other methods for recovering copper from used waste liquid.
=K Is it possible to consider a method using a % agent or a precipitant? If a dispersing agent is used, the recovery rate is poor and a large amount of addition is required, which is a problem.If a precipitant is used, the treated liquid or colored state There is a problem in that a separate decolorization process is required.
（問題点を解決するための手段）
未発ＩＴＪは、Ｊ：、述のような問題点を解消するため
になされたものて、その目的とするところは、処理工程
かＩ！！ｉ巾で銅の回収率か高く、かつ、無色の処理済
液か得られる金属銅の無電解析出用廃液の処理方法の提
供にあり、この目的を達成するための手段として未発Ｉ
Ｉでは、金属銅の無電解析出用廃液に、塩酸ヒドロキル
アミンを添加することによって廃液中に含まれる有機物
の分解と銅の還元とを行なった後に、更にカセイソーダ
を添加して加温熟成させることによって水酸化第一銅の
沈澱物を生成・沈澱させ、次いで該沈殿物を一過するこ
とによって金属銅及び酸化物相を分離回収するという方
法を採用した。(Means for solving the problems) Undeveloped ITJ was developed to solve the problems mentioned above, and its purpose is to solve the problems in the processing process or I! ! The purpose of the present invention is to provide a method for treating a waste liquid for electroless deposition of metallic copper, which has a high copper recovery rate in a width of 100 m and yields a colorless treated liquid.
In I, hydroxylamine hydrochloride is added to the waste liquid for electroless deposition of metallic copper to decompose organic matter contained in the waste liquid and reduce copper, and then caustic soda is further added and heated and aged. A method was adopted in which a precipitate of cuprous hydroxide was generated and precipitated, and then the precipitate was passed through to separate and recover the metallic copper and oxide phases.
（作用）
未発１１の金属銅の無電解析出用廃液の処理方法では、
上述のように、まず、塩酸ヒドロキルアミンを添加する
ことによって廃液中に含まれる有機物の分解と銅の還元
とを行なった後に、更にカセイソーダを添加して加温熟
成させることによって水酸化第一銅の沈澱物を生成・沈
澱させるようにしたことて、この沈澱物を濾過すること
によって廃液中に含まれる金属銅及び酸化物相の分離回
収か簡単な装置で容易に行なえるようになる。(Function) In the method for treating the waste liquid for electroless deposition of 11 unexploited metallic copper,
As mentioned above, first, hydroxylamine hydrochloride is added to decompose the organic matter contained in the waste liquid and copper is reduced, and then caustic soda is added and heated and aged to produce cuprous hydroxide. By filtering this precipitate, the metallic copper and oxide phases contained in the waste liquid can be easily separated and recovered using a simple device.
また、この処理方法によれば、銅の回収率か高く、しか
も濾過処理された濾液は無色に近いのて、その後の脱色
処理も必要なく、従って工程か大幅に簡略化できるよう
になる。Further, according to this treatment method, the recovery rate of copper is high, and since the filtrate after filtration is almost colorless, there is no need for subsequent decolorization treatment, and the process can therefore be greatly simplified.
（実施例） 以下、本発明の詳細な説明する。(Example) The present invention will be explained in detail below.
まず、この実施例て用いられるサンプル廃液の分析結果
によると２サンプル廃液５ｍ文中における銅の含有量は
：ＩＯ，５ｍｇであった。First, according to the analysis results of the sample waste liquids used in this example, the copper content in 5 m of the two sample waste liquids was: IO, 5 mg.
そこて、このサンプル廃液５立に、ａ Ｗ ｔ ｏ％の
塩酸ヒドロキシルアミンを５文添加して１〜２分間放置
することによって、廃液中に含まれる有機物を分解させ
ると共に、銅を還元させ、次いでこれにｌｆｉ定のカセ
イソーダ（ＮＡＯＩ＋）を２０２添加して８０〜９０℃
の温度で約１０分間加温熟成させることによって水酸化
第一銅の沈Ｖ物を生成させ、かつこれを沈澱させた。Then, by adding 5 volumes of hydroxylamine hydrochloride (a w t o %) to 5 volumes of this sample waste liquid and leaving it for 1 to 2 minutes, the organic matter contained in the waste liquid was decomposed and the copper was reduced. Next, 202 lfi constant caustic soda (NAOI+) was added to this and heated to 80-90°C.
By heating and aging at a temperature of about 10 minutes, a cuprous hydroxide precipitate was produced and precipitated.
次に、この沈澱物を目通処理することによって廃液中に
含まれる金属銅及び酸化物相を：ｌＯ，：Ｉｇ回収する
ことかできた。Next, by visually processing this precipitate, the metallic copper and oxide phases contained in the waste liquid could be recovered in :1O, :Ig.
従って、Ｌ記実施例による銅の回収−、Ｅ（除去；Ｖ）
！土ＱＱｌ’ＸｆＸｎ 繍妨３ｎｏ山Ｌ” ｆｆ Ｌ
−ｔ スＮ ノ含有量はわずか０．２ｇてあった。Therefore, recovery of copper according to Example L-, E (removal; V)
! Sat QQl'XfXn Shuja 3no mountain L" ff L
-t Sun content was only 0.2 g.
また、以上のようにして得られた濾液は無色に近いもの
であるか、アルカリ性であるため、放流するためには塩
酸等を添加して中和させる必要かある。Furthermore, since the filtrate obtained as described above is nearly colorless or alkaline, it is necessary to neutralize it by adding hydrochloric acid or the like in order to discharge it.
以上説明してきたように本実施例の金属銅の無電解析出
用廃液の処理方法にあっては、上述のように、まず、塩
酸ヒドロキルアミンを添加することによって廃液中に含
まれる有機物の分解と銅の還元とを行なった後に、更に
カセイソーダを添加して加温熟成させることによって水
酸化第一銅の沈Ｈｍを生成・沈澱させるようにしたこと
で、この沈殿物を一過することによって廃液中に含まれ
る金属銅及び酸化物相の分離回収か簡単な装ごて容易に
行なえるようになる。As explained above, in the method of treating the waste solution for electroless deposition of metallic copper in this example, first, as mentioned above, hydroxylamine hydrochloride is added to decompose the organic matter contained in the waste solution. After the reduction of copper, caustic soda is further added and heated and aged to generate and precipitate cuprous hydroxide (Hm), and by passing this precipitate, waste liquid can be The metal copper and oxide phase contained therein can be easily separated and recovered using a simple trowel.
また、この処理方法によれば、銅の回収率が高く、しか
も濾過処理された濾液は無色に近いので、その後の脱色
処理も必要なく、従って工程か大幅に簡略化できるよう
になる。Further, according to this treatment method, the recovery rate of copper is high, and the filtrate after the filtration treatment is almost colorless, so there is no need for a subsequent decolorization treatment, and the process can therefore be greatly simplified.
以上、本発明の実施例を詳述してきたが、具体的な方法
はこの実施例に限られるものではなく。Although the embodiments of the present invention have been described in detail above, the specific method is not limited to these embodiments.
本発明の要旨を逸脱しない範囲における具体的方法等の
変更かあっても本発明に含まれる。Even if there are changes in the specific method without departing from the gist of the present invention, they are included in the present invention.
例えば、実施例では８０〜９０°Ｃの温度で加温すると
したか、この温度範囲には限定されず、たた８０〜９０
°Ｃの温度範囲で加温した場合が最も銅の回収率（除去
率）か高かった。For example, in the example, heating was performed at a temperature of 80 to 90°C, but the temperature is not limited to this range, and the heating temperature is 80 to 90°C.
The copper recovery rate (removal rate) was highest when heated in the temperature range of °C.
また、放置時間や加温熟成時間も任意であるし、沈澱物
の濾過方法や使用装置も任意である。Further, the standing time and heating aging time are arbitrary, and the method of filtering the precipitate and the equipment used are also arbitrary.
また、１１！酎ヒドロキシルアミンやカセイソーダの濃
度及び添加量も任意である。Also, 11! The concentration and amount of addition of chu hydroxylamine and caustic soda are also optional.
（発明の効果）
以上説明してきたように本発明の金属銅の無電解析出用
廃液の処理方法にあっては、まず、塩酸ヒドロキルアミ
ンを添加することによって廃液中に含まれる有機物の分
解と銅の還元とを行なった後に、更にカセイソーダを添
加して加温熟成させることによって水酸化第一銅の沈澱
物を生成・沈澱させるようにしたことて、この沈澱物を
吐過することによって廃液中に含まれる金属銅及び酸化
物相の分離回収か簡単な装置て容易に行なえるようにな
る。(Effects of the Invention) As explained above, in the method for treating a waste solution for electroless deposition of metallic copper according to the present invention, first, by adding hydroxylamine hydrochloride, organic matter contained in the waste solution is decomposed and copper is removed. After the reduction, caustic soda is further added and heated and aged to generate and precipitate a precipitate of cuprous hydroxide. The separation and recovery of the metallic copper and oxide phases contained in the copper can be easily carried out using a simple device.
また、この処理方法によれば、銅の回収率か高く、しか
も症過処理された濾液は無色に近いのて、その後の脱色
処理も必要なく、従って工程か大幅に簡略化できるよう
になるという効果か得られる。In addition, according to this treatment method, the recovery rate of copper is high, and since the treated filtrate is almost colorless, there is no need for subsequent decolorization treatment, so the process can be greatly simplified. You can get some effect.
特 許 出 願 人
ハイカワ株式会社
手続補正書く自発）
昭和６１年１２月２６日
特許庁長官 黒 １） 明 雄 殿
！、事件の表示
昭和６１年特許願第２７９３５１号
２、発明の名称
金属銅の無電解析出用廃液の処理方法
３、補正をする者
・１￥件との関係 特許出願人
名称 ハイカワ株式会社
４、代理人
〒８１０
住所 福岡市中央区赤坂３丁目８番２６号赤坂エクセル
２階
氏名 （８５１２）弁理士 綾 １） 正 １廿 （
０９２）７１１００９３■
５、補正の対象
ｉ １ ′）３１ ａ ７ ａ ＩＩ Ｏ４ｍ、
。Patent application Hikawa Co., Ltd. (Volunteer to write procedural amendments) December 26, 1985 Commissioner of the Patent Office Kuro 1) Mr. Akio! , Indication of the case Patent Application No. 279351 filed in 1985 2, Title of the invention: Process for treating waste liquid from electroless deposition of metallic copper 3, Person making the amendment: 1 yen Relationship with the matter Patent applicant name: Hikawa Co., Ltd. 4, Agent 〒810 Address 2nd floor, Akasaka Excel, 3-8-26 Akasaka, Chuo-ku, Fukuoka Name (8512) Patent attorney Aya 1) Positive 1 廿 (
092) 7110093■ 5, Correction target i 1') 31 a 7 a II O4m,
.
６、補正の内容 （！。6. Contents of correction (!.
乞 情シ゛″゛。begging I feel sorry for you.
１２４Ａパ124A pa
Claims (1)
ンを添加することによって廃液中に含まれる有機物の分
解と銅の還元とを行なった後に、更にカセイソーダを添
加して加温熟成させることによって水酸化第一銅の沈澱
物を生成・沈澱させ、次いで該沈澱物を濾過することに
よって金属銅及び酸化物銅を分離回収することを特徴と
する金属銅の無電解析出用廃液の処理方法。1) Hydroxylamine hydrochloride is added to the waste liquid for electroless deposition of metallic copper to decompose the organic matter contained in the waste liquid and reduce the copper, and then caustic soda is further added and heated and aged. 1. A method for treating a waste liquid for electroless deposition of metallic copper, which comprises generating and precipitating a precipitate of cuprous hydroxide, and then separating and recovering metallic copper and copper oxide by filtering the precipitate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61279351A JPS63134639A (en) | 1986-11-22 | 1986-11-22 | Treatment of waste liquor for electroless precipitation of metallic copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61279351A JPS63134639A (en) | 1986-11-22 | 1986-11-22 | Treatment of waste liquor for electroless precipitation of metallic copper |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63134639A true JPS63134639A (en) | 1988-06-07 |
| JPS645093B2 JPS645093B2 (en) | 1989-01-27 |
Family
ID=17609958
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61279351A Granted JPS63134639A (en) | 1986-11-22 | 1986-11-22 | Treatment of waste liquor for electroless precipitation of metallic copper |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63134639A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5006262A (en) * | 1989-11-21 | 1991-04-09 | Met. Rev. Inc. | Process for recovering copper from copper ion containing aqueous solutions |
| EP0730500A1 (en) * | 1993-11-22 | 1996-09-11 | Lilly Industries, Inc. | Ammonia-free deposition of copper by disproportionation |
| JP2001340872A (en) * | 2000-06-05 | 2001-12-11 | Japan Organo Co Ltd | Method for treating wastewater containing boron and/or fluorine |
-
1986
- 1986-11-22 JP JP61279351A patent/JPS63134639A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5006262A (en) * | 1989-11-21 | 1991-04-09 | Met. Rev. Inc. | Process for recovering copper from copper ion containing aqueous solutions |
| EP0730500A1 (en) * | 1993-11-22 | 1996-09-11 | Lilly Industries, Inc. | Ammonia-free deposition of copper by disproportionation |
| EP0730500A4 (en) * | 1993-11-22 | 1997-01-29 | Lilly Ind Inc | Ammonia-free deposition of copper by disproportionation |
| JP2001340872A (en) * | 2000-06-05 | 2001-12-11 | Japan Organo Co Ltd | Method for treating wastewater containing boron and/or fluorine |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS645093B2 (en) | 1989-01-27 |
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