JPH0217616B2 - - Google Patents
Info
- Publication number
- JPH0217616B2 JPH0217616B2 JP16743087A JP16743087A JPH0217616B2 JP H0217616 B2 JPH0217616 B2 JP H0217616B2 JP 16743087 A JP16743087 A JP 16743087A JP 16743087 A JP16743087 A JP 16743087A JP H0217616 B2 JPH0217616 B2 JP H0217616B2
- Authority
- JP
- Japan
- Prior art keywords
- waste liquid
- catalyst waste
- filtrate
- tin
- liquid
- 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.)
- Expired
Links
- 239000007788 liquid Substances 0.000 claims description 107
- 239000002699 waste material Substances 0.000 claims description 76
- 239000003054 catalyst Substances 0.000 claims description 69
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 53
- 239000000706 filtrate Substances 0.000 claims description 40
- 239000006228 supernatant Substances 0.000 claims description 37
- 239000002244 precipitate Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000007747 plating Methods 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 230000001235 sensitizing effect Effects 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 229910052763 palladium Inorganic materials 0.000 description 18
- 235000011121 sodium hydroxide Nutrition 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 150000004679 hydroxides Chemical class 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 125000005402 stannate group Chemical group 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- PEKJGTXPLVPTCJ-UHFFFAOYSA-J tin(4+) tetrahydroxide hydrate Chemical class [OH-].O.[Sn+4].[OH-].[OH-].[OH-] PEKJGTXPLVPTCJ-UHFFFAOYSA-J 0.000 description 1
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1617—Purification and regeneration of coating baths
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Chemically Coating (AREA)
- Removal Of Specific Substances (AREA)
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、プラスチツク表面にめつきを施す際
のセンシタイジング、アクチベイテイング工程に
おいて用いたキヤタリスト廃液から高純度の錫を
回収する、キヤタリスト廃液からの錫回収法に関
する。[Detailed Description of the Invention] [Industrial Application Field] The present invention is directed to a catalyst system that recovers high-purity tin from catalyst waste liquid used in the sensitizing and activating process when plating plastic surfaces. Concerning a method for recovering tin from waste liquid.
［従来の技術］
プラスチツク表面にめつきを施す際には、エツ
チング処理を施したプラスチツク表面の小穴に、
化学めつきを施す際の核となるパラジウムなどの
触媒粒子を析出させるためのセンシタイジング
（触媒賦与）、アクチベイテイング（活性化）を行
う必要がある。[Prior art] When plating a plastic surface, small holes in the etched plastic surface are plated.
It is necessary to perform sensitizing (catalyst provision) and activation (activation) in order to precipitate catalyst particles such as palladium that serve as the core when chemical plating is applied.
このセンシタイジング、アクチベイテイング工
程に用いたキヤタリスト廃液には、高付加価値の
パラジウム、錫が大量に含まれている。 The catalyst waste liquid used in this sensitizing and activating process contains large amounts of high value-added palladium and tin.
そのため、従来は、上記キヤタリスト廃液に、
カセイソーダ（NaOH）等のアルカリ剤を添加
して、上記キヤタリスト廃液を中和し、該キヤタ
リスト廃液に含まれるパラジウム、錫を、Pd
（OH）2、Sn（OH）2、Sn（OH）4等の水酸化物にし
て、キヤタリスト廃液底部に沈澱させて、キヤタ
リスト廃液から回収した後、上記回収した沈澱物
を溶液中に再溶解させて電解分離等することによ
り、パラジウムと錫に分離して、上記キヤタリス
ト廃液から高付加価値のパラジウム、錫を回収し
ていた。 Therefore, conventionally, the above-mentioned catalyst waste liquid was
The catalyst waste liquid is neutralized by adding an alkaline agent such as caustic soda (NaOH) to remove palladium and tin contained in the catalyst waste liquid.
(OH) 2 , Sn(OH) 2 , Sn(OH) 4 and other hydroxides are precipitated at the bottom of the catalyst waste liquid and recovered from the catalyst waste liquid, and then the recovered precipitate is redissolved in the solution. Palladium and tin are separated into palladium and tin by electrolytic separation, etc., and high value-added palladium and tin are recovered from the catalyst waste liquid.
［発明が解決しようとする問題点］
ところで、上述従来の回収法を用いてキヤタリ
スト廃液からパラジウム、錫を回収した場合に
は、キヤタリスト廃液底部に沈澱させた沈澱物を
電解分離法等により高純度のパラジウムと錫に分
離するための大掛かりな設備や多大な手数を必要
とした。[Problems to be Solved by the Invention] By the way, when palladium and tin are recovered from the catalyst waste liquid using the above-mentioned conventional recovery method, the precipitate settled at the bottom of the catalyst waste liquid can be purified to high purity by electrolytic separation method or the like. Separating the metal into palladium and tin required large-scale equipment and a great deal of effort.
本発明は、かかる問題点を解決するために為さ
れたもので、その目的は、大掛かりな設備を用い
たり手数を掛けずに、容易にキヤタリスト廃液か
ら高純度の錫を回収できる、キヤタリスト廃液か
らの錫回収法を提供することにある。 The present invention was made to solve these problems, and its purpose is to easily recover high-purity tin from catalyst waste liquid without using large-scale equipment or requiring much effort. The aim is to provide a tin recovery method.
［問題点を解決するための手段］
上記目的を達成するために、本発明のキヤタリ
スト廃液からの錫回収法は、プラスチツク表面に
めつきを施す際のセンシタイジング、アクチベイ
テイング工程に用いたキヤタリスト廃液に、アル
カリ剤を添加し、該キヤタリスト廃液をPH12以上
の強アルカリ域に移行させて、所定時間放置した
後、上記強アルカリ域に移行させたキヤタリスト
廃液の濾液またはその上澄み液を回収して、所定
時間放置し、該濾液または上澄み液底部に析出、
沈澱する晶析物を取り出すことを特徴とする。[Means for Solving the Problems] In order to achieve the above object, the method of recovering tin from catalyst waste liquid of the present invention can be used in the sensitizing and activating steps when plating the plastic surface. An alkaline agent is added to the catalyst waste liquid, the catalyst waste liquid is moved to a strong alkaline range of pH 12 or higher, and after being left for a predetermined period of time, the filtrate or its supernatant liquid of the catalyst waste liquid that has been moved to the strong alkaline range is collected. and leave it for a predetermined period of time to precipitate at the bottom of the filtrate or supernatant.
It is characterized by taking out the precipitated crystallized product.
本発明においては、強アルカリ域に移行させて
所定時間放置したキヤタリスト廃液の濾液または
その上澄み液を、順次冷却して、該濾液または上
澄み液中の錫の含有量を繰り返し過飽和、飽和状
態としつつ、上記濾液または上澄み液を所定時間
放置することが好適である。 In the present invention, the filtrate or supernatant liquid of catalyst waste liquid that has been transferred to a strongly alkaline region and left for a predetermined period of time is sequentially cooled, and the tin content in the filtrate or supernatant liquid is repeatedly brought to a supersaturated or saturated state. It is preferable to leave the filtrate or supernatant liquid for a predetermined period of time.
［作用］
本発明のキヤタリスト廃液からの錫回収法にお
いては、キヤタリスト廃液に含まれるパラジウ
ム、錫が、該キヤタリスト廃液に添加したアルカ
リ剤でPd（OH）2、Sn（OH）2、Sn（OH）4等の水酸
化物となつて、該キヤタリスト廃液底部に沈澱す
る。そして、上記沈澱した水酸化物のうちのSn
（OH）2、Sn（OH）4等の水酸化錫が、キヤタリス
ト廃液をPH12以上の強アルカリ域に移行させたた
めに、キヤタリスト廃液中に錫酸塩となつて再び
解け出す。そして、上記強アルカリ域に移行させ
たキヤタリスト廃液に、錫が過飽和状態で含まれ
ることとなる。そのため、上記錫が溶解したキヤ
タリスト廃液の濾液またはその上澄み液を回収し
て、所定時間放置すると、該濾液または上澄み液
に含まれるパラジウムが核となつて、還元性雰囲
気下にある上記濾液または上澄み液底部に高純度
の金属錫の晶析物が析出、沈澱するものと推定さ
れる。[Function] In the method for recovering tin from catalyst waste liquid of the present invention, palladium and tin contained in the catalyst waste liquid are converted into Pd(OH) 2 , Sn(OH) 2 , Sn(OH) by an alkaline agent added to the catalyst waste liquid. ) It turns into hydroxides such as 4 and precipitates at the bottom of the catalyst waste liquid. And Sn of the above precipitated hydroxide
Tin hydroxides such as (OH) 2 and Sn(OH) 4 move the catalyst waste liquid to a strongly alkaline range of pH 12 or higher, and therefore become stannate and dissolve again in the catalyst waste liquid. Then, the catalyst waste liquid transferred to the strong alkaline region contains tin in a supersaturated state. Therefore, when the filtrate or supernatant of catalyst waste liquid in which tin is dissolved is collected and left for a predetermined period of time, the palladium contained in the filtrate or supernatant becomes a nucleus, and the filtrate or supernatant under a reducing atmosphere is It is presumed that high-purity metal tin crystallizes and precipitates at the bottom of the liquid.
［実施例］ 次に、本発明の実施例について説明する。[Example] Next, examples of the present invention will be described.
実施例 １
パラジウム280mg／、錫31000mg／を含むキ
ヤタリスト廃液に40W／Ｗ％のカセイソーダ
（NaOH）を添加し、上記キヤタリスト廃液を、
PH13以上の強アルカリ域に移行させて、常温状態
で２時間放置した。すると、上記強アルカリ域に
移行させたキヤタリスト廃液底部に、Pd（OH）2、
Sn（OH）2、Sn（OH）4等の水酸化物からなる沈澱
物が沈澱した。次に、上記底部に沈澱物が沈澱し
たキヤタリスト廃液を、濾紙等を用いて濾過し、
沈澱物と濾液とに分離した。すると、上記キヤタ
リスト廃液からパラジウムを１〜3W／Ｗ％含む
沈澱スラリーを回収できた。また、上記キヤタリ
スト廃液の濾液または上記強アリカリ域に移行さ
せて２時間放置したキヤタリスト廃液の上澄み液
を、常温状態で５時間放置した。すると、該濾液
または上澄み液底部に、金属錫を多量に含む晶析
物が析出、沈澱した。次に、上記底部に晶析物が
析出、沈澱した濾液または上澄み液を、濾紙等を
用いて濾過し、該濾液または上澄み液から晶析物
を取り出した。そして、この濾液または上澄み液
から取り出した晶析物を２回水洗した後、110℃
で12時間乾燥した。すると、錫を98〜100W／Ｗ
％含む高純度の金属錫が得られた。Example 1 40W/W% caustic soda (NaOH) was added to catalyst waste liquid containing 280 mg of palladium and 31000 mg of tin, and the catalyst waste liquid was
The temperature was changed to a strong alkaline range of pH 13 or higher, and the mixture was left at room temperature for 2 hours. Then, Pd(OH) 2 ,
A precipitate consisting of hydroxides such as Sn(OH) 2 and Sn(OH) 4 was precipitated. Next, the catalyst waste liquid in which the precipitate has settled at the bottom is filtered using a filter paper or the like,
It was separated into a precipitate and a filtrate. Then, a precipitated slurry containing 1 to 3% W/W of palladium was recovered from the catalyst waste liquid. Further, the filtrate of the catalyst waste liquid or the supernatant liquid of the catalyst waste liquid that had been transferred to the strong alkaline region and left for 2 hours was left to stand at room temperature for 5 hours. Then, a crystallized substance containing a large amount of metallic tin was deposited and precipitated at the bottom of the filtrate or supernatant liquid. Next, the filtrate or supernatant liquid in which the crystallized substance was deposited and precipitated at the bottom was filtered using a filter paper or the like, and the crystallized substance was taken out from the filtrate or supernatant liquid. Then, the crystallized product taken out from this filtrate or supernatant liquid was washed twice with water, and then heated to 110°C.
and dried for 12 hours. Then, tin is 98~100W/W
% of high purity metallic tin was obtained.
実施例 ２
パラジウム280mg／、錫31000mg／を含むキ
ヤタリスト廃液に25W／Ｗ％のカセイソーダ
（NaOH）を添加し、上記キヤタリスト廃液を、
PH13以上の強アルカリ域に移行させて、常温状態
で２時間放置した。すると、上記強アルカリ域に
移行させたキヤタリスト廃液底部に、Pd（OH）2、
Sn（OH）2、Sn（OH）4等の水酸化物からなる沈澱
物が沈澱した。次に、上記底部に沈澱物が沈澱し
たキヤタリスト廃液を、濾紙等を用いて濾過し、
沈澱物と濾液とに分離した。すると、上記キヤタ
リスト廃液からパラジウムを１〜3W／Ｗ％含む
沈澱スラリーを回収できた。また、上記キヤタリ
スト廃液の濾液または上記強アリカリ域に移行さ
せて２時間放置したキヤタリスト廃液の上澄み液
を、常温状態で５時間放置した。すると、該濾液
または上澄み液底部に、金属錫を多量に含む晶析
物が析出、沈澱した。次に、上記底部に晶析物が
析出、沈澱した濾液または上澄み液を、濾紙等を
用いて濾過し、上記濾液または上澄み液から晶析
物を取り出した。そして、この濾液または上澄み
液から取り出した晶析物を２回水洗した後、110
℃で12時間乾燥した。すると、錫を98〜100W／
Ｗ％含む高純度の金属錫が得られた。Example 2 25 W/W% caustic soda (NaOH) was added to catalyst waste liquid containing 280 mg of palladium and 31000 mg of tin, and the catalyst waste liquid was
The temperature was changed to a strong alkaline range of pH 13 or higher, and the mixture was left at room temperature for 2 hours. Then, Pd(OH) 2 ,
A precipitate consisting of hydroxides such as Sn(OH) 2 and Sn(OH) 4 was precipitated. Next, the catalyst waste liquid in which the precipitate has settled at the bottom is filtered using a filter paper or the like,
It was separated into a precipitate and a filtrate. Then, a precipitated slurry containing 1 to 3% W/W of palladium was recovered from the catalyst waste liquid. Further, the filtrate of the catalyst waste liquid or the supernatant liquid of the catalyst waste liquid that had been transferred to the strong alkaline region and left for 2 hours was left to stand at room temperature for 5 hours. Then, a crystallized substance containing a large amount of metallic tin was deposited and precipitated at the bottom of the filtrate or supernatant liquid. Next, the filtrate or supernatant liquid in which the crystallized substance was deposited and precipitated at the bottom was filtered using a filter paper or the like, and the crystallized substance was taken out from the filtrate or supernatant liquid. Then, after washing the crystallized product taken out from this filtrate or supernatant twice with water,
Dry at ℃ for 12 hours. Then, tin is 98~100W/
High purity metallic tin containing W% was obtained.
実施例 ３
パラジウム280mg／、錫31000mg／を含むキ
ヤタリスト廃液に10W／Ｗ％のカセイソーダ
（NaOH）を添加し、上記キヤタリスト廃液を、
PH13以上の強アルカリ域に移行させて、常温状態
で２時間放置した。すると、上記強アルカリ域に
移行させたキヤタリスト廃液底部に、Pd（OH）2、
Sn（OH）2、Sn（OH）4等の水酸化物からなる沈澱
物が沈澱した。次に、上記底部に沈澱物が沈澱し
たキヤタリスト廃液を、濾紙等を用いて濾過し、
沈澱物と濾液とに分離した。すると、上記キヤタ
リスト廃液からパラジウムを１〜3W／Ｗ％含む
沈澱スラリーを回収できた。また、上記キヤタリ
スト廃液の濾液または上記強アリカリ域に移行さ
せて２時間放置したキヤタリスト廃液の上澄み液
を、常温状態で５時間放置した。すると、該濾液
または上澄み液底部に、金属錫を多量に含む晶析
物が析出、沈澱した。次に、上記底部に晶析物が
析出、沈澱した濾液または上澄み液を、濾紙等を
用いて濾過し、上記濾液または上澄み液から晶析
物を取り出した。そして、この濾液または上澄み
液から取り出した晶析物を２回水洗した後、110
℃で12時間乾燥した。すると、錫を82W／Ｗ％含
む高純度の金属錫が得られた。Example 3 10 W/W% caustic soda (NaOH) was added to catalyst waste liquid containing 280 mg of palladium and 31000 mg of tin, and the catalyst waste liquid was
The temperature was changed to a strong alkaline range of pH 13 or higher, and the mixture was left at room temperature for 2 hours. Then, Pd(OH) 2 ,
A precipitate consisting of hydroxides such as Sn(OH) 2 and Sn(OH) 4 was precipitated. Next, the catalyst waste liquid in which the precipitate has settled at the bottom is filtered using a filter paper or the like,
It was separated into a precipitate and a filtrate. Then, a precipitated slurry containing 1 to 3% W/W of palladium was recovered from the catalyst waste liquid. Further, the filtrate of the catalyst waste liquid or the supernatant liquid of the catalyst waste liquid that had been transferred to the strong alkaline region and left for 2 hours was left to stand at room temperature for 5 hours. Then, a crystallized substance containing a large amount of metallic tin was deposited and precipitated at the bottom of the filtrate or supernatant liquid. Next, the filtrate or supernatant liquid in which the crystallized substance was deposited and precipitated at the bottom was filtered using a filter paper or the like, and the crystallized substance was taken out from the filtrate or supernatant liquid. Then, after washing the crystallized product taken out from this filtrate or supernatant twice with water,
Dry at ℃ for 12 hours. As a result, highly pure metallic tin containing 82 W/W% of tin was obtained.
なお、上述実施例１、２、３において、キヤタ
リスト廃液に添加して、該廃液を強アルカリ域に
移行させるアルカリ剤は、水酸化カリウム、水酸
化カルシウム等でも良い。 In Examples 1, 2, and 3 described above, the alkaline agent added to the catalyst waste liquid to transfer the waste liquid to a strongly alkaline region may be potassium hydroxide, calcium hydroxide, or the like.
また、上述各実施例１、２、３において、金属
錫の晶析物を取り出した残りの廃液は、それぞれ
19ｇ／、16ｇ／、11ｇ／の錫を含む。従つ
て、上記金属錫の晶析物を一旦取り出した残りの
廃液を、順次冷却して、上記錫を含む残りの廃液
を繰り返し過飽和、飽和状態に置くようにして、
上記残りの廃液からさらに金属錫の晶析物を析
出、沈澱させて取り出し、上記残りの廃液の有効
利用を図つても良い。 In addition, in each of the above-mentioned Examples 1, 2, and 3, the remaining waste liquid from which the metal tin crystallized product was taken out was
Contains 19g/, 16g/, 11g/ of tin. Therefore, the remaining waste liquid from which the metal tin crystallized product has been removed is sequentially cooled, and the remaining waste liquid containing tin is repeatedly brought into a supersaturated and saturated state.
It is also possible to further precipitate and extract a crystallized product of metal tin from the remaining waste liquid, thereby making effective use of the remaining waste liquid.
さらに、上述実施例１、２、３において、強ア
ルカリ域に移行させて所定時間放置したキヤタリ
スト廃液の濾液またはその上澄み液を、順次冷却
して、上記キヤタリスト廃液の濾液またはその上
澄み液中の錫の含有量を繰り返し過飽和、飽和状
態としつつ、上記キヤタリスト廃液の濾液または
その上澄み液を放置するようにすれば、該キヤタ
リスト廃液の濾液やその上澄み液を常温状態のま
ま放置する場合と比べて、上記キヤタリスト廃液
の濾液またはその上澄み液中の錫をその底部に金
属錫の晶析物として余す所なく迅速かつ的確に析
出、沈澱させることができて都合が良い。 Furthermore, in Examples 1, 2, and 3 described above, the filtrate of the catalyst waste liquid or its supernatant liquid, which had been transferred to a strong alkaline region and left for a predetermined period of time, was sequentially cooled to remove tin from the catalyst waste liquid filtrate or its supernatant liquid. If the filtrate of the catalyst waste liquid or its supernatant liquid is left to stand while repeatedly bringing the content of It is advantageous that the tin in the filtrate of the catalyst waste liquid or its supernatant liquid can be thoroughly and quickly and precisely precipitated and precipitated as metallic tin crystals at the bottom thereof.
また、本発明の錫回収法において、キヤタリス
ト廃液のアルカリ域への移行度が、PH12以上に達
しない状態では、キヤタリスト廃液を所定時間放
置した後の該廃液の上澄み液に溶解している錫の
量が少なく、該濾液または上澄み液中に含まれる
錫が過飽和状態にならない等のために、上記濾液
または上澄み液を所定時間放置した際に、該濾液
または上澄み液底部に金属錫の晶析物がほとんど
析出、沈澱しなかつた。従つて、本発明の錫回収
法を実施する場合には、キヤタリスト廃液をPH12
以上の強アルカリ域に移行させる必要がある。 In addition, in the tin recovery method of the present invention, if the degree of transition of the catalyst waste liquid to the alkaline region does not reach PH12 or higher, tin dissolved in the supernatant liquid of the waste liquid after the catalyst waste liquid is left to stand for a predetermined period of time. Because the amount of tin contained in the filtrate or supernatant liquid is small and the tin contained in the filtrate or supernatant liquid does not reach a supersaturated state, when the filtrate or supernatant liquid is left for a predetermined period of time, metallic tin crystallization occurs at the bottom of the filtrate or supernatant liquid. Almost no precipitation occurred. Therefore, when carrying out the tin recovery method of the present invention, catalyst waste liquid should be adjusted to pH 12.
It is necessary to move to the above strong alkaline range.
［発明の効果］
以上説明したように、本発明のキヤタリスト廃
液からの錫回収法によれば、従来のように多大な
手数を掛けたり大掛かりな設備を用いたりせず
に、キヤタリスト廃液からら高純度の金属錫を極
めて容易かつ的確に取り出すことができる。[Effects of the Invention] As explained above, according to the method for recovering tin from catalyst waste liquid of the present invention, high tin can be recovered from catalyst waste liquid without requiring a lot of effort or using large-scale equipment as in the past. Metallic tin of high purity can be extracted extremely easily and accurately.
また加えて、本発明のキヤタリスト廃液からの
錫回収法によれば、キヤタリスト廃液にアルカリ
剤を添加して、該廃液を強アルカリ域に移行させ
て所定時間放置する過程において、キヤタリスト
廃液底部に沈澱するパラジウムと錫との水酸化物
の沈澱物のうち水酸化錫の沈澱物が、錫酸ソーダ
（Na2SnO3）等の錫酸塩となつて上記キヤタリス
ト廃液中に再溶解する。そのため、上記強アルカ
リ域に移行させて所定時間放置したキヤタリスト
廃液を、濾紙等を用いて濾過して、沈澱物と濾液
とに分離した場合に、上記キヤタリスト廃液から
回収した沈澱スラリーに含まれるパラジウムの含
有量を、従来のようにキヤタリスト廃液をアルカ
リ剤で中和して該廃液底部に沈澱する沈澱スラリ
ーを回収した場合に比べて、一桁以上向上させる
ことができる等の副次的効果を有する。 In addition, according to the method for recovering tin from catalyst waste liquid of the present invention, in the process of adding an alkaline agent to the catalyst waste liquid, moving the waste liquid to a strong alkaline region, and leaving it for a predetermined period of time, tin is precipitated at the bottom of the catalyst waste liquid. Among the precipitates of hydroxides of palladium and tin, the precipitates of tin hydroxide become stannate salts such as sodium stannate (Na 2 SnO 3 ) and are redissolved in the catalyst waste liquid. Therefore, when catalyst waste liquid that has been transferred to the strong alkaline region and left for a predetermined time is filtered using filter paper or the like and separated into precipitate and filtrate, palladium contained in the precipitated slurry recovered from the catalyst waste liquid is filtered using filter paper or the like. This method has secondary effects such as being able to increase the content of catalyst waste by more than an order of magnitude compared to the conventional method of neutralizing catalyst waste liquid with an alkaline agent and collecting the precipitated slurry that settles at the bottom of the waste liquid. have
Claims (1)
タイジング、アクチベイテイング工程に用いたキ
ヤタリスト廃液に、アルカリ剤を添加し、該キヤ
タリスト廃液をPH12以上の強アルカリ域に移行さ
せて、所定時間放置した後、上記強アルカリ域に
移行させたキヤタリスト廃液の濾液またはその上
澄み液を回収して、所定時間放置し、該濾液また
は上澄み液底部に析出、沈澱する晶析物を取り出
すことを特徴とするキヤタリスト廃液からの錫回
収法。 ２ 強アリカリ域に移行させて所定時間放置した
キヤタリスト廃液の濾液またはその上澄み液を、
順次冷却して、該濾液または上澄み液中の錫の含
有量を繰り返し過飽和、飽和状態としつつ、上記
濾液または上澄み液を所定時間放置するようにし
た特許請求の範囲第１項記載のキヤタリスト廃液
からの錫回収法。[Scope of Claims] 1. Adding an alkaline agent to the catalyst waste liquid used in the sensitizing and activating process when plating the plastic surface, and moving the catalyst waste liquid to a strong alkaline range with a pH of 12 or higher. After leaving it for a predetermined time, collect the filtrate of the catalyst waste liquid transferred to the strong alkaline region or its supernatant liquid, leave it for a predetermined time, and take out the crystallized substance that precipitates at the bottom of the filtrate or supernatant liquid. A method for recovering tin from catalyst waste liquid, which is characterized by the following. 2. The filtrate of catalyst waste liquid that has been transferred to a strongly alkaline region and left for a specified period of time, or its supernatant liquid,
From catalyst waste liquid according to claim 1, wherein the filtrate or supernatant liquid is allowed to stand for a predetermined period of time while the tin content in the filtrate or supernatant liquid is repeatedly brought to a supersaturated or saturated state by sequential cooling. tin recovery method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16743087A JPS6411928A (en) | 1987-07-03 | 1987-07-03 | Recovery of tin from waste liquid of catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16743087A JPS6411928A (en) | 1987-07-03 | 1987-07-03 | Recovery of tin from waste liquid of catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6411928A JPS6411928A (en) | 1989-01-17 |
| JPH0217616B2 true JPH0217616B2 (en) | 1990-04-23 |
Family
ID=15849560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16743087A Granted JPS6411928A (en) | 1987-07-03 | 1987-07-03 | Recovery of tin from waste liquid of catalyst |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6411928A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0789180B2 (en) * | 1989-03-24 | 1995-09-27 | 大阪大学長 | Electro-optical demultiplexing device and beam deflecting device |
| JPH0759276B2 (en) * | 1989-05-10 | 1995-06-28 | シャープ株式会社 | Dryer |
| JP6653778B1 (en) * | 2019-03-14 | 2020-02-26 | 松田産業株式会社 | Method and apparatus for recovering catalytic metal from aqueous solution containing catalytic metal co-precipitated with tin |
-
1987
- 1987-07-03 JP JP16743087A patent/JPS6411928A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6411928A (en) | 1989-01-17 |
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