JPS61110731A - Method for collecting platinum and palladium from platinum catalyst - Google Patents

Method for collecting platinum and palladium from platinum catalyst

Info

Publication number
JPS61110731A
JPS61110731A JP23347184A JP23347184A JPS61110731A JP S61110731 A JPS61110731 A JP S61110731A JP 23347184 A JP23347184 A JP 23347184A JP 23347184 A JP23347184 A JP 23347184A JP S61110731 A JPS61110731 A JP S61110731A
Authority
JP
Japan
Prior art keywords
platinum
iron powder
catalyst
palladium
excessive iron
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
JP23347184A
Other languages
Japanese (ja)
Inventor
Mitsuo Muraki
村木 光男
Yukihiro Mitsui
光井 之弘
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.)
Nippon Jiryoku Senko Co Ltd
Original Assignee
Nippon Jiryoku Senko 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 Nippon Jiryoku Senko Co Ltd filed Critical Nippon Jiryoku Senko Co Ltd
Priority to JP23347184A priority Critical patent/JPS61110731A/en
Publication of JPS61110731A publication Critical patent/JPS61110731A/en
Pending legal-status Critical Current

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  • Manufacture And Refinement Of Metals (AREA)

Abstract

PURPOSE:To collect a platinum metal with a high yield by dissolving and extracting a waste catalyst using the platinum metal, by a strong acid, adding an excessive iron powder to said catalyst, executing simultaneously hydrogen reduction and cementation, precipitating the platinum metal, and thereafter, adsorbing and removing the excessive iron powder by a magnetic separating machine. CONSTITUTION:A used waste catalyst of a Pt precious metal catalyst of Pt, Pd, etc. carried by a carrier of alumina, silica, etc. is treated by a strong acid water solution of >=60 deg.C of HCl=1.0N, HNO3>0.2N, in a state that it remains uncrashed, and Pt, Pd, etc. are dissolved and extracted. An excessive iron powder is added to an extracted liquid separated from the carrier, a reducing reaction of an H2 gas and a cementation are executed simultaneously within a range of -50mV-250mV of the reducing potential, and Pt and Pd dissolved in the acid liquid are precipitated with a yield of >=95% in a short time. The excessive iron powder mixed to Pt and Pd precipitated in the end is adsorbed and separated by a magnetic separating machine, and Pt and Pd are collected with a high yield.

Description

【発明の詳細な説明】 本発明は、自動車排ガス浄化に使用した使用済白金触媒
から低コストで、しかも95%以上の高収率で白金とパ
ラジウムを同時に回収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 simultaneously recovering platinum and palladium from spent platinum catalysts used for automobile exhaust gas purification at low cost and with a high yield of 95% or more.

一般に触媒の担体にはアルミナやシリカそれにカーボン
等酸に対して不溶性のものが多く使用され、この担体に
強力な触媒反応を保持している白金属系の元素が塗布さ
れている。然し乍らこのような元素は国内資源としては
殆ど恵まれていないにもかかわらず、需要は自動車産業
の発展に伴い益々増大するばかりである。又半面回収に
関しては回収の技術面とあわせてまだ十分とはいえない
In general, catalyst carriers are often made of acid-insoluble materials such as alumina, silica, and carbon, and these carriers are coated with platinum metal elements that maintain strong catalytic reactions. However, although such elements are scarcely available as domestic resources, their demand is only increasing with the development of the automobile industry. On the other hand, the technical aspect of collection is still not sufficient.

自動車の触媒にはベレット状とハニカム式の形状に大別
されるが、いづれの形状共未粉砕のままの状態で抽出す
ることができる。
Automotive catalysts are broadly divided into pellet-shaped and honeycomb-shaped catalysts, but both shapes can be extracted in an unpulverized state.

そこで本発明は次の三工程の結合からなるものである。Therefore, the present invention consists of a combination of the following three steps.

第一工程 使用済の触媒を固液比が173()1.0)
の比になるように抽出槽に入れ、それにHCl 18以
上(1,5〜2.0Nが望ましい)と更にHHO30,
2N以上(0,4Nが望ましい)とし、60’C以上(
75〜80°Cが最も望ましい)として2時間反応抽出
を行う。
First step: The used catalyst has a solid-liquid ratio of 173 () 1.0)
Add HCl 18 or more (preferably 1.5 to 2.0N) and HHO30,
2N or more (0.4N is preferable) and 60'C or more (
The reaction extraction is carried out for 2 hours at a temperature of 75-80°C (most preferably 75-80°C).

反応後月水で約2倍に希釈し沈降法によって固液分離す
る。
After the reaction, the mixture is diluted approximately twice with water and subjected to solid-liquid separation using a sedimentation method.

第二工程 抽出液からの析出は常温とし、一般にセメン
テーションは所定のpHにするためアルカリを添加し、
それから鉄又は亜鉛でセメンテーションを行うのが公知
の方法とされているが、本発明では中和剤を全く使用し
ない方法を提供するものである。従ワて本発明では強酸
性の抽出液(pHO以下)に鉄粉を添加しH1ガスの還
元反応とセメンテーションを同時に反応きせ、相乗効果
のもとに短時間に白金、パラジウムを析出させるごとが
できるものである。更にこの析出反応は還元電位−50
〜−25On+Vの範囲内で行うことを特徴とするもの
である。
Second step: Precipitation from the extract is carried out at room temperature, and generally cementation involves the addition of alkali to achieve a predetermined pH.
A known method is to then perform cementation with iron or zinc, but the present invention provides a method that does not use any neutralizing agent. Accordingly, in the present invention, iron powder is added to a strongly acidic extract (pH below), and the reduction reaction of H1 gas and cementation are simultaneously carried out, and platinum and palladium are precipitated in a short time due to a synergistic effect. It is something that can be done. Furthermore, this precipitation reaction has a reduction potential of −50
It is characterized in that it is carried out within the range of -25On+V.

これによって白金属元素の溶液中からの収率が98%以
上の比較的高収率を維持することができる。
This makes it possible to maintain a relatively high yield of 98% or more of the platinum metal element from the solution.

第三工程 還元電位が一50mV以下では析出した白金
、パラジウムが再溶解の恐れがあるので、鉄粉は一般に
やや過剰に添加することによって高収率が維持できる。
Third Step If the reduction potential is less than 150 mV, there is a risk that the precipitated platinum and palladium will be redissolved, so a high yield can generally be maintained by adding iron powder in a slightly excessive amount.

従って過剰の鉄粉は析出した白金、パラジウムの品位を
低下させる原因となるので、磁力選鉱によって分離回収
し第二工程に戻し再利用する。
Therefore, excess iron powder causes a decrease in the quality of precipitated platinum and palladium, so it is separated and recovered by magnetic separation and returned to the second step for reuse.

次に本発明を実施例により詳しく説明する。本実施例で
使用した触媒の組成は第1表に示した通りであり、これ
を第1図の処理フローに従って行った結果を第2表から
第4表に示す。
Next, the present invention will be explained in detail with reference to examples. The composition of the catalyst used in this example is shown in Table 1, and the results of this process according to the process flow shown in FIG. 1 are shown in Tables 2 to 4.

第1 表  触媒の組成 (重量%) 第2表 第一工程の条件と結果 第4表  第三工程の結果 第一の溶出工程では強力な酸化剤の使用は好しくない。Table 1: Composition of catalyst (weight%) Table 2 Conditions and results of the first step Table 4 Results of the third step The use of strong oxidizing agents is not preferred in the first elution step.

なぜならば第二工程で多量の鉄粉を必要とするからであ
る。又第二工程での析出反応では多種類の還元剤が使用
きれるが、いずれも高価でありそれに過剰に添加した分
の回収技術が確立されていない。本発明では回収可能な
鉄粉を使用し生産コストを大幅に低減される。
This is because a large amount of iron powder is required in the second step. Furthermore, although many types of reducing agents can be used in the precipitation reaction in the second step, all of them are expensive, and no technology has been established to recover the amount added in excess. The present invention uses recoverable iron powder and significantly reduces production costs.

又還元反応では還元電位−50mV以下では析出が不完
全であると共に、析出した白金属元素が再溶解し収率を
著しく低下させる。
Further, in the reduction reaction, if the reduction potential is -50 mV or less, the precipitation is incomplete, and the precipitated platinum metal element is redissolved, resulting in a significant decrease in yield.

3種類の触媒について、本発明を適用してみた結果、い
ずれの触媒も95%以上の高収率で回収できたことから
、本発明によって低コストでしかも迅速に更に高い収率
で回収する技術が確立され、資源の開発に大きく寄与す
るものである。
As a result of applying the present invention to three types of catalysts, all catalysts could be recovered with a high yield of 95% or more. Therefore, the present invention is a technology for recovering even higher yields quickly at low cost. has been established and will greatly contribute to resource development.

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

第1図は本発明の一実施例の処理フローを示すものであ
る。 特許出願人  日本磁力選鉱株式会社 第 1 図
FIG. 1 shows a processing flow of an embodiment of the present invention. Patent applicant: Japan Magnetic Separation Co., Ltd. Figure 1

Claims (1)

【特許請求の範囲】[Claims] 1、アルミナ、シリカ、炭素を生体とした担体に白金、
パラジウム等を含む白金系触媒を未粉砕の状態にHCl
1.0NそれにHHO_30.2N以上とし、60℃以
上で抽出する第一工程と、該抽出物を固液分離した強酸
性液(pH1.0以下)に鉄粉を添加し、還元電位−5
0mVから−250mVの範囲内で水素還元とセメンテ
ーションを同時に反応させる第二工程と、第二工程で添
加された過剰の鉄粉を磁力選鉱で回収し第二工程に戻す
第三工程との結合によって回収することを特徴とする白
金系触媒から白金、パラジウムの回収方法。
1. Platinum on alumina, silica, and carbon carriers,
Platinum-based catalysts containing palladium etc. are treated with HCl in an unpulverized state.
1.0N and HHO_30.2N or more, the first step is extraction at 60°C or higher, and the solid-liquid separation of the extract is performed, and iron powder is added to the strongly acidic liquid (pH 1.0 or less) to reduce the reduction potential to -5.
A second step in which hydrogen reduction and cementation are simultaneously reacted within the range of 0 mV to -250 mV, and a third step in which excess iron powder added in the second step is recovered by magnetic beneficiation and returned to the second step. A method for recovering platinum and palladium from a platinum-based catalyst, the method comprising recovering platinum and palladium from a platinum-based catalyst.
JP23347184A 1984-11-05 1984-11-05 Method for collecting platinum and palladium from platinum catalyst Pending JPS61110731A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP23347184A JPS61110731A (en) 1984-11-05 1984-11-05 Method for collecting platinum and palladium from platinum catalyst

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP23347184A JPS61110731A (en) 1984-11-05 1984-11-05 Method for collecting platinum and palladium from platinum catalyst

Publications (1)

Publication Number Publication Date
JPS61110731A true JPS61110731A (en) 1986-05-29

Family

ID=16955541

Family Applications (1)

Application Number Title Priority Date Filing Date
JP23347184A Pending JPS61110731A (en) 1984-11-05 1984-11-05 Method for collecting platinum and palladium from platinum catalyst

Country Status (1)

Country Link
JP (1) JPS61110731A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004050926A1 (en) * 2002-12-02 2004-06-17 Council Of Scientific And Industrial Research A process for the recovery of adsorbed palladium from spent silica
US7108839B2 (en) 2002-12-03 2006-09-19 Council Of Scientific And Industrial Research Process for the recovery of palladium from spent silica
KR100792639B1 (en) 2005-06-02 2008-01-09 카운슬 오브 사이언티픽 앤드 인더스트리얼 리서치 A process for the recovery of adsorbed palladium from spent silica
CN106319240A (en) * 2016-08-29 2017-01-11 金川集团股份有限公司 Method for removing noble metal impurities from iridium-containing material liquid

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004050926A1 (en) * 2002-12-02 2004-06-17 Council Of Scientific And Industrial Research A process for the recovery of adsorbed palladium from spent silica
CN1306048C (en) * 2002-12-02 2007-03-21 科学与工业研究会 A process for the recovery of adsorbed palladium from spent silica
US7108839B2 (en) 2002-12-03 2006-09-19 Council Of Scientific And Industrial Research Process for the recovery of palladium from spent silica
KR100792639B1 (en) 2005-06-02 2008-01-09 카운슬 오브 사이언티픽 앤드 인더스트리얼 리서치 A process for the recovery of adsorbed palladium from spent silica
CN106319240A (en) * 2016-08-29 2017-01-11 金川集团股份有限公司 Method for removing noble metal impurities from iridium-containing material liquid

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