WO2001088211A2 - Procede de traitement de pieces a usiner au moyen d'une solution colloidale de palladium - Google Patents

Procede de traitement de pieces a usiner au moyen d'une solution colloidale de palladium Download PDF

Info

Publication number
WO2001088211A2
WO2001088211A2 PCT/EP2001/005064 EP0105064W WO0188211A2 WO 2001088211 A2 WO2001088211 A2 WO 2001088211A2 EP 0105064 W EP0105064 W EP 0105064W WO 0188211 A2 WO0188211 A2 WO 0188211A2
Authority
WO
WIPO (PCT)
Prior art keywords
palladium
solution
work pieces
liquid
colloid solution
Prior art date
Application number
PCT/EP2001/005064
Other languages
English (en)
Other versions
WO2001088211A3 (fr
Inventor
Hermann Middeke
Mariola Brandes
Brigitta Dyrbusch
Original Assignee
Atotech Deutschland Gmbh
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 Atotech Deutschland Gmbh filed Critical Atotech Deutschland Gmbh
Priority to EP01949313A priority Critical patent/EP1354073A2/fr
Priority to JP2001584593A priority patent/JP2004500976A/ja
Priority to CA002404620A priority patent/CA2404620A1/fr
Publication of WO2001088211A2 publication Critical patent/WO2001088211A2/fr
Publication of WO2001088211A3 publication Critical patent/WO2001088211A3/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/027—Nanofiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/145—Ultrafiltration
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/16—Regeneration of process solutions
    • C25D21/20—Regeneration of process solutions of rinse-solutions

Definitions

  • the present invention relates to a method for the treatment of work pieces with a palladium colloid solution, preferably to a method for the treatment with a hydrochloric palladium colloid solution being stabilized with tin.
  • the surfaces thereof For the electroplating of work pieces the surfaces thereof must first be treated to render them electrically conductive if the work pieces have electrically nonconducting surfaces.
  • the work pieces are dipped into a solution containing colloidal palladium.
  • the palladium particles thereupon adsorbed on the surfaces serve as activators for initiating electroless metal deposition, which results in the production of an electrically conductive layer on the surface of the work pieces.
  • This conductive layer may afterwards be electroplated with any metal.
  • This process may for example be applied to the production of printed circuit boards and of sanitary appliances, metallized parts for automotive industry and of furniture mountings, especially for chromium plating of plastics parts.
  • Palladium containing activating solutions are also used for direct plating on electrically nonconducting surfaces without using electroless plating methods.
  • the adsorbed layer containing palladium is converted into an electrically conducting layer, which may be used to directly electrodeposit metal on an activated nonconducting surface.
  • a higher concentration of the palladium colloid particles of about 200 mg palladium per liter solution is required.
  • the problem of the present invention therefore consists in avoiding the disadvantages of the known methods and especially in finding a method to treat work pieces with a palladium colloid solution which may be carried out easily. Only small amounts of additional chemicals shall be required for performing the method. Moreover the method shall be carried out with low expense of energy and time.
  • the method according to the invention serves to treat work pieces with a palladium colloid solution by bringing the work pieces into contact with the colloid solution.
  • the invention relates to the treatment of work pieces with a hydrochloric palladium colloid solution being stabilized with tin.
  • the method according the present invention advantageously leads to complete separation of palladium between the concentrate part and the permeate part of the liquid.
  • the known method suffers from the fact that a considerable part of palladium is oxidized to bivalent soluble palladium during the precipitation method. Therefore palladium cannot be separated entirely from the solution by filtration. For this reason palladium is lost partly due to the recovery method.
  • the method according to the present invention advantageously does not require considerable expenditure of additional chemicals, such as for example of metallic tin, as well as of additional energy and time for heating the colloid solution as is the case if the known method would be carried out.
  • the method according to the invention also has the additional advantage to be a single-stage recovery method. This is in contrast to the method as described in US-A-4,435,258. Therefore the method according to the invention is very easy to perform. Furthermore palladium can be removed essentially completely from palladium containing solutions, whereas, if the method as described in US-A-4,435,258 is used, only a very low current yield may be achieved when the palladium concentration is low which is normally the case after prolonged electrolysis time. Therefore complete removal of palladium is very complicated oder not at all possible if this known method is used.
  • Colloidal palladium activating solutions contain palladium particles which are surrounded by a protective coating (protective colloid).
  • HREM high-resolution electron microscopy
  • AFM atomic force microscopy
  • the palladium particles have a diameter of at least 2.5 nm.
  • the size distribution is extremely narrow: It has proven that no considerable deviations from the mean particle size of 2.5 nm occurs in solutions containing colloidal palladium that are usually used to activate nonconductor surfaces.
  • molecular filters are used that preferably have an exclusion pore size of from 200 Dalton to 10.000 Dalton.
  • exclusion pore size of at least 500 Dalton is especially preferred. Most advantageous has proven an exclusion pore size of at least 2.000 Dalton. These further lower limits of the range represent preferred embodiments of the present invention, presenting an even better selectivity of separation between palladium particles and tin compounds under the circumstances mentioned.
  • the rinsing liquid is pressed through the selective molecular filter membrane by means of a pressurized pump, the membrane holding back the palladium particles und letting pass the rinsing liquid, especially rinsing water, and all other components contained in the rinsing liquid.
  • the permeate liquid can then be led to waste water treatment.
  • the palladium being held back and present as a homogeneous metal dispersion concentrate can be used to produce an activating solution.
  • tin(II) or tin(IV) salts and hydrochloric acid in higher or lower amounts are to be added to the concentrate liquid.
  • the palladium held back may be dissolved und be used as a solution, for example a palladium chloride solution, in order to produce an activating solution or alternatively to use this solution for any other purpose.
  • the rinsing liquid made acidic with hydrochloric acid is afterwards led to the molecular filter unit 10 via a pump 9.
  • a filter membrane is arranged inside the molecular filter 10.
  • the liquid present in the region in front of the filter membrane in the molecular filter is pumped in a circuit (not shown). Therefore the colloid particles are permanently in motion in the region in front of the filter membrane, so that the pores of the membrane may not be clogged (cross- flow).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Water Supply & Treatment (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemically Coating (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un procédé destiné à traiter des pièces à usiner au moyen d'une solution colloïdale de palladium par mise en contact de ces pièces à usiner avec la solution colloïdale, le palladium étant recouvert après l'utilisation de cette solution colloïdale. Pour ce faire, on sépare des particules colloïdales de palladium du liquide colloïdal à l'aide d'un filtre moléculaire. Grâce à ce procédé, on peut facilement séparer la totalité du palladium des solutions de traitement utilisées de manière continue, en peu de temps et sans faire intervenir une quantité importante de produits chimiques et d'énergie. La solution de traitement utilisée peut notamment être traitée après la séparation de la partie de la solution contenant le palladium de façon que ce palladium puisse être entièrement récupéré et réutilisé en vue d'un traitement ultérieur.
PCT/EP2001/005064 2000-05-15 2001-05-04 Procede de traitement de pieces a usiner au moyen d'une solution colloidale de palladium WO2001088211A2 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP01949313A EP1354073A2 (fr) 2000-05-15 2001-05-04 Procede de traitement de pieces a usiner au moyen d'une solution colloidale de palladium
JP2001584593A JP2004500976A (ja) 2000-05-15 2001-05-04 パラジウムコロイド溶液を用いた被処理物の処理方法
CA002404620A CA2404620A1 (fr) 2000-05-15 2001-05-04 Procede de traitement de pieces a usiner au moyen d'une solution colloidale de palladium

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10024239.1 2000-05-15
DE10024239A DE10024239C1 (de) 2000-05-15 2000-05-15 Verfahren zum galvanotechnischen Behandeln von Werkstücken mit einer Palladiumkolloidlösung

Publications (2)

Publication Number Publication Date
WO2001088211A2 true WO2001088211A2 (fr) 2001-11-22
WO2001088211A3 WO2001088211A3 (fr) 2003-08-28

Family

ID=7642432

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2001/005064 WO2001088211A2 (fr) 2000-05-15 2001-05-04 Procede de traitement de pieces a usiner au moyen d'une solution colloidale de palladium

Country Status (6)

Country Link
US (1) US20030155250A1 (fr)
EP (1) EP1354073A2 (fr)
JP (1) JP2004500976A (fr)
CA (1) CA2404620A1 (fr)
DE (1) DE10024239C1 (fr)
WO (1) WO2001088211A2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115282789A (zh) * 2022-01-24 2022-11-04 浙江师范大学 一种ABS-Ni复合分离膜及其制备方法与应用

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10148632C1 (de) * 2001-09-26 2003-06-05 Atotech Deutschland Gmbh Verfahren und Vorrichtung zum galvanotechnischen Behandeln von Werkstücken mit einer Edelmetalle enthaltenden Flüssigkeit
JP2003247029A (ja) * 2001-11-21 2003-09-05 Shipley Co Llc 多孔性金属を使用する触媒金属を回収する方法
US6908496B2 (en) * 2002-01-02 2005-06-21 William Marsh Rice University Method for scalable production of nanoshells using salt assisted purification of intermediate colloid-seeded nanoparticles
EP1884278A1 (fr) * 2006-07-24 2008-02-06 ATOTECH Deutschland GmbH Appareil et méthode pour rincer des liquides de pièces à façonner
JP6340302B2 (ja) * 2014-10-24 2018-06-06 田中貴金属工業株式会社 廃液の処理方法、廃液の処理装置および廃液の再利用方法
EP3133175A1 (fr) * 2015-08-19 2017-02-22 Enthone, Inc. Système et procédé de récupération de métal noble catalytique à partir de solution de traitement galvanique aqueuse
CN106987877A (zh) * 2017-04-01 2017-07-28 厦门建霖工业有限公司 一种塑料电镀用胶体钯回收及水回用的系统及方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5348657A (en) * 1992-05-25 1994-09-20 Degussa Aktiengesellschaft Process for the separation of catalyst-free working solution from the hydrogenation circuit of the anthraquinone process for the production of hydrogen peroxide

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3532518A (en) * 1967-06-28 1970-10-06 Macdermid Inc Colloidal metal activating solutions for use in chemically plating nonconductors,and process of preparing such solutions
DE2240317C3 (de) * 1971-08-21 1975-07-10 Asahi Kasei Kogyo K.K., Osaka (Japan) Verfahren zur Wiedergewinnung erneut einsetzbarer palladiumhaltiger Katalysatoren aus flüssigen Reaktionsgemischen, die bei der Herstellung von Essigsäurearylestern anfallen
CA1053994A (fr) * 1974-07-03 1979-05-08 Amp Incorporated Sensibilisation de polymeres de type polyimide pour deposition non electrolytique de metal
US4008343A (en) * 1975-08-15 1977-02-15 Bell Telephone Laboratories, Incorporated Process for electroless plating using colloid sensitization and acid rinse
US4078918A (en) * 1976-11-26 1978-03-14 Perman Craig A Method for precious metal recovery
DE3040631A1 (de) * 1980-10-29 1982-05-27 Merck Patent Gmbh, 6100 Darmstadt Verfahren zur abtrennung von metallkatalysatoren und verwendung von membrantrennvorrichtungen
US4435258A (en) * 1982-09-28 1984-03-06 Western Electric Co., Inc. Method and apparatus for the recovery of palladium from spent electroless catalytic baths
US4600699A (en) * 1983-02-14 1986-07-15 Enthone, Incorporated Reclamation of a palladium-tin based electroless plating catalyst from the exhausted catalyst solution and accompanying rinse waters
AU6017398A (en) * 1997-01-10 1998-08-03 Ellipsis Corporation Micro and ultrafilters with controlled pore sizes and pore size distribution andmethod for making
CA2307500C (fr) * 1997-10-30 2010-01-12 Hw Process Technologies, Inc. Procede pour eliminer des contaminants de liquides a traiter dans des procedes de rendement metal
DE60106498T2 (de) * 2000-01-20 2006-07-13 Westfalia Separator Ag Verfahren und Vorrichtung für die Reinigung und/oder Behandlung von edelmetallhaltigen Suspensionen mittels Membranfiltration
EP1224972A1 (fr) * 2001-01-18 2002-07-24 Shipley Co. L.L.C. Procédé de récupération des métaux catalytiques à partir d'une solution colloidale

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5348657A (en) * 1992-05-25 1994-09-20 Degussa Aktiengesellschaft Process for the separation of catalyst-free working solution from the hydrogenation circuit of the anthraquinone process for the production of hydrogen peroxide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DATABASE CA [Online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; REITER, ARPAD: "Recovery of the colloidal palladium content of exhausted activating solutions used for the current-free metal coating of resin surfaces" retrieved from STN Database accession no. 85:81575 CA XP002210024 cited in the application & HU 11 100 A (VIDEOTON RADIO ES TELEVIZIOGYAR, HUG.)) 28 January 1976 (1976-01-28) *
See also references of EP1354073A2 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115282789A (zh) * 2022-01-24 2022-11-04 浙江师范大学 一种ABS-Ni复合分离膜及其制备方法与应用

Also Published As

Publication number Publication date
DE10024239C1 (de) 2001-09-20
CA2404620A1 (fr) 2001-11-22
WO2001088211A3 (fr) 2003-08-28
US20030155250A1 (en) 2003-08-21
JP2004500976A (ja) 2004-01-15
EP1354073A2 (fr) 2003-10-22

Similar Documents

Publication Publication Date Title
WO1994012684A1 (fr) Bains de depot de nickel chimique
JPS60106583A (ja) 沈殿可能な材料と酸及び／又は塩基を含む水性流の処理方法
KR20020086883A (ko) 이온 교환에 의해 금속을 제거하는 방법 및 장치
US20030155250A1 (en) Method for the treatment of work pieces with a palladium colloid solution
US5328616A (en) Methods and apparatus for treating electroless plating baths
JP2006000792A (ja) 電解析出処理装置および方法
CN100396627C (zh) 一种纳滤法处理电镀废水的清洁生产方法
CN115745295A (zh) 一种pcb生产过程中产生的含铜废水的膜法处理工艺
JP6518834B2 (ja) 水性ガルバニック処理溶液から触媒貴金属を回収するためのシステム及び方法
EP1884278A1 (fr) Appareil et méthode pour rincer des liquides de pièces à façonner
KR100429763B1 (ko) 인쇄회로기판의 세척폐액으로부터 유효성분의 회수방법
EP1430163B1 (fr) Recuperation de metal precieux
CN106865850A (zh) 氰化镀镉废水零排放处理方法
Ramachandraiah et al. Separation and concentration of metals present in industrial effluent and sludge samples by using electrodialysis, coulometry, and photocatalysis
JP2016160493A (ja) 電子基板から貴金属を分離、回収する方法およびそのための装置
WO1994012683A1 (fr) Procede et appareil de traitement de bain de metallisation sans courant electrique
JP3826497B2 (ja) 純水製造方法
KR20050076668A (ko) 도금조를 유지하기 위한 방법
CN218620523U (zh) 一种电子行业含铜废水的回收处理系统
McINTYRE Wastewater Pollution Prevention, Precipitation and Separation Processes
CN102815828B (zh) 表面处理湿制程清洗液中金及氰化物的循环利用系统
JP2001131652A (ja) パラジウムの分離、回収方法
JPS5824515B2 (ja) コケイリユウシオケンダクサセタタソウニツケルメツキコウテイノクロ−ズドシステムカホウホウ
DD284487A5 (de) Verfahren zur rueckgewinnung von metallen aus spuelbaedern

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A2

Designated state(s): CA JP US

AL Designated countries for regional patents

Kind code of ref document: A2

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE TR

121 Ep: the epo has been informed by wipo that ep was designated in this application
DFPE Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101)
WWE Wipo information: entry into national phase

Ref document number: 2001949313

Country of ref document: EP

WWE Wipo information: entry into national phase

Ref document number: 2404620

Country of ref document: CA

WWE Wipo information: entry into national phase

Ref document number: 10276351

Country of ref document: US

WWP Wipo information: published in national office

Ref document number: 2001949313

Country of ref document: EP

WWW Wipo information: withdrawn in national office

Ref document number: 2001949313

Country of ref document: EP