Author Topic: Palladium recovery/recycling patents  (Read 5105 times)

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PolytheneSam

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Palladium recovery/recycling patents
« on: December 14, 2002, 06:10:00 PM »
Here's some patents on recovering/recycling palladium catalysts:

Patent US4419525

wacker catalysts

Patent US4822760

regenerating Pd salt catalysts

Patent US5302183

Pd from residue

Patent US3947543

Pd etc from residue

Patent US3536443

CuCl2/acetic acid

Patent US3488144

Pd recovered as double salt

Patent US3484235

wacker Pd recovery

Patent US2875040

NH3

Patent US2049488

interesting apparatus (noble metals)

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The hardest thing to explain is the obvious

PolytheneSam

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Japanese patent abstracts on the subject.
« Reply #1 on: December 15, 2002, 12:53:00 AM »
Japanese patent abstracts on the subject.

PAT-NO: JP407145427A
DOCUMENT-IDENTIFIER: JP 07145427 A
TITLE: METHOD FOR RECOVERING AND RECYCLING PALLADIUM OR PALLADIUM ALLOY FROM CONTACT MATERIAL

PUBN-DATE: June 6, 1995

INVENTOR-INFORMATION:
NAME COUNTRY
NAKANISHI, MOTOYUKI
FUJII, KOICHI

ASSIGNEE-INFORMATION:
NAME COUNTRY
TANAKA KIKINZOKU KOGYO N/A KK

APPL-NO: JP05317278
APPL-DATE: November 24, 1993

INT-CL (IPC): C22B011/00 , B01D011/02

ABSTRACT:
PURPOSE: To recover high-grade palladium capable of being recycled as such at a low cost in a short time by treating a contact material electrolytically or with an acidic soln. to dissolve and separate the base material and then treating the obtained palladium with acid.
CONSTITUTION: Noble metals are recovered from the scraps of the contact material obtained by welding palladium or palladium alloy to the base material of copper or copper alloy. The contact material is electrolyzed as an anode and/or treated with hot concd. sulfuric acid or sulfuric acid-hydrogen peroxide mixed soln. to dissolve and separate the base material. The palladium or palladium alloy as an anode slime is treated with acid to dissolve off the surface part rich in impurities such as the diffused layer of the base material. The acid treatment is conducted with a hydrochloric acid-hydrogen peroxide mixed soln., nitric acid, aqua regia or nitric acid-hydrogen peroxide mixed soln., and about 1-5wt.% of palladium is appropriately dissolved in this case.
COPYRIGHT: (C)1995,JPO

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PAT-NO: JP410008155A
DOCUMENT-IDENTIFIER: JP 10008155 A
TITLE: METHOD FOR RECOVERING PALLADIUM

PUBN-DATE: January 13, 1998

INVENTOR-INFORMATION:
NAME COUNTRY
NAKAZAWA, HIROYUKI

ASSIGNEE-INFORMATION:
NAME COUNTRY
NAKAZAWA HIROYUKI N/A

APPL-NO: JP08192651
APPL-DATE: June 19, 1996

INT-CL (IPC): C22B011/00

ABSTRACT:
PROBLEM TO BE SOLVED: To efficiently recover palladium to a high grade by dissolving the palladium in a strong acid, such as aqua regia, and adding iodine to form palladium iodide and separating the palladium iodide.
SOLUTION: After the palladium is dissolved in the strongly acidic liquid, such as aqua regia, the iodine or iodide is added to the liquid and the palladium is separated in the form of the palladium iodide. Potassium iodide, sodium iodide, calcium iodide, hydroiodic hydrogen acid, etc., are used as the iodide. The amt. of the iodine or iodine ions to be added is confined up to about 1.5 times the equiv. derived from the reaction formula. The separated palladium iodide is dissolved in an aq. alkaline iodide soln. and is then reduced by using reducing agents, such as sodium baron hydride, hydrazine, hydrazine sulfate and sulfite, by which the palladium is recovered. The filtrate after the recovery is repetitively used as the iodine ion-contg. liquid. The concn. of the aq. alkaline iodide soln. is preferably specified to 10wt.% to satd. concn.
COPYRIGHT: (C)1998,JPO

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PAT-NO: JP02001131646A
DOCUMENT-IDENTIFIER: JP 2001131646 A
TITLE: METHOD FOR RECOVERING PALLADIUM

PUBN-DATE: May 15, 2001

INVENTOR-INFORMATION:
NAME COUNTRY
HIRATA, SUEHIDE N/A

ASSIGNEE-INFORMATION:
NAME COUNTRY
KAWASAKI KASEI CHEM LTD N/A

APPL-NO: JP11307842
APPL-DATE: October 28, 1999

INT-CL (IPC): C22B003/24 , C02F001/62 , C02F001/70 , C22B007/00 , C22B011/00

ABSTRACT:
PROBLEM TO BE SOLVED: To efficiently recover palladium without being affected by a coexistent copper ion, etc.
SOLUTION: A copper (II) ion alone is selectively reduced by a tin (II) ion, etc., and then palladium is collected by a metal ion processing agent, when the palladium in a palladium-containing water wherein the copper (II) ion, etc., are coexistent is reduced and collected by the metal ion processing agent prepared by depositing an anthrahydroquinone compound on a porous carrier.
COPYRIGHT: (C)2001,JPO

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The hardest thing to explain is the obvious

PolytheneSam

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PAT-NO: JP358088124A DOCUMENT-IDENTIFIER: JP ...
« Reply #2 on: December 15, 2002, 12:59:00 AM »
PAT-NO: JP358088124A
DOCUMENT-IDENTIFIER: JP 58088124 A
TITLE: PALLADIUM PURIFICATION AND RECOVERY

PUBN-DATE: May 26, 1983

INVENTOR-INFORMATION:
NAME COUNTRY
TANIGAWA, TORU
SHIGA, SHOJI

ASSIGNEE-INFORMATION:
NAME COUNTRY
FURUKAWA ELECTRIC CO N/A LTD:THE

APPL-NO: JP56184727
APPL-DATE: November 18, 1981

INT-CL (IPC): C01G055/00 , C22B011/00

US-CL-CURRENT: 423/22
ABSTRACT:
PURPOSE: Contaminated palladium is dissolved in nitric acid, chlorine ion is added to adjust its pH to remove silver and iron by precipitation, a Cu dust is added to cause replace precipitation, the precipitate is treated with a Cu selection solution, then dissolved again with nitric acid, and sulfurous acid is added to recover purified palladium salt simply and reasonably.
CONSTITUTION: Palladium containing a variety of impurities is dissolved in nitric acid and chlorine ion is added, e.g., by adding sodium chloride as well as sodium hydroxide to adjust the pH to 2~3 to cause the precipitation of large amounts of Ag and Fe. The precipitate is removed by filtration, a Cu powder is added to the solution in an amount 0.6~1.8 times that of the palladium contained to cause replace precipitation. The precipitate is recovered by filtration, the remaining Cu powder is removed with a solution for dissolving the Cu powder selectively such as an inorganic acid other than nitric acid and hydrogen peroxide, then filtered again. The precipitate is dissolved in nitric acid again and sulfurous acid or a sulfite salt is added to the solution, while the pH is adjusted to 8~ 12 with sodium hydroxide or the like to form the precipitate of palladium salt, which is recovered.
COPYRIGHT: (C)1983,JPO&Japio

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PAT-NO: JP411036020A
DOCUMENT-IDENTIFIER: JP 11036020 A
TITLE: TREATMENT OF WASTE PRINTED CIRCUIT BOARD

PUBN-DATE: February 9, 1999

INVENTOR-INFORMATION:
NAME COUNTRY
TAKANO, KOICHI
FUJIYOSHI, KATSUSATO
FUJIYOSHI, MASASUKE

ASSIGNEE-INFORMATION:
NAME COUNTRY
KK JUSTY N/A

APPL-NO: JP09207213
APPL-DATE: July 15, 1997

INT-CL (IPC): C22B007/00 , B09B003/00 , B09B005/00 , C22B003/44

ABSTRACT:
PROBLEM TO BE SOLVED: To provide a method for the treatment of waste printed circuit boards, etc., capable of efficiently recovering noble metals such as gold, palladium, rhodium and platinum, and recovering the glass fiber reinforced expoxy resin and polyimide, etc., which cannot be dissolved by acids capable of dissolving the metals.
SOLUTION: This method includes a metal dissolving process for dissolving the waste printed circuit boards, etc., by feeding the boards, etc., into an acid, such as nitric acid, hydrochloric acid, sulfuric acid, capable of dissolving the metals, a non-pollution treatment stage for gases, etc., for making the vapor and gases generated in this metal dissolving process non-pollutant, a recovering process for the noble metals by adding an alkali to the metal dissolving acids contg. the dissolved metal in the metal dissolving stage described above to adjust the pH thereof to 4 to 5 and recovering the precipitated noble metals, such as Pt, Pd, Rh, Os, Ru and Au, by filtering and a non-dissolved matter removing process for removing the non-dissolved matter, such as glass fiber reinforced expoxy resin and polyimide, which are not dissolved in the metal dissolving process.
COPYRIGHT: (C)1999,JPO

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PAT-NO: JP358174532A
DOCUMENT-IDENTIFIER: JP 58174532 A
TITLE: RECOVERY OF PALLADIUM OR NOBLE METAL MIXED IN PALLADIUM

PUBN-DATE: October 13, 1983

INVENTOR-INFORMATION:
NAME COUNTRY
TAKAYAMA, SHINGO

ASSIGNEE-INFORMATION:
NAME COUNTRY
TANAKA KIKINZOKU KOGYO N/A KK

APPL-NO: JP57056462
APPL-DATE: April 5, 1982

INT-CL (IPC): C22B011/04

ABSTRACT:
PURPOSE: To efficiently recover Pd and noble metals mixed in Pd, by dipping a material covered with Pd (or its alloy) in a mixed solution containing a water- soluble iodine solution and an aqueous iodide solution, dissolving the coating Pd (or its alloy) and then reducing it.
CONSTITUTION: A material covered with Pd or a Pd alloy containing other noble metals is dipped in a mixed solution containing a water-soluble iodine solution and an aqueous iodide solution. As said mixed solution, a mixed one comprising 2pts. iodine, 19pts. KI and 22pts. water is used, for instance. After Pd (or its alloy) is dissolved by said dipping treatment, a reducing agent such as hydrazine is added to the dissolved solution to precipitate and recover Pd and the noble metals mixed in Pd. The mixed solution after being subjected to the precipitation treatment can be regenerated by adding anoxidizing agent to it.
COPYRIGHT: (C)1983,JPO&Japio

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PAT-NO: JP403102298A
DOCUMENT-IDENTIFIER: JP 03102298 A
TITLE: RECOVERY OF PALLADIUM

PUBN-DATE: April 26, 1991

INVENTOR-INFORMATION:
NAME COUNTRY
KUBOTA, MASUMITSU
KOBAYASHI, TSUTOMU

ASSIGNEE-INFORMATION:
NAME COUNTRY
JAPAN ATOM ENERGY RES N/A INST

APPL-NO: JP01239889
APPL-DATE: September 18, 1989

INT-CL (IPC): G21F009/10 , C01G055/00 , C02F001/62

US-CL-CURRENT: 423/11, 423/22
ABSTRACT:
PURPOSE: To enable recovery of a palladium Pd by adding an ascorbic acid to a solution containing platinum group elements, such as a high level radioactive liquid waste.
CONSTITUTION: After decreasing nitric acid concentration of a high level radioactive liquid waste down to some 0.5 to 0.3M and removing a Zr, a Mo and a Te as a precipitation, a Pd can be solely and selectively recovered by adding an ascorbic acid to make the concentration to be 0.0588M and agitating under room temperature for 15 minutes. In this occasion, by increment of an adding amount of the ascorbic acid, a recovery efficiency of the Pd is much improved. Also, by adding an oxalic acid after addition of the ascorbic acid, the Pd, with transuranium elements and rare earth elements, can be recovered as a precipitation at higher recovery ion efficiency. In this case, the transuranium elements and the rare earth elements can be easily separated from the Pd during a dissolving stage of the oxalic acid.
COPYRIGHT: (C)1991,JPO&Japio

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PAT-NO: JP402138424A
DOCUMENT-IDENTIFIER: JP 02138424 A
TITLE: METHOD FOR RECOVERING PALLADIUM

PUBN-DATE: May 28, 1990

INVENTOR-INFORMATION:
NAME COUNTRY
HIRAKO, MAMORU

ASSIGNEE-INFORMATION:
NAME COUNTRY
TANAKA KIKINZOKU KOGYO N/A KK

APPL-NO: JP63288652
APPL-DATE: November 15, 1988

INT-CL (IPC): C22B011/00 , C22B007/00

ABSTRACT:
PURPOSE: To easily separate Pd by extraction and to recover the Pd in high yield by crushing a ceramic laminate contg. Pd, allowing the crushed material to react with concd. nitric acid to elute Pd, and further washing the material with dil. nitric acid.
CONSTITUTION: Pd is recovered from a ceramic laminate consisting essentially of BaTiO3 and contg. Pd. The ceramic laminate is firstly crushed preferably to = about 100 mesh particles. The crushed material is allowed to react with =5 N nitric acid or preferably with commercially available 15 N concd. nitric acid to elute Pd. The Pd is filtered off by using =1 N nitric acid as washing water. By this method, Pd is fixed and separated without decreasing filterability, and Pd is recovered in the high yield of about 90%.
COPYRIGHT: (C)1990,JPO&Japio

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PAT-NO: JP403154640A
DOCUMENT-IDENTIFIER: JP 03154640 A
TITLE: METHOD FOR NOBLE METAL RECOVERY FROM METAL CATALYST

PUBN-DATE: July 2, 1991

INVENTOR-INFORMATION:
NAME COUNTRY
OGAWA, HIROSUMI
HORIE, HIDEAKI

ASSIGNEE-INFORMATION:
NAME COUNTRY
NISSAN MOTOR CO LTD N/A

APPL-NO: JP01292414
APPL-DATE: November 13, 1989

INT-CL (IPC): B01J038/52 , B01J038/00 , C01G055/00

ABSTRACT:
PURPOSE: To heighten noble metal recovery efficiency by recovering catalytic components separately from a metal support after taking off a wash coat layer from the metal support by heating the metal catalyst in an aqueous nitric acid solution.
CONSTITUTION: A metal catalyst containing at least one kind of noble metals selected from a group of platinum, palladium, and rhodium as a catalytic component and coated with a wash coat layer comprised of mainly alumina and ceria is heated in an aqueous nitric acid solution or an aqueous nitric acid solution containing an aqueous hydrogen peroxide solution so as to take off the wash coat layer from the metal support. Then, noble metals are separated and recovered from the metal support. Optionally, a method for recovery of the noble metals by dissolving only noble metals using aqua regia or a mixed solution of hydrochloric acid and hydrogen peroxide after the wash coat layer is taken off followed by precipitating and recovering the noble metals is adopted.
COPYRIGHT: (C)1991,JPO&Japio

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PAT-NO: JP355164044A
DOCUMENT-IDENTIFIER: JP 55164044 A
TITLE: RECOVERING PALLADIUM FROM PALLADIUM PLATING WASTE LIQUID

PUBN-DATE: December 20, 1980

INVENTOR-INFORMATION:
NAME COUNTRY
NISHIYAMA, GORO
HAYASHI, HIROSHI

ASSIGNEE-INFORMATION:
NAME COUNTRY
AGENCY OF IND SCIENCE & N/A TECHNOL

APPL-NO: JP54072608
APPL-DATE: June 8, 1979

INT-CL (IPC): C22B011/04 , C01G055/00

ABSTRACT:
PURPOSE: To separate and recover Pd in high yield as sodium chloroplalladate by a method wherein non-electrolytic palladium plating waste liquid is added with HCl and iron powder, and precipitated cpd. is separated and dissolved in HCl, then the solution is evaporated and dried.
CONSTITUTION: Non-electrolytic Pd plating waste liquid contg. Pd is made acidic by adding HCl, then iron powder is added and heated to produce hydrogen. By the reducing action of produced hydrogen, red crystal of sodium chloropalladate is precipitated. The red precipitate is separated from the liquid and dissolved in HCl and the solution is evaporated and dried, so that sodium chloropalladate crystal is separated and recovered in high yield.
COPYRIGHT: (C)1980,JPO&Japio

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The hardest thing to explain is the obvious

PolytheneSam

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PAT-NO: JP402197531A DOCUMENT-IDENTIFIER: JP ...
« Reply #3 on: December 15, 2002, 01:02:00 AM »
PAT-NO: JP402197531A
DOCUMENT-IDENTIFIER: JP 02197531 A
TITLE: METHOD FOR RECOVERING PALLADIUM

PUBN-DATE: August 6, 1990

INVENTOR-INFORMATION:
NAME COUNTRY
HIRAKO, MAMORU

ASSIGNEE-INFORMATION:
NAME COUNTRY
TANAKA KIKINZOKU KOGYO N/A KK

APPL-NO: JP01017226
APPL-DATE: January 26, 1989

INT-CL (IPC): C22B011/00 , C22B007/00

US-CL-CURRENT: 423/22
ABSTRACT:
PURPOSE: To recover palladium at high extraction rate by crushing a ceramics laminated body containing barium titanate as a dielectric component and combinedly applying a stage of leaching by dissolution in nitric acid and a stage of leaching by dissolution in aqua regia to the crushed matter.
CONSTITUTION: A ceramics laminated body of chip capacitor containing palladi um and also containing barium titanate as a principal dielectric component is crushed. The crushed matter is allowed to react with nitric acid, by which metallic palladium in the crushed matter is dissolved and leached out. Subse quently, solid-liquid separation is carried out by using =1N nitric acid as a cleaning solution. The residue obtained after extraction and cleaning is allowed to react with aqua regia, by which palladium is dissolved and leached out. Then, solid-liquid separation is carried out by using =1N acid, such as nitric acid and hydrochloric acid, as a cleaning solution. Further, it is preferable that reaction temp. in the stage of leaching by dissolution in nitric acid is regu lated to a value higher than that in the stage of leaching by dissolution in aqua regia. By this method, palladium can be separated and recovered at high extraction rate.
COPYRIGHT: (C)1990,JPO&Japio

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PAT-NO: JP355134137A
DOCUMENT-IDENTIFIER: JP 55134137 A
TITLE: PALLADIUM RECOVERING METHOD

PUBN-DATE: October 18, 1980

INVENTOR-INFORMATION:
NAME COUNTRY
ITAYA, HIROSHI
SHIOTANI, AKINORI
YOSHIKIYO, MOTOZO

ASSIGNEE-INFORMATION:
NAME COUNTRY
UBE IND LTD N/A


APPL-NO: JP54040372
APPL-DATE: April 5, 1979

INT-CL (IPC): C22B011/04 , B01J023/96

US-CL-CURRENT: 502/24
ABSTRACT:
PURPOSE: To separation-recover Pd as metallic Pd in a high yield by subjecting an arom. cpd. to oxidation coupling reaction in the presence of an org. Pd catalyst in a solventless state and mixing an alkali metal carbonate and a reducing agent into the resulting soln.
CONSTITUTION: An arom. cpd. such as benzene, toluene or xylene is dehydrogenation-dimerized in the presence of an org. Pd catalyst such as Pd salt of aliph. carboxylic acid in a solventless phase under a press. of 2~200kg/cm2 at a temp. of 40~300°C to form a biphenyl cpd. To the resulting soln. after the oxidation coupling reaction is added a carbonate such as Na2CO3, K2CO3 or Li2CO3, a hydrogencarbonate such as NaHCO3 or KHCO3 or other alkali metal carbonate in an amt. of 0.01~10g per kg of the soln., and they are mixed. After adding a reducing agent such as hydrogen gas, formic acid or oxalic acid the mixed soln. is agitated for 10min~10hr. Pd contained is deposited as large particles of 30µ or more and recovered in a high yield.
COPYRIGHT: (C)1980,JPO&Japio

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PAT-NO: JP407258758A
DOCUMENT-IDENTIFIER: JP 07258758 A
TITLE: METHOD FOR RECOVERING NOBLE METAL FROM AQUEOUS ALKALINE HYDROXIDE SOLUTION

PUBN-DATE: October 9, 1995

INVENTOR-INFORMATION:
NAME COUNTRY
KIKUCHI, HIROTO
ETO, YOSHIYUKI

ASSIGNEE-INFORMATION:
NAME COUNTRY
NISSAN MOTOR CO LTD N/A

APPL-NO: JP06050482
APPL-DATE: March 22, 1994

INT-CL (IPC): C22B011/00

ABSTRACT:
PURPOSE: To provide an industrially inexpensive and rational method for efficiently recovering the noble metal dissolved in an aq. alkali hydroxide soln. with one time of operation without requiring a pretreatment stage.
CONSTITUTION: An amphoteric metal or the alloy of the amphoteric metal is added to the aq. alkali hydroxide soln., by which the noble metals dissolved in the aq. alkali hydroxide soln. are reduced, precipitated and recovered at the time of recovering the noble metals. This method is particularly effective if the noble metal is platinum or palladium. The amphoteric metal is aluminum, zinc, tin, lead or antimony and the alloy of the amphoteric metal is the alloy of =2 kinds of the metals selected from a group consisting of these metals. The amt. of the metal to be added is effective in recovering the noble metal at a high recovery rate if the amt. is 6 to 15g per 1 liter of the aq. alkali hydroxide soln.
COPYRIGHT: (C)1995,JPO

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The hardest thing to explain is the obvious

PolytheneSam

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Another excellent patent
« Reply #4 on: December 17, 2002, 12:58:00 AM »

Patent US3927111

Pd recovery col. 9 L. 45+

This seems to bee related

Post 107796

(smokemouth: "Practical palladium salt recovery - rev drone", Methods Discourse)


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The hardest thing to explain is the obvious

epistemologicide

  • Guest
safety
« Reply #5 on: January 11, 2003, 06:10:00 AM »
thank goodness there is some thing safer than adams catalyst to use now as the consensus,


economical too!! ;D


PolytheneSam

  • Guest
Here's some more
« Reply #6 on: January 22, 2003, 01:39:00 AM »

Patent US3437431

Pd recovery using amines

Patent US3922330

Pd etc. using dimethylglyoxime

Patent US4290967

Pd using HNO3 and sucrose