CN106282581A - A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst - Google Patents

A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst Download PDF

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Publication number
CN106282581A
CN106282581A CN201610935982.2A CN201610935982A CN106282581A CN 106282581 A CN106282581 A CN 106282581A CN 201610935982 A CN201610935982 A CN 201610935982A CN 106282581 A CN106282581 A CN 106282581A
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ruthenium
catalyst
activated carbon
carbon supported
recovery method
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CN106282581B (en
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倪军
涂子龙
林建新
江莉龙
林炳裕
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Fuzhou University
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Fuzhou University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • C22B11/048—Recovery of noble metals from waste materials from spent catalysts
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Catalysts (AREA)

Abstract

The invention provides the recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst, comprise the following steps: the activated carbon supported ruthenium catalyst that will reduce or do not reduced, at 400～800 DEG C of roastings 4～20 h, roasting remaining solid is dissolved in excess acid and filters again, obtain being mainly composed of the solid of ruthenic oxide, the invention has the advantages that calcining heat is low, operation sequence is easy, Product recycling form multiselect, the response rate is high, saves the energy.

Description

A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst
Technical field
The present invention relates to catalyst recovery method field, the recovery side of a kind of ruthenium in activated carbon supported ruthenium catalyst Method.
Background technology
From BP companies of Britain in 1992 and Kellogg company of the U.S. successfully develop activated carbon supported ruthenium ammonia synthesis catalyst with Coming, ruthenium is considered as the later second filial generation catalyst of ferrum-based catalyst that continues.But the storage capacity of ruthenium is fewer in the world, in addition valency Lattice are expensive, limit the development of ruthenium ammonia synthesis catalyst, especially catalyst and can lose activity in use for some time, and ruthenium The shortage of resource just requires to need efficient recovery in dead catalyst to obtain ruthenium.
Chinese invention patent CN200610052073.0 and CN200810117483.8 discloses the catalysis of activated carbon supported ruthenium The recovery method of ruthenium in agent.Wherein technical scheme disclosed in the patent of Patent No. CN200610052073.0 is: soaks and removes Alkali and alkaline earth metal ions compound, then carries out high-temperature roasting by sample to be recycled, removes charcoal, contains in catalyst to be recycled Alkali metal ion is to have catalytic action to the roasting of charcoal, removes alkali metal ion unfavorable to roasting below on the contrary, energy resource consumption More.After removing charcoal, carry out high-temperature alkali and melt, then utilize oxidant to obtain RuO4, then absorb with strong acid, thus ruthenium is carried out back Receive；But due to RuO4For toxic gas, there is potential danger.Skill disclosed in the patent of Patent No. CN200810117483.8 Art scheme is: first passing through immersion and remove alkali and alkaline earth metal ions compound, roasting carbon removal, then high-temperature alkali is melted, then by adding Alkaline precipitation obtains hydroxide ruthenium precipitation, thus reclaims ruthenium；This method operation is more complicated, during the disappearing of the energy Loss-rate is bigger.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention provides a kind of recovery process simple, and process energy consumption is little, and the response rate is high The recovery method of ruthenium in activated carbon supported ruthenium catalyst.
In order to realize above-mentioned technical purpose, the technical scheme is that
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) catalyst is placed under 100～130 DEG C of environment dry 2～24h；
(2) dried catalyst is placed on roasting 4～20h under 400～800 DEG C of environment；
(3) remaining solid after roasting is joined in excess acid solution impregnate；
(4) carry out filtering by the solution after dipping and washing obtains insoluble solid, i.e. reclaim and obtain ruthenium, will filter and after washing Filtrate reclaim as the fresh water (FW) preparing activated carbon supported ruthenium catalyst.
The catalyst of described step (1) is the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium or metal Ru Activated carbon supported ruthenium catalyst.
Described alkali metal be barium or potassium therein more than one.
Described step (2) is additionally included in and is continually fed into oxygenous gas in roasting process until roasting terminates.
In described step (3), acid solution is nitric acid, hydrochloric acid, formic acid, acetic acid or ethanedioic acid.
In described step (3), acid solution mass fraction is 10%～40%.
Described step (4) reclaims the ruthenium obtained and is mainly composed of ruthenic oxide.
By above-mentioned technical purpose, the invention have the benefit that by activated carbon supported ruthenium catalyst is dried Carry out roasting, utilize acid solution to be dissolved by the remaining solid after roasting, by the most recyclable after insoluble solid filtration washing Obtaining ruthenium, program step is simple, and removal process energy consumption is low, and will not produce toxic gas.
Detailed description of the invention
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) catalyst is placed under 100～130 DEG C of environment dry 2～24h；
(2) dried catalyst is placed on roasting 4～20h under 400～800 DEG C of environment；
(3) remaining solid after roasting is joined in excess acid solution impregnate；
(4) carry out filtering by the solution after dipping and washing obtains insoluble solid, i.e. reclaim and obtain ruthenium, will filter and after washing Filtrate reclaim as the fresh water (FW) preparing activated carbon supported ruthenium catalyst.
The catalyst of described step (1) is the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium or metal Ru Activated carbon supported ruthenium catalyst.
Described alkali metal be barium or potassium therein more than one.
Described step (2) is additionally included in and is continually fed into oxygenous gas in roasting process until roasting terminates.
In described step (3), acid solution is nitric acid, hydrochloric acid, formic acid, acetic acid or ethanedioic acid.
In described step (3), acid solution mass fraction is 10%～40%.
Described step (4) reclaims the ruthenium obtained and is mainly composed of ruthenic oxide.
Embodiment 1
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium and barium is placed on 2h it is dried under 130 DEG C of environment；
(2) take the dried catalyst of 10g and be placed on roasting 8h under 400 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined in the salpeter solution that mass fraction is 10% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) salpeter solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, will filter and after washing, filtrate containing barium is reclaimed as preparing activated carbon supported ruthenium and urged The fresh water (FW) of agent.
Embodiment 2
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium, barium and potassium is put Put under 100 DEG C of environment, be dried 24h；
(2) take the dried catalyst of 10g and be placed on roasting 6h under 400 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined in the formic acid solution that mass fraction is 10% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) formic acid solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, and after filtering and washing, the filtrate containing potassium and barium is reclaimed activated carbon supported as preparing The fresh water (FW) of ruthenium catalyst.
Embodiment 3
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing metal Ru and potassium is placed on 10h it is dried under 110 DEG C of environment；
(2) take the dried catalyst of 10g and be placed on roasting 6h under 600 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined in the acetic acid solution that mass fraction is 10% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) acetic acid solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, will filter and after washing, filtrate containing potassium is reclaimed as preparing activated carbon supported ruthenium and urged The fresh water (FW) of agent.
Embodiment 4
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium and barium is placed on 10h it is dried under 110 DEG C of environment；
(2) take the dried catalyst of 10g and be placed on roasting 4h under 800 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined and the ethanedioic acid solution that mass fraction is 10% of excess carries out dipping to surplus Remaining solid has no substantially dissolving；
(4) the ethanedioic acid solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, Described ruthenium is mainly composed of ruthenic oxide, will filter and contains the filtrate recovery of barium after washing as preparing activated carbon supported ruthenium The fresh water (FW) of catalyst.
Embodiment 5
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing metal Ru, barium and potassium is put Put under 110 DEG C of environment, be dried 10h；
(2) take the dried catalyst of 10g and be placed on roasting 10h under 500 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined in the hydrochloric acid solution that mass fraction is 10% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) hydrochloric acid solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, and after filtering and washing, the filtrate containing barium and potassium is reclaimed activated carbon supported as preparing The fresh water (FW) of ruthenium catalyst.
Embodiment 6
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium is placed on 110 10h it is dried under DEG C environment；
(2) take the dried catalyst of 10g and be placed on roasting 20h under 500 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined in the salpeter solution that mass fraction is 30% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) salpeter solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, will filter and filtrate after washing is reclaimed as preparing activated carbon supported ruthenium catalyst Fresh water (FW).
Embodiment 7
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing metal Ru and potassium is placed on 10h it is dried under 110 DEG C of environment；
(2) take the dried catalyst of 10g and be placed on roasting 8h under 500 DEG C of atmospheres being passed through air；
(3) remaining solid after roasting is joined in the hydrochloric acid solution that mass fraction is 20% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) salpeter solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, will filter and after washing, filtrate containing potassium is reclaimed as preparing activated carbon supported ruthenium and urged The fresh water (FW) of agent.
Embodiment 8
A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst, it comprises the following steps:
(1) activated carbon supported ruthenium catalyst of the alkali and alkaline earth metal ions compound auxiliary agent containing metal Ru and barium is placed on 10h it is dried under 110 DEG C of environment；
(2) take the dried catalyst of 10g and be placed on roasting under the atmosphere of 700 DEG C of mixed gas being passed through nitrogen and oxygen 4h；
(3) remaining solid after roasting is joined in the salpeter solution that mass fraction is 40% of excess and carry out dipping to residue Solid has no substantially dissolving；
(4) salpeter solution after step (3) being impregnated carries out filtering and washing obtains insoluble solid, i.e. reclaims and obtains ruthenium, institute The ruthenium stated is mainly composed of ruthenic oxide, will filter and after washing, filtrate containing barium is reclaimed as preparing activated carbon supported ruthenium and urged The fresh water (FW) of agent.
The above is embodiments of the invention, for the ordinary skill in the art, according to the religion of the present invention Leading, the most all equalizations done according to scope of the present invention patent change, repair Change, replace and modification, all should belong to the covering scope of the present invention.

Claims (7)

1. the recovery method of a ruthenium in activated carbon supported ruthenium catalyst, it is characterised in that: it comprises the following steps:
(1) catalyst is placed under 100～130 DEG C of environment dry 2～24h；
(2) dried catalyst is placed on roasting 4～20h under 400～800 DEG C of environment；
(3) remaining solid after roasting is joined in excess acid solution impregnate；
(4) carry out filtering by the solution after dipping and washing obtains insoluble solid, i.e. reclaim and obtain ruthenium, will filter and after washing Filtrate reclaim as the fresh water (FW) preparing activated carbon supported ruthenium catalyst.
The recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst the most according to claim 1, it is characterised in that: described The catalyst of step (1) is the activated carbon supported ruthenium of the alkali and alkaline earth metal ions compound auxiliary agent containing nitric acid ruthenium or metal Ru Catalyst.
The recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst the most according to claim 2, it is characterised in that: described Alkali metal be barium or potassium therein more than one.
The recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst the most according to claim 1, it is characterised in that: described Step (2) is additionally included in and is continually fed into oxygenous gas in roasting process until roasting terminates.
The recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst the most according to claim 1, it is characterised in that: described In step (3), acid solution is nitric acid, hydrochloric acid, formic acid, acetic acid or ethanedioic acid.
The recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst the most according to claim 1, it is characterised in that: described In step (3), acid solution mass fraction is 10%～40%.
The recovery method of a kind of ruthenium in activated carbon supported ruthenium catalyst the most according to claim 1, it is characterised in that: described Step (4) reclaims the ruthenium obtained and is mainly composed of ruthenic oxide.
CN201610935982.2A 2016-11-01 2016-11-01 A kind of recovery method of ruthenium in activated carbon supported ruthenium catalyst Active CN106282581B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108531732A (en) * 2018-01-31 2018-09-14 福州大学 A kind of activated carbon supported ruthenium catalyst gives up the recovery method of ruthenium in agent

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CN102560128A (en) * 2012-03-05 2012-07-11 武汉凯迪工程技术研究总院有限公司 Method for recovering ruthenium from waste aluminum oxide loaded ruthenium catalyst

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CN102476052A (en) * 2010-11-29 2012-05-30 中国石油化工股份有限公司 Supported ruthenium catalyst and preparation method thereof
CN102108444A (en) * 2011-04-01 2011-06-29 开滦能源化工股份有限公司 Method for recycling ruthenium in supported type ruthenium catalyst
CN102560128A (en) * 2012-03-05 2012-07-11 武汉凯迪工程技术研究总院有限公司 Method for recovering ruthenium from waste aluminum oxide loaded ruthenium catalyst

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108531732A (en) * 2018-01-31 2018-09-14 福州大学 A kind of activated carbon supported ruthenium catalyst gives up the recovery method of ruthenium in agent
CN108531732B (en) * 2018-01-31 2019-05-17 福州大学 A kind of activated carbon supported ruthenium catalyst gives up the recovery method of ruthenium in agent

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