CN106282578A - A kind of method reclaiming noble metal from discarded noble metal catalyst - Google Patents

A kind of method reclaiming noble metal from discarded noble metal catalyst Download PDF

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Publication number
CN106282578A
CN106282578A CN201610792867.4A CN201610792867A CN106282578A CN 106282578 A CN106282578 A CN 106282578A CN 201610792867 A CN201610792867 A CN 201610792867A CN 106282578 A CN106282578 A CN 106282578A
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CN
China
Prior art keywords
noble metal
metal catalyst
discarded
amount ratio
activated carbon
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Pending
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CN201610792867.4A
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Chinese (zh)
Inventor
蔡万煜
李伟峰
张峰
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SHAANXI ROCK NEW MATERIALS CO Ltd
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SHAANXI ROCK NEW MATERIALS CO Ltd
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Priority to CN201610792867.4A priority Critical patent/CN106282578A/en
Publication of CN106282578A publication Critical patent/CN106282578A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/009General processes for recovering metals or metallic compounds from spent catalysts
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a kind of method reclaiming noble metal from discarded noble metal catalyst, add sodium sulfide and activated carbon can form precipitation with the precious metal ion in use departing from carrier, and then absorption is on the activated carbon, prevent the loss of this part noble metal, improve the response rate;Activated carbon and Organic substance is removed by high temperature incineration, reduce volume, advantage is provided for follow-up noble metal removal, the purpose pulverized is to increase response area, improve reaction completion rate, utilize hydrochloric acid and hydrogen peroxide to dissolve and can reduce to final solution is brought into other impurity elements, affect the direct use of precious metal salt solution, this method is simple to operate, substantially increase the recovery extraction ratio of noble metal, the response rate can reach more than 99.0%, the discharge of harmful gas is decreased compared to traditional method for recovering precious metals, reduce the pollution to environment, it is worthy to be popularized.

Description

A kind of method reclaiming noble metal from discarded noble metal catalyst
Technical field
The invention belongs to noble metal recovery technology field, be specifically related to your gold is one reclaim from discarded noble metal catalyst The method belonged to.
Background technology
Noble metal catalyst (precious metal catalyst) one can change chemical reaction velocity and itself not Participate in the precious metal material of reaction end product.Almost all of noble metal is used as catalyst, but conventional be platinum, palladium, Rhodium, silver, ruthenium etc., especially the most most widely used with platinum, rhodium.Their d electron orbit is the most unfilled, the easy adsorption reaction in surface thing, and Moderate strength, is beneficial to form centre " reactive compound ", has higher catalysis activity, the most also have high temperature resistant, antioxidation, Corrosion-resistant comprehensive good characteristic such as grade, becomes most important catalyst material.
Annual nearly 1,000,000 tons of the industrial waste catalyst produced in the whole world, wherein contains substantial amounts of platinum-group noble metals and oxidation thereof Thing, therefore, reclaims noble metal from industrial waste catalyst, is recycled as secondary resource, be possible not only to obtain Objectively economic benefit, moreover it is possible to improve the utilization rate of resource, it is achieved the sustainable development of resource.At present from discarded precious metal catalyst The method reclaiming noble metal in agent mainly has pyrogenic process and wet method two kinds, but two kinds of techniques all exist pollution greatly, and organic efficiency is not High problem.
Summary of the invention
It is an object of the invention to provide a kind of method reclaiming noble metal from discarded noble metal catalyst, solve existing The problem that recovery process is big for environment pollution and noble metal organic efficiency is the highest.
The technical solution adopted in the present invention is, a kind of method reclaiming noble metal from discarded noble metal catalyst, tool Body is implemented according to following steps:
Step 1, puts into the noble metal catalyst of recovery in the reactor filling water, stirs and is added thereto to sulfuration Sodium and activated carbon, after continuing stirring 2~4h, centrifugation, filter cake is standby;
Step 2, puts in Muffle furnace by step 1 gained filter cake, after burning 8~10h, obtains slag at 600~800 DEG C, standby With;
Step 3, pulverizes step 2 gained slag, crosses 200~300 eye mesh screens, and siftage is placed in hydrochloric acid and hydrogen peroxide In mixed liquor dissolve, with after through accurate filter filter, filtrate is standby;
Step 4, by step 3 gained filtrate reduced in volume to PH >=3, add pure water regulation precious metal concentration to 0.5-2%, Solution after adjustment can be directly used in production as the precious metal raw material that new noble metal catalyst produces.
Inventive feature also resides in,
In step 1, noble metal catalyst is 1:3~5 with the amount ratio of water.
In step 1, noble metal catalyst is 1:0.05~0.10 with the amount ratio of sodium sulfide, sodium sulfide and the use of activated carbon Amount ratio is 1:2~3.
In step 3, siftage is 1:8~15 with the amount ratio of mixed liquor.
In step 3, in mixed liquor, hydrochloric acid is 3:1~3 with the amount ratio of hydrogen peroxide.
In step 4, precious metal concentration utilizes inductive coupling plasma emission spectrograph to detect.
The invention has the beneficial effects as follows, add sodium sulfide and activated carbon can be with your gold in use departing from carrier Belong to ion and form precipitation, and then absorption is on the activated carbon, prevents the loss of this part noble metal, improves the response rate;Pass through high temperature Burn and remove activated carbon and Organic substance, reduce volume, provide advantage for follow-up noble metal removal, the purpose of pulverizing be in order to Increase response area, improve reaction completion rate, utilize hydrochloric acid and hydrogen peroxide dissolving to reduce and bring other into in final solution Impurity element, affects the direct use of precious metal salt solution, and this method is simple to operate, and the recovery substantially increasing noble metal is extracted Rate, the response rate can reach more than 99.0%, decreases the discharge of harmful gas compared to traditional method for recovering precious metals, fall The low pollution to environment, is worthy to be popularized.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
A kind of method reclaiming noble metal from discarded noble metal catalyst of the present invention, specifically implements according to following steps:
Step 1, puts into the noble metal catalyst of recovery in the reactor filling water, stirs and is added thereto to sulfuration Sodium and activated carbon, after continuing stirring 2~4h, centrifugation, filter cake is standby;Wherein, noble metal catalyst with the amount ratio of water is 1:3~5.Noble metal catalyst is 1:0.05~0.10 with the amount ratio of sodium sulfide, and sodium sulfide is 1:2 with the amount ratio of activated carbon ~3.
Step 2, puts in Muffle furnace by step 1 gained filter cake, after burning 8~10h, obtains slag at 600~800 DEG C, standby With.
Step 3, pulverizes step 2 gained slag, crosses 200~300 eye mesh screens, and siftage is placed in hydrochloric acid and hydrogen peroxide In mixed liquor dissolve, with after through accurate filter filter, filtrate is standby;Wherein, the amount ratio of siftage and mixed liquor be 1:8~ 15.In mixed liquor, hydrochloric acid is 3:1~3 with the amount ratio of hydrogen peroxide.
Step 4, by step 3 gained filtrate reduced in volume to PH >=3, add pure water regulation precious metal concentration to 0.5-2%, Solution after adjustment can be directly used in production as the precious metal raw material that new noble metal catalyst produces.Precious metal concentration utilizes Inductive coupling plasma emission spectrograph detects.
Embodiment 1
Step 1, puts into the noble metal catalyst of recovery in the reactor filling water, stirs and is added thereto to sulfuration Sodium and activated carbon, after continuing stirring 2h, centrifugation, filter cake is standby;Wherein, noble metal catalyst is 1:3 with the amount ratio of water. Noble metal catalyst is 1:0.05 with the amount ratio of sodium sulfide, and sodium sulfide is 1:2 with the amount ratio of activated carbon.
Step 2, puts in Muffle furnace by step 1 gained filter cake, after burning 10h, obtains slag at 600 DEG C, standby.
Step 3, pulverizes step 2 gained slag, crosses 200 eye mesh screens, siftage is placed in the mixing of hydrochloric acid and hydrogen peroxide In liquid dissolve, with after through accurate filter filter, filtrate is standby;Wherein, siftage is 1:8 with the amount ratio of mixed liquor.Mixing In liquid, hydrochloric acid is 3:1 with the amount ratio of hydrogen peroxide.
Step 4, by step 3 gained filtrate reduced in volume to PH >=3, interpolation pure water regulation precious metal concentration, to 0.5%, is adjusted Solution after whole can be directly used in production as the precious metal raw material that new noble metal catalyst produces.Precious metal concentration utilizes electricity Sense coupled plasma optical emission spectrogrph detection.The final noble metal response rate reaches 99.3%.
Embodiment 2
Step 1, puts into the noble metal catalyst of recovery in the reactor filling water, stirs and is added thereto to sulfuration Sodium and activated carbon, after continuing stirring 3h, centrifugation, filter cake is standby;Wherein, noble metal catalyst is 1:4 with the amount ratio of water. Noble metal catalyst is 1:0.08 with the amount ratio of sodium sulfide, and sodium sulfide is 1:2.5 with the amount ratio of activated carbon.
Step 2, puts in Muffle furnace by step 1 gained filter cake, after burning 9h, obtains slag at 700 DEG C, standby.
Step 3, pulverizes step 2 gained slag, crosses 250 eye mesh screens, siftage is placed in the mixing of hydrochloric acid and hydrogen peroxide In liquid dissolve, with after through accurate filter filter, filtrate is standby;Wherein, siftage is 1:12 with the amount ratio of mixed liquor.Mixing In liquid, hydrochloric acid is 3:2 with the amount ratio of hydrogen peroxide.
Step 4, by step 3 gained filtrate reduced in volume to PH >=3, interpolation pure water regulation precious metal concentration, to 1%, adjusts After solution can be directly used in production as the precious metal raw material that new noble metal catalyst produces.Precious metal concentration utilizes inductance Coupled plasma optical emission spectrogrph detects.The final noble metal response rate reaches 99.2%.
Embodiment 3
Step 1, puts into the noble metal catalyst of recovery in the reactor filling water, stirs and is added thereto to sulfuration Sodium and activated carbon, after continuing stirring 4h, centrifugation, filter cake is standby;Wherein, noble metal catalyst is 1:5 with the amount ratio of water. Noble metal catalyst is 1:0.10 with the amount ratio of sodium sulfide, and sodium sulfide is 1:3 with the amount ratio of activated carbon.
Step 2, puts in Muffle furnace by step 1 gained filter cake, after burning 8h, obtains slag at 800 DEG C, standby.
Step 3, pulverizes step 2 gained slag, crosses 300 eye mesh screens, siftage is placed in the mixing of hydrochloric acid and hydrogen peroxide In liquid dissolve, with after through accurate filter filter, filtrate is standby;Wherein, siftage is 1:15 with the amount ratio of mixed liquor.Mixing In liquid, hydrochloric acid is 1:1 with the amount ratio of hydrogen peroxide.
Step 4, by step 3 gained filtrate reduced in volume to PH >=3, interpolation pure water regulation precious metal concentration, to 2%, adjusts After solution can be directly used in production as the precious metal raw material that new noble metal catalyst produces.Precious metal concentration utilizes inductance Coupled plasma optical emission spectrogrph detects.The final noble metal response rate reaches 99.5%.

Claims (6)

1. the method reclaiming noble metal from discarded noble metal catalyst, it is characterised in that specifically real according to following steps Execute:
Step 1, puts into the noble metal catalyst of recovery in the reactor filling water, stir and be added thereto to sodium sulfide and Activated carbon, after continuing stirring 2~4h, centrifugation, filter cake is standby;
Step 2, puts in Muffle furnace by step 1 gained filter cake, after burning 8~10h, obtains slag at 600~800 DEG C, standby;
Step 3, pulverizes step 2 gained slag, crosses 200~300 eye mesh screens, siftage is placed in the mixing of hydrochloric acid and hydrogen peroxide In liquid dissolve, with after through accurate filter filter, filtrate is standby;
Step 4, by step 3 gained filtrate reduced in volume to PH >=3, adds pure water regulation precious metal concentration to 0.5-2%, adjustment After solution can be directly used in production as the precious metal raw material that new noble metal catalyst produces.
A kind of method reclaiming noble metal from discarded noble metal catalyst the most according to claim 1, it is characterised in that In step 1, noble metal catalyst is 1:3~5 with the amount ratio of water.
A kind of method reclaiming noble metal from discarded noble metal catalyst the most according to claim 1, it is characterised in that In step 1, noble metal catalyst is 1:0.05~0.10 with the amount ratio of sodium sulfide, and sodium sulfide is 1 with the amount ratio of activated carbon: 2~3.
A kind of method reclaiming noble metal from discarded noble metal catalyst the most according to claim 1, it is characterised in that In step 3, siftage is 1:8~15 with the amount ratio of mixed liquor.
A kind of method reclaiming noble metal from discarded noble metal catalyst the most according to claim 1, it is characterised in that In step 3, in mixed liquor, hydrochloric acid is 3:1~3 with the amount ratio of hydrogen peroxide.
A kind of method reclaiming noble metal from discarded noble metal catalyst the most according to claim 1,
It is characterized in that, in step 4, precious metal concentration utilizes inductive coupling plasma emission spectrograph to detect.
CN201610792867.4A 2016-08-31 2016-08-31 A kind of method reclaiming noble metal from discarded noble metal catalyst Pending CN106282578A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111004923A (en) * 2019-12-13 2020-04-14 昆山全亚冠环保科技有限公司 Preparation method and use method of precious metal recovery adsorption material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1153219A (en) * 1995-12-29 1997-07-02 中国科学院新疆化学研究所 Method for extraction of gold from coal-oil gold-carried aggregate (gold chamber)
CN104032143A (en) * 2014-05-15 2014-09-10 浙江省冶金研究院有限公司 Recycling and purifying method of waste palladium-carbon catalyst

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1153219A (en) * 1995-12-29 1997-07-02 中国科学院新疆化学研究所 Method for extraction of gold from coal-oil gold-carried aggregate (gold chamber)
CN104032143A (en) * 2014-05-15 2014-09-10 浙江省冶金研究院有限公司 Recycling and purifying method of waste palladium-carbon catalyst

Non-Patent Citations (3)

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Title
屠海令等: "《有色金属冶金、材料、再生与环保》", 31 January 2003, 化学工业出版社 *
杨建文等: "废催化剂选择法浸渣中提取钯新工艺", 《过程工程学报》 *
杨洪飚: "失效载体催化剂回收铂族金属工艺和技术", 《上海有色金属》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111004923A (en) * 2019-12-13 2020-04-14 昆山全亚冠环保科技有限公司 Preparation method and use method of precious metal recovery adsorption material

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Application publication date: 20170104