CN114150160A - Method for recovering gold from waste gold-carbon catalyst - Google Patents

Method for recovering gold from waste gold-carbon catalyst Download PDF

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Publication number
CN114150160A
CN114150160A CN202111274709.7A CN202111274709A CN114150160A CN 114150160 A CN114150160 A CN 114150160A CN 202111274709 A CN202111274709 A CN 202111274709A CN 114150160 A CN114150160 A CN 114150160A
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gold
carbon catalyst
recovering
slag
spent
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CN202111274709.7A
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Inventor
许晓龙
王光应
赵羽
薛晚林
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Anhui Yuanchen Environmental Protection Science and Technology Co Ltd
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Anhui Yuanchen Environmental Protection Science and Technology Co Ltd
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Priority to CN202111274709.7A priority Critical patent/CN114150160A/en
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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
    • C22B11/00Obtaining noble metals
    • C22B11/02Obtaining noble metals by dry processes
    • C22B11/021Recovery of noble metals from waste materials
    • C22B11/026Recovery of noble metals from waste materials 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
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • C22B11/048Recovery of noble metals from waste materials 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
    • C22B7/001Dry processes
    • 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

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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)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Processing Of Solid Wastes (AREA)
  • Catalysts (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a method for recovering gold from a waste gold-carbon catalyst, relates to the technical field of precious metal catalyst recovery, and is provided based on the problem of the defect that corrosive gas is generated in the gold recovery process of the existing waste gold-carbon catalyst. The method comprises the following steps: (1) roasting the waste gold-carbon catalyst; (2) ball milling treatment; (3) the configuration contains KI and I2The mixed solution is used as the leaching solution of Au in the crude gold slag; (4) immersing the ball-milled coarse gold slag into a solution containing KI and I2In the Au leaching solution; (5) filtering to obtain an Au-containing filtrate; (6) and separating to obtain the high-purity simple substance Au. Compared with the prior art for recovering Au in the waste gold-carbon catalyst, KI-I is used in the method2The dissolving leachate system is used for leaching Au, and the use of aqua regia, hydrochloric acid, sodium chlorate and bis-sodium chlorate in the traditional acid leaching and dissolving process is avoided on the premise of ensuring higher Au recovery rateOxygen water and the like may generate corrosive gas.

Description

Method for recovering gold from waste gold-carbon catalyst
Technical Field
The invention relates to the technical field of precious metal catalyst recovery, in particular to a method for recovering gold from a waste gold-carbon catalyst.
Background
Gold (Au) has excellent catalytic performance for many chemical reaction processes, for example, gold can be loaded on an activated carbon carrier to be used in the process of preparing vinyl chloride through acetylene hydrochlorination so as to replace the mercury catalyst used in the industry at present, but as one of noble metals, the high cost of gold per se limits the industrial application of gold. Therefore, the recycling of the gold catalyst becomes the key for realizing the industrial application of the gold catalyst.
The method for recovering noble metal from waste noble metal catalyst usually adopts aqua regia and H2O2-HCl system or HCl-NaClO3The system is realized by the steps of dissolving and leaching, precipitation, reduction and the like. Chinese patent CN201911003157.9 discloses a method for dissolving gold in waste gold-carbon catalyst by using aqua regia; chinese patent CN200710009132.0 discloses a method for dissolving palladium in a waste supported palladium catalyst by using a hydrochloric acid-hydrogen peroxide system; chinese patent CN201410677816.8 discloses a method for recovering precious metals from waste automobile exhaust catalysts, and the precious metal acid leaching system adopted is a mixed solution of sodium chloride, sodium chlorate and sulfuric acid.
The three methods for leaching the precious metals in the waste precious metal catalyst have the defect of generating corrosive gas in the implementation process, and the process has certain insecurity.
Disclosure of Invention
The invention aims to solve the technical problem of the defect that corrosive gas is generated in the gold recovery process in the existing waste gold-carbon catalyst.
The invention solves the technical problems through the following technical means:
a method for recovering gold from a waste gold-carbon catalyst comprises the following steps:
(1) roasting the waste gold-carbon catalyst to remove carbon carriers to obtain crude gold slag with Au as a main component;
(2) putting the coarse gold slag obtained in the step (1) into a planetary ball mill for ball milling treatment;
(3) the configuration contains KI and I2The mixed solution is used as the leaching solution of Au in the crude gold slag; wherein the mass concentration of KI is 20-30 percent, I2The mass concentration of (A) is 10-20%;
(4) according to the natureThe weight ratio is 5-10:100, and the ball-milled crude gold slag is immersed into the alloy containing KI and I2Stirring the Au leaching solution to enable the crude gold slag to suspend in the leaching solution, and then heating and insulating the mixed solution;
(5) stopping heating and stirring, filtering the mixed solution to obtain an Au-containing filtrate, and measuring the concentration of Au in the Au filtrate by ICP (inductively coupled plasma);
(6) adding analytically pure hydrochloric acid into the Au-containing filtrate, adjusting the pH of the solution to 5-7, and then adding Na2SO3Adding a proper amount of anhydrous Na into the Au according to the stoichiometric ratio of 1.005:22SO3Fully stirring to reduce the gold in the filtrate into a simple substance to form a precipitate, and filtering and separating to obtain the high-purity simple substance Au.
The present invention uses KI-I2The dissolving leaching liquid system leaches Au, and avoids the danger of generating corrosive gas due to the use of aqua regia, hydrochloric acid, sodium chlorate, hydrogen peroxide and other substances in the traditional acid leaching and dissolving process on the premise of ensuring higher Au recovery rate.
Preferably, the temperature for calcination in the step (1) is 800-.
Preferably, the roasting time in the step (1) is 2-4 h.
Preferably, the rotation speed of the ball milling in the step (2) is 600-900 rpm.
Preferably, the ball milling time in the step (2) is 2-4 h.
Preferably, the granularity of the ball milling output material in the step (2) is controlled to be 0.1-0.5 mu m.
Preferably, the stirring speed in the step (4) is 300-500 rpm.
Preferably, the stirring time in the step (4) is 6-10 h.
Preferably, the temperature of heating in the step (4) is 50-90 ℃.
Preferably, the temperature keeping time in the step (4) is 6-10 h.
The invention has the following beneficial effects: compared with the prior art for recovering Au in the waste gold-carbon catalyst, KI-I is used in the method2The dissolving leaching liquid system can leach Au, and avoids the problem of dissolving Au by traditional acid leaching on the premise of ensuring higher Au recovery rateThe process uses aqua regia, hydrochloric acid, sodium chlorate, hydrogen peroxide and other substances to generate corrosive gas.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
A method for recovering gold from a waste gold-carbon catalyst comprises the following steps:
(1) 1kg of waste gold carbon catalyst is roasted at 850 ℃ for 3h to remove carrier active carbon, and gold-containing roasting slag is obtained;
(2) putting the gold-containing roasting slag obtained in the step (1) into a planetary ball mill for ball milling, wherein the ball milling rotation speed is 600rpm, the ball milling time is 2 hours, and the discharging particle size is controlled to be 0.5 mu m;
(3) the configuration contains KI and I2The mixed solution is used as the leaching solution of Au in the crude gold slag, wherein the mass concentration of KI is 30 percent, and I2The mass concentration of (2);
(4) immersing the ball-milled coarse gold slag into KI and I according to the mass ratio of 10:1002Stirring to enable the crude gold slag to suspend in the leaching solution, wherein the stirring speed is 500rpm, the stirring time is 10 hours, then heating the mixed solution to 90 ℃, and preserving heat for 10 hours;
(5) stopping heating and stirring, filtering the mixed solution to obtain an Au-containing filtrate, and measuring the concentration of Au in the Au filtrate by ICP (inductively coupled plasma);
(6) adding analytically pure hydrochloric acid to the Au-containing filtrate, adjusting the pH of the solution to 5, and then adjusting the pH to Na2SO3Adding a proper amount of anhydrous Na into the Au according to the stoichiometric ratio of 1.005:22SO3Fully stirring to reduce the gold in the filtrate into a simple substance to form a precipitate, filtering and separating to obtain the high-purity simple substance Au, wherein the purity of the gold powder is 99.8 percent by ICP (inductively coupled plasma).
According to the concentration and volume of Au in the Au-containing filtrate measured in the step (5) and the mass of the simple substance Au powder obtained in the step (6), the recovery rate of Au from the waste gold carbon in the embodiment is calculated to be 98%.
Example 2
A method for recovering gold from a waste gold-carbon catalyst comprises the following steps:
(1) 0.5kg of waste gold carbon catalyst is roasted at 850 ℃ for 3h to remove carrier active carbon, and gold-containing roasting slag is obtained;
(2) putting the gold-containing roasting slag obtained in the step (1) into a planetary ball mill for ball milling, wherein the ball milling rotation speed is 900rpm, the ball milling time is 4 hours, and the discharging particle size is controlled to be 0.1 mu m;
(3) the configuration contains KI and I2The mixed solution is used as leaching solution of Au in the crude gold slag, wherein the mass concentration of KI is 20 percent, and I2The mass concentration of (2) is 10%;
(4) immersing the ball-milled coarse gold slag into KI and I according to the mass ratio of 5:1002Stirring to enable the crude gold slag to suspend in the leaching solution, wherein the stirring speed is 300rpm, the stirring time is 10 hours, then heating the mixed solution to 50 ℃, and preserving heat for 10 hours;
(5) stopping heating and stirring, filtering the mixed solution to obtain an Au-containing filtrate, and measuring the concentration of Au in the Au filtrate by ICP (inductively coupled plasma);
(6) adding analytically pure hydrochloric acid to the Au-containing filtrate, adjusting the pH of the solution to 6.5, and then adjusting the pH to Na2SO3Adding a proper amount of anhydrous Na into the Au according to the stoichiometric ratio of 1.005:22SO3Fully stirring to reduce the gold in the filtrate into a simple substance to form a precipitate, filtering and separating to obtain the high-purity simple substance Au, wherein the purity of the gold powder is 99.9 percent by ICP (inductively coupled plasma).
According to the concentration and volume of Au in the Au-containing filtrate measured in the step (5) and the mass of the simple substance Au powder obtained in the step (6), the recovery rate of Au from the waste gold carbon in the embodiment is calculated to be 99%.
Example 3
A method for recovering gold from a waste gold-carbon catalyst comprises the following steps:
(1) 0.5kg of waste gold carbon catalyst is roasted at 850 ℃ for 3h to remove carrier active carbon, and gold-containing roasting slag is obtained;
(2) putting the gold-containing roasting slag obtained in the step (1) into a planetary ball mill for ball milling, wherein the ball milling rotation speed is 750rpm, the ball milling time is 3 hours, and the discharging particle size is controlled to be 0.25 mu m;
(3) the configuration contains KI and I2The mixed solution is used as leaching solution of Au in the crude gold slag, wherein the mass concentration of KI is 20 percent, and I2The mass concentration of (2);
(4) immersing the ball-milled coarse gold slag into KI and I according to the mass ratio of 7.5:1002Stirring to enable the crude gold slag to suspend in the leaching solution, wherein the stirring speed is 400rpm, the stirring time is 6 hours, then heating the mixed solution to 75 ℃, and preserving heat for 8 hours;
(5) stopping heating and stirring, filtering the mixed solution to obtain an Au-containing filtrate, and measuring the concentration of Au in the Au filtrate by ICP (inductively coupled plasma);
(6) adding analytically pure hydrochloric acid to the Au-containing filtrate, adjusting the pH of the solution to 7, and then adjusting the pH to Na2SO3Adding a proper amount of anhydrous Na into the Au according to the stoichiometric ratio of 1.005:22SO3Fully stirring to reduce the gold in the filtrate into a simple substance to form a precipitate, filtering and separating to obtain the high-purity simple substance Au, wherein the purity of the gold powder is 99.5 percent by ICP (inductively coupled plasma).
According to the concentration and volume of Au in the Au-containing filtrate measured in the step (5) and the mass of the simple substance Au powder obtained in the step (6), the recovery rate of Au from the waste gold carbon in the embodiment is calculated to be 99%.
Comparative example
A method for recovering gold from a waste gold-carbon catalyst comprises the following steps:
(1) 1kg of waste gold carbon catalyst is roasted at 850 ℃ for 3h to remove carrier active carbon, and gold-containing roasting slag is obtained;
(2) putting the gold-containing roasting slag obtained in the step (1) into a planetary ball mill for ball milling, wherein the ball milling rotation speed is 600rpm, the ball milling time is 2 hours, and the discharging particle size is controlled to be 0.5 mu m;
(3) the configuration contains KI and I2The mixed solution is used as leaching solution of Au in the crude gold slag, wherein the mass concentration of KI is 10 percent, and I25% of (A);
(4) immersing the ball-milled coarse gold slag into KI and I according to the mass ratio of 4:1002Stirring to enable the crude gold slag to suspend in the leaching solution, wherein the stirring speed is 300rpm, the stirring time is 6 hours, then heating the mixed solution to 90 ℃, and preserving heat for 10 hours;
(5) stopping heating and stirring, filtering the mixed solution to obtain an Au-containing filtrate, and measuring the concentration of Au in the Au filtrate by ICP (inductively coupled plasma);
(6) adding analytically pure hydrochloric acid to the Au-containing filtrate, adjusting the pH of the solution to 5, and then adjusting the pH to Na2SO3Adding a proper amount of anhydrous Na into the Au according to the stoichiometric ratio of 1.005:22SO3Fully stirring to reduce the gold in the filtrate into a simple substance to form a precipitate, filtering and separating to obtain the high-purity simple substance Au, wherein the purity of the gold powder is 99.8 percent by ICP (inductively coupled plasma).
According to the concentration and volume of Au in the Au-containing filtrate measured in the step (5) and the mass of the simple substance Au powder obtained in the step (6), the recovery rate of Au from the waste gold carbon in the embodiment is 89% by calculation.
In conclusion, compared with the prior art for recovering Au in the waste gold-carbon catalyst, KI-I is used in the method2The dissolving leaching liquid system leaches Au, and avoids the danger of generating corrosive gas due to the use of aqua regia, hydrochloric acid, sodium chlorate, hydrogen peroxide and other substances in the traditional acid leaching and dissolving process on the premise of ensuring higher Au recovery rate.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for recovering gold from a waste gold-carbon catalyst is characterized by comprising the following steps:
(1) roasting the waste gold-carbon catalyst to remove carbon carriers to obtain crude gold slag with Au as a main component;
(2) putting the coarse gold slag obtained in the step (1) into a planetary ball mill for ball milling treatment;
(3) the configuration contains KI and I2The mixed solution is used as the leaching solution of Au in the crude gold slag; wherein the mass concentration of KI is 20-30 percent, I2The mass concentration of (A) is 10-20%;
(4) immersing the ball-milled coarse gold slag into KI and I according to the mass ratio of 5-10:1002Stirring the Au leaching solution to enable the crude gold slag to suspend in the leaching solution, and then heating and insulating the mixed solution;
(5) stopping heating and stirring, filtering the mixed solution to obtain an Au-containing filtrate, and measuring the concentration of Au in the Au filtrate by ICP (inductively coupled plasma);
(6) adding analytically pure hydrochloric acid into the Au-containing filtrate, adjusting the pH of the solution to 5-7, and then adding Na2SO3Adding a proper amount of anhydrous Na into the Au according to the stoichiometric ratio of 1.005:22SO3Fully stirring to reduce the gold in the filtrate into a simple substance to form a precipitate, and filtering and separating to obtain the high-purity simple substance Au.
2. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the roasting temperature in the step (1) is 800-900 ℃.
3. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the roasting time in the step (1) is 2-4 h.
4. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the rotation speed of ball milling in the step (2) is 600-900 rpm.
5. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the ball milling time in the step (2) is 2-4 h.
6. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the granularity of the ball-milled material in the step (2) is controlled to be 0.1-0.5 mu m.
7. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the stirring speed in the step (4) is 300-500 rpm.
8. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the stirring time in the step (4) is 6-10 h.
9. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the heating temperature in the step (4) is 50-90 ℃.
10. The method for recovering gold from a spent gold-on-carbon catalyst according to claim 1, wherein: the heat preservation time in the step (4) is 6-10 h.
CN202111274709.7A 2021-10-29 2021-10-29 Method for recovering gold from waste gold-carbon catalyst Pending CN114150160A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4670052A (en) * 1985-08-07 1987-06-02 Noranda, Inc. Process for the recovery of gold from a precious metal bearing sludge concentrate
US5328669A (en) * 1993-01-26 1994-07-12 South Dakota School Of Mines And Technology Extraction of precious metals from ores and other precious metal containing materials using halogen salts
WO1998005569A1 (en) * 1996-08-02 1998-02-12 Jacques Leibovitz Gold extraction from ores with chemicals regeneration
US5948140A (en) * 1996-06-25 1999-09-07 Paul L. Hickman Method and system for extracting and refining gold from ores
CN104762479A (en) * 2015-04-01 2015-07-08 郴州雄风环保科技有限公司 Process for comprehensively recovering rare and precious metals including gold, silver, platinum and palladium from gold-bearing wastes
JP2017133084A (en) * 2016-01-29 2017-08-03 Jx金属株式会社 Method of treating gold and silver slag
CN111074303A (en) * 2020-01-19 2020-04-28 北京科技大学 Method for separating antimony and gold by crude antimony non-anode-residue electrolysis
JP2021080511A (en) * 2019-11-15 2021-05-27 学校法人 関西大学 Gold recovery method, gold recovery agent and gold recovery apparatus

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4670052A (en) * 1985-08-07 1987-06-02 Noranda, Inc. Process for the recovery of gold from a precious metal bearing sludge concentrate
US5328669A (en) * 1993-01-26 1994-07-12 South Dakota School Of Mines And Technology Extraction of precious metals from ores and other precious metal containing materials using halogen salts
US5948140A (en) * 1996-06-25 1999-09-07 Paul L. Hickman Method and system for extracting and refining gold from ores
WO1998005569A1 (en) * 1996-08-02 1998-02-12 Jacques Leibovitz Gold extraction from ores with chemicals regeneration
CN104762479A (en) * 2015-04-01 2015-07-08 郴州雄风环保科技有限公司 Process for comprehensively recovering rare and precious metals including gold, silver, platinum and palladium from gold-bearing wastes
JP2017133084A (en) * 2016-01-29 2017-08-03 Jx金属株式会社 Method of treating gold and silver slag
JP2021080511A (en) * 2019-11-15 2021-05-27 学校法人 関西大学 Gold recovery method, gold recovery agent and gold recovery apparatus
CN111074303A (en) * 2020-01-19 2020-04-28 北京科技大学 Method for separating antimony and gold by crude antimony non-anode-residue electrolysis

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Title
张亦飞, 冶金工业出版社 *

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Application publication date: 20220308