CN115595451A - Method for recovering gold from gold-plating wastewater - Google Patents

Method for recovering gold from gold-plating wastewater Download PDF

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Publication number
CN115595451A
CN115595451A CN202211164175.7A CN202211164175A CN115595451A CN 115595451 A CN115595451 A CN 115595451A CN 202211164175 A CN202211164175 A CN 202211164175A CN 115595451 A CN115595451 A CN 115595451A
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CN
China
Prior art keywords
gold
recovering
wastewater
gold plating
plating
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Pending
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CN202211164175.7A
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Chinese (zh)
Inventor
陈新德
陈雪芳
徐文萍
姚时苗
张海荣
薛兆能
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Anhui Wandong Resin Technology Co ltd
Guangzhou Institute of Energy Conversion of CAS
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Anhui Wandong Resin Technology Co ltd
Guangzhou Institute of Energy Conversion of CAS
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Priority to CN202211164175.7A priority Critical patent/CN115595451A/en
Publication of CN115595451A publication Critical patent/CN115595451A/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
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • C22B11/044Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • 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 method for recovering gold from gold-plating wastewater, relating to the technical field of heavy metal wastewater treatment 4 Or Au (CN) 2 The method has the outstanding advantages of low cost, high efficiency, simple equipment and the like, can obviously reduce the economic and environmental protection pressure of gold plating enterprises in the wastewater treatment process, can realize the harmless treatment and resource utilization of the wastewater, and recovers and obtains the pure gold with the purity of more than 99 percent.

Description

Method for recovering gold from gold-plating wastewater
The technical field is as follows:
the invention relates to the technical field of heavy metal wastewater treatment, in particular to a method for recovering gold from gold-plating wastewater.
Background art:
electroplating production is used as an important surface treatment processing procedure and is mainly applied to the industrial fields of furniture hardware, automobile accessories, high-grade bathrooms, PCBs, electronic components, precise instruments and the like. The gold plating layer has golden yellow appearance, stable chemical property, good ductility, easy polishing, high temperature resistance, easy welding, strong corrosion resistance, good anti-discoloration performance, lower contact resistance, good conductive performance and certain wear resistance, so the gold plating process is widely applied to the electroplating of parts requiring long-term stable electrical parameter performance, such as precise instruments, printing plates, integrated circuits, electronic tube shells, electric contacts and the like. The gold plating solution is generally divided into cyanide plating solution and cyanide-free plating solution, the generated waste water has great harm to the environment and human body, contains a large amount of heavy metal ions and organic compounds, and has great difficulty in waste water treatment.
At present, methods for recovering gold from gold-plating wastewater mainly comprise a solvent extraction method, an electrolytic deposition method and an adsorption method. Solvent extraction is a process of extracting substances from immiscible solution phases using an organic solvent. The extractant generally extracts metal ions into the organic phase by complexation, association, chelation, and the like, while other metals remain in the aqueous phase, and then separates the organic phase from which the gold is stripped. The solvent extraction method has good selectivity and mild reaction conditions. However, at the end of the extraction, a stripping process has to be carried out, the extractant having a stronger tendency to complex with gold ions, which results in higher costs.
Electrodeposition is an electrochemical process in which ions form a metal deposit by applying different potentials or amperages with good selectivity and high product purity. However, copper is co-precipitated with gold during electrolysis, which seriously affects the grade and recovery rate of gold.
The adsorption method has the advantages of high efficiency, low cost, energy conservation, environmental protection, easy operation and the like, and is widely applied to a plurality of fields of chemical industry, petroleum, metal smelting and the like. The adsorbents commonly used are mainly activated carbon, adsorption resins and ion exchange resins. The activated carbon is mainly microporous and has good adsorption performance, but the adsorption rate is slow, the desorption is difficult, the reuse is difficult, and the secondary pollution is easy to cause. The adsorption resin can realize the selective separation, enrichment and recovery of a certain specific substance from wastewater by accessing different surface functional groups, is easy to elute and has good repeatability, but mainly takes physical adsorption as the main part and has weaker adsorption force. The ion exchange resin realizes adsorption of adsorbate through electrostatic interaction, ion exchange action and the like with the adsorbate, and mainly adopts chemical adsorption.
Therefore, the technical route of recovering and enriching gold from the gold-plating wastewater by using the macroporous weak base anion exchange resin special for gold extraction with high adsorption capacity and high adsorption selectivity is developed, the harmless treatment and resource utilization of the gold-plating wastewater can be realized, and the method has important significance for improving the quality of ecological environment, ensuring the health of people and preventing the risk of ecological environment.
The invention content is as follows:
the invention aims to solve the technical problem of providing a method for recovering gold from gold-plating wastewater, which adopts macroporous weak base anion exchange resin special for gold extraction to efficiently recover gold from the gold-plating wastewater, wherein the purity of the gold can reach more than 99 percent.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for recovering gold from gold plating wastewater comprises the following steps:
(1) Loading the macroporous weak base anion exchange resin special for gold extraction into a glass fixed bed column;
(2) Pumping the gold-plating wastewater into a glass fixed bed column at a fixed flow rate for gold adsorption, and obtaining gold-loaded resin when the concentration of an effluent liquid is equal to that of an influent liquid and the adsorption is saturated;
(3) Eluting the gold-loaded resin by using an eluant, evaporating the eluant to recover a solvent, and burning the obtained precipitate at high temperature to obtain crude gold;
(4) And (3) pickling the crude gold, heating to boil, standing overnight, filtering to remove supernatant, washing the gold simple substance with water, and drying to obtain pure gold.
Preferably, the macroporous weak base anion exchange resin special for gold extraction in the step (1) is obtained by a preparation method of patent CN 113042113A.
Preferably, the filling height of the macroporous weak base anion exchange resin special for gold extraction in the step (1) is 0.6-1 m.
Preferably, the gold plating wastewater in step (2) is wastewater generated in a potassium cyanide gold plating process and a chloroauric acid gold plating process.
Preferably, the fixed flow rate in step (2) is 20 to 40L/L resin.
Preferably, the eluent in the step (3) is an acetone hydrochloride solution, and the acetone hydrochloride solution is prepared from hydrochloric acid, water and acetone in a mass ratio of 1.
Preferably, the dosage ratio of the eluent to the gold-loaded resin in the step (3) is 8.
Preferably, the elution temperature in the step (3) is 20-30 ℃; the evaporation temperature is 56-57 ℃.
Preferably, the burning temperature in the step (3) is 480-530 ℃, and the burning time is 1-3 h.
Preferably, industrial nitric acid is adopted in the acid washing in the step (4), and the using amount ratio of the industrial nitric acid to the crude gold is 80mL (1-2) g.
The invention has the beneficial effects that: the invention uses-NH-functional group of macroporous weak base anion exchange resin special for extracting gold and AuCl in wastewater 4 - Or Au (CN) 2 - The method has the outstanding advantages of low cost, high efficiency, simple equipment and the like, can obviously reduce the economic and environmental protection pressure of gold plating enterprises in the wastewater treatment process, and can realize the harmless treatment and resource utilization of the wastewater.
Description of the drawings:
FIG. 1 is a schematic view of the process for recovering gold from gold plating wastewater according to the present invention.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained by combining the specific embodiments and the drawings.
Example 1
(1) The macroporous weak base anion exchange resin special for gold extraction prepared in example 2 of patent CN113042113A is filled into a glass fixed bed column, and the height of the filled column is 0.6m.
(2) Pumping the gold-plating wastewater into a glass fixed bed column for gold adsorption at the flow rate of 20L/L resin, and stopping the pump when the adsorption saturation is reached to obtain the gold-loaded resin.
(3) Eluting the gold-loaded resin by using an acetone hydrochloride solution (prepared from hydrochloric acid, water and acetone in a mass ratio of 1; evaporating the eluate to recover acetone at 57 deg.C; the obtained precipitate is burned at 480 ℃ for 3h to obtain crude gold.
(4) And (2) pickling the crude gold by using industrial nitric acid, wherein the use ratio of the industrial nitric acid to the crude gold is 80mL (1g), heating to boil for 20min, standing overnight, filtering to remove supernate, washing a gold simple substance by using pure water, and drying to obtain pure gold with the purity of 99.23%.
Example 2
(1) The macroporous weak base anion exchange resin special for gold extraction prepared in example 1 of patent CN113042113A is filled into a glass fixed bed column, and the height of the filled column is 0.8m.
(2) Pumping the gold-plating wastewater into a glass fixed bed column for gold adsorption at the flow rate of 30L/L resin, and stopping the pump when the adsorption saturation is reached to obtain the gold-loaded resin.
(3) Eluting the gold-loaded resin by adopting an acetone hydrochloride solution (prepared by hydrochloric acid, water and acetone in a mass ratio of 1; evaporating the eluate to recover acetone at 57 deg.C; the obtained precipitate is burned at 530 ℃ for 1h to obtain crude gold.
(4) The method comprises the following steps of pickling crude gold by using industrial nitric acid, wherein the using amount ratio of the industrial nitric acid to the crude gold is 80mL, heating to boil for 20min, standing overnight, filtering to remove supernate, washing a gold simple substance by using pure water, and drying to obtain pure gold, wherein the purity of the pure gold is 99.52%.
Example 3
(1) The macroporous weak base anion exchange resin special for gold extraction prepared in example 3 of patent CN113042113A is filled into a glass fixed bed column, and the height of the filled column is 1.0m.
(2) Pumping the gold-plating wastewater into a glass fixed bed column for gold adsorption at the flow rate of 40L/L resin, and stopping the pump when the adsorption saturation is reached to obtain the gold-loaded resin.
(3) Eluting the gold-loaded resin by using an acetone hydrochloride solution (prepared by hydrochloric acid, water and acetone in a mass ratio of 0.5 to 0.5); evaporating the eluate to recover acetone at 56 deg.C; the obtained precipitate is burned at 500 ℃ for 2h to obtain crude gold.
(4) And (2) pickling the crude gold by using industrial nitric acid, wherein the using amount ratio of the industrial nitric acid to the crude gold is 80mL (1g), heating to boil for 20min, standing overnight, filtering to remove a supernatant, washing a gold simple substance by using pure water, and drying to obtain pure gold, wherein the purity is 99.90%.
Example 4
(1) The macroporous weak base anion exchange resin special for gold extraction prepared in example 3 of patent CN113042113A is filled into a glass fixed bed column, and the height of the filled column is 0.9m.
(2) Pumping the gold-plating wastewater into a glass fixed bed column for gold adsorption at the flow rate of 35L/L resin, and stopping the pump when the adsorption saturation is reached to obtain the gold-loaded resin.
(3) Eluting the gold-loaded resin by using an acetone hydrochloride solution (prepared from hydrochloric acid, water and acetone in a mass ratio of 1.5 to 8.5), wherein the use ratio of the acetone hydrochloride solution to the gold-loaded resin is 8mL 1g, and the elution temperature is 30 ℃; evaporating the eluate to recover acetone at 57 deg.C; the obtained precipitate is burned at 530 ℃ for 1h to obtain crude gold.
(4) The method comprises the following steps of pickling crude gold by using industrial nitric acid, wherein the using amount ratio of the industrial nitric acid to the crude gold is 80mL, heating to boil for 20min, standing overnight, filtering to remove supernate, washing a gold simple substance by using pure water, and drying to obtain pure gold, wherein the purity of the pure gold is 99.98%.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A method for recovering gold from gold plating wastewater is characterized by comprising the following steps:
(1) Loading macroporous weak base anion exchange resin special for gold extraction into a glass fixed bed column;
(2) Pumping the gold-plating wastewater into a glass fixed bed column at a fixed flow rate for gold adsorption, and obtaining gold-loaded resin when the effluent concentration is equal to the influent concentration and the effluent concentration reaches adsorption saturation;
(3) Eluting the gold-loaded resin by using an eluant, evaporating the eluant to recover the solvent, and burning the obtained precipitate at high temperature to obtain crude gold;
(4) And (3) pickling the crude gold, heating to boil, standing overnight, filtering to remove supernatant, washing the gold simple substance with water, and drying to obtain pure gold.
2. The method for recovering gold from gold plating wastewater according to claim 1, characterized in that: the macroporous weak base anion exchange resin special for gold extraction in the step (1) is obtained by adopting a preparation method of patent CN 113042113A.
3. The method for recovering gold from gold plating wastewater according to claim 1, characterized in that: the filling height of the macroporous weak base anion exchange resin special for gold extraction in the step (1) is 0.6-1 m.
4. The method for recovering gold from gold plating wastewater according to claim 1, characterized in that: the gold plating wastewater in the step (2) is wastewater generated by a potassium cyanide gold plating process and a chloroauric acid gold plating process.
5. The method for recovering gold from gold plating waste water according to claim 1, characterized in that: the fixed flow rate in the step (2) is 20-40L/L resin.
6. The method for recovering gold from gold plating waste water according to claim 1, characterized in that: the eluent in the step (3) is an acetone hydrochloride solution, and the acetone hydrochloride solution is prepared from hydrochloric acid, water and acetone according to a mass ratio of 1.
7. The method for recovering gold from gold plating waste water according to claim 1, characterized in that: the dosage ratio of the eluent to the gold-loaded resin in the step (3) is 8.
8. The method for recovering gold from gold plating waste water according to claim 1, characterized in that: the elution temperature in the step (3) is 20-30 ℃; the evaporation temperature is 56-57 ℃.
9. The method for recovering gold from gold plating wastewater according to claim 1, characterized in that: in the step (3), the burning temperature is 480-530 ℃, and the burning time is 1-3 h.
10. The method for recovering gold from gold plating waste water according to claim 1, characterized in that: in the step (4), industrial nitric acid is adopted for pickling, and the using amount ratio of the industrial nitric acid to the crude gold is 80mL (1-2) g.
CN202211164175.7A 2022-09-23 2022-09-23 Method for recovering gold from gold-plating wastewater Pending CN115595451A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1987000072A1 (en) * 1985-06-28 1987-01-15 Resource Technology Associates Method for recovery of cyanide from waste streams
CA2131575A1 (en) * 1993-09-08 1995-03-09 Keishiro Hata Agent for treating metal ions in an aqueous solution, process for producing the metal ion-treating agent and method for treating metal ions in an aqueous solution
CN1203280A (en) * 1997-06-23 1998-12-30 徐胜 Wet-metallurgical non-cyanogen process and its special equipment
CN101618898A (en) * 2008-07-02 2010-01-06 深圳市众恒隆实业有限公司 Method for recovering gold, platinum and porpezite from acidic waste water by ion exchange
CN101660048A (en) * 2009-09-24 2010-03-03 无锡市霄鹰环境科技有限公司 Multilevel processing technology for recovering and utilizing precious metal wastes or waste liquid
CN102531233A (en) * 2011-12-21 2012-07-04 邵梦馨 Heavy-metal-containing electroplating wastewater treatment and heavy metal recycling method
CN113042113A (en) * 2021-03-22 2021-06-29 中国科学院广州能源研究所 Preparation method of macroporous weak base anion exchange resin special for gold extraction

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1987000072A1 (en) * 1985-06-28 1987-01-15 Resource Technology Associates Method for recovery of cyanide from waste streams
CA2131575A1 (en) * 1993-09-08 1995-03-09 Keishiro Hata Agent for treating metal ions in an aqueous solution, process for producing the metal ion-treating agent and method for treating metal ions in an aqueous solution
CN1203280A (en) * 1997-06-23 1998-12-30 徐胜 Wet-metallurgical non-cyanogen process and its special equipment
CN101618898A (en) * 2008-07-02 2010-01-06 深圳市众恒隆实业有限公司 Method for recovering gold, platinum and porpezite from acidic waste water by ion exchange
CN101660048A (en) * 2009-09-24 2010-03-03 无锡市霄鹰环境科技有限公司 Multilevel processing technology for recovering and utilizing precious metal wastes or waste liquid
CN102531233A (en) * 2011-12-21 2012-07-04 邵梦馨 Heavy-metal-containing electroplating wastewater treatment and heavy metal recycling method
CN113042113A (en) * 2021-03-22 2021-06-29 中国科学院广州能源研究所 Preparation method of macroporous weak base anion exchange resin special for gold extraction

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