CN110106354A - A method of extracting gold from useless circuit board - Google Patents

A method of extracting gold from useless circuit board Download PDF

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Publication number
CN110106354A
CN110106354A CN201910380498.1A CN201910380498A CN110106354A CN 110106354 A CN110106354 A CN 110106354A CN 201910380498 A CN201910380498 A CN 201910380498A CN 110106354 A CN110106354 A CN 110106354A
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gold
circuit board
golden
dbc
useless circuit
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CN201910380498.1A
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CN110106354B (en
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黄魁
黄朝冉
董海丽
蒋中伟
陈继文
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Guangxi University
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Guangxi University
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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
    • C22B11/046Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/262Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds using alcohols or phenols
    • 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)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The method that the invention discloses a kind of to extract gold from useless circuit board, comprising the following steps: (1) useless circuit board is crushed, crosses sieve, obtained containing golden object powder;(2) golden object powder will be contained to be pre-processed with nitric acid, obtain gold-containing residue;(3) gold-containing residue is added in chloroazotic acid and is cleared up, obtained containing Jin Wangshui;(4) golden chloroazotic acid and extract liquor hybrid extraction will be contained, at least extracted twice;Extraction carries out extracting gold with the extract liquor of DBC- Isopropanol Solvent, obtains isolating raffinate containing golden organic phase, adding and be sufficiently mixed carry out reextraction with the extract liquor of raffinate same volume after extracting liquid separation for the first time;It wherein, include: DBC the and 20-40% isopropanol of 60-80%, room temperature extraction by percent by volume in the DBC- Isopropanol Solvent;(5) sodium sulfite reduction is added in Xiang Hanjin organic phase, obtains cake of gold.The method that the present invention extracts gold, reextraction rate is up to 96%, and for extraction reduction rate up to 95%, cost reduces by 20%, has apparent economic benefit.

Description

A method of extracting gold from useless circuit board
Technical field
The present invention relates to the field of extracting gold from, in particular to a kind of method that gold is extracted from useless circuit board.
Background technique
It is reported that containing multiple harmful substances such as lead, cadmium, mercury in waste mobile phone part, if directly abandoning seriously to pollute Soil and groundwater.If waste mobile phone is transported to soot to incinerate, plastic shell can also generate the noxious material containing chlorine, even It is level-one carcinogenic substance " dioxin ".Circuit board of mobile phone and shell all brominated flame-retardants, can destroy human health, cause thyroid gland function It can disorder, endocrine disorder and nerve, immune system problem etc..It include a variety of valuable materials in machine internals, including 0.01% gold, 20%~25% copper, 40%~50% recyclable plastic.It is containing recycling key golden in golden dead meal It must try to separate gold with most unclassified stores.The golden system of most common leaching is that chloroazotic acid soaks golden system, because of king Water logging gold system has the advantages that process is simple, gold leaching rate is high, so chloroazotic acid, which soaks golden system, has gradually replaced cyanide gold-leaching method.King The cardinal principle of water logging gold system is that the strong oxidizing property of chloroazotic acid can be the noble metal removal in useless circuit board.However existing extraction The defects of taking technique extraction and recovery gold, the rate of recovery is lower, and cost recovery is high.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The method that the purpose of the present invention is to provide a kind of to extract gold from useless circuit board, to overcome the golden cost of recycling Disadvantage high, the rate of recovery is low.
To achieve the above object, the method that the present invention provides a kind of extracts gold from useless circuit board, comprising the following steps:
(1) useless circuit board is crushed, crosses sieve, obtained containing golden object powder;
(2) step (1) the object powder obtained containing gold is pre-processed with nitric acid, obtains gold-containing residue;
(3) gold-containing residue made from the step (2) is added in chloroazotic acid and is cleared up, obtained containing Jin Wangshui;
(4) step (3) is obtained containing golden chloroazotic acid and extract liquor hybrid extraction, at least extracted twice;Extraction Extracting gold is carried out with the extract liquor of DBC- Isopropanol Solvent, obtains isolating raffinate containing golden organic phase after extracting liquid separation for the first time Liquid adds and is sufficiently mixed carry out reextraction with the extract liquor of raffinate same volume;Wherein, the DBC- Isopropanol Solvent In by percent by volume include: 60-80% DBC and 20-40% isopropanol, room temperature extraction;
(5) containing sodium sulfite reduction is added in golden organic phase, cake of gold will be obtained in the step (6).
Preferably, 35-100 mesh is crossed after circuit board is crushed in above-mentioned technical proposal, in step (1).
Preferably, in above-mentioned technical proposal, the liquid-solid ratio of chloroazotic acid and gold-containing residue is 60-140ml/g in step (3).
Preferably, in above-mentioned technical proposal, gold-containing residue and the reaction temperature of chloroazotic acid are 25-45 DEG C in step (3).
Preferably, in above-mentioned technical proposal, the reaction of step (3) gold-containing residue and chloroazotic acid is normal-temperature reaction 21-27 hours.
Preferably, in above-mentioned technical proposal, after the processing of step (3) chloroazotic acid, the filtering of golden chloroazotic acid will be contained, obtain containing golden filtrate and Filter residue, then filter residue is subjected to extracting gold with extract liquor.
It preferably, in DBC- Isopropanol Solvent by percent by volume include: 60- in step (4) in above-mentioned technical proposal 80% DBC and 20-40% isopropanol.
Preferably, in above-mentioned technical proposal, the mass concentration of step (5) sulfite sodium solution is 5-10%.
Preferably, in above-mentioned technical proposal, the time containing golden organic phase and sodium sulfite reduction reaction is in step (5) The stream of 60-120S, organic phase and water phase compares for 4-6:2.
Compared with prior art, the invention has the following beneficial effects:
(1) method that the present invention extracts gold from useless circuit board, the DBC- isopropyl alcohol extraction system of use, DBC is in hydrochloric acid Very strong to the extracting power of gold in solution, preferably, isopropanol can form the good hydrotropy system of effect with DBC to selectivity.I.e. DBC- isopropyl alcohol extraction system is synergic solvent extraction, compared with existing single extractant, has extraction efficiency high, at low cost, soaks The advantages such as the time is fast out.It is being stripping agent with sodium sulfite, can carrying out at normal temperature, it is more more economical and square than with oxalic acid solution Just.
(2) method that the present invention extracts gold, golden reextraction rate is up to 96%, and up to 95%, cost reduces extraction reduction rate 20%, there is apparent economic benefit.Gold in used chloroazotic acid leaching waste mobile phone, the advantage with industrial application, process letter It is single, and gold leaching rate is high.Also there is resource circulation utilization, environmentally protective, low in cost, the features such as real operation is strong, tool There are certain economy, environmental benefit.
Detailed description of the invention
Fig. 1 is the process flow chart of the method according to the present invention that gold is extracted from useless circuit board.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members Part or other component parts.
Embodiment 1
A method of extracting gold from useless circuit board, process flow chart is as shown in Figure 1, including physics pretreatment, changing Pretreatment, chloroazotic acid leaching gold are learned, DBC- isopropyl alcohol extraction system extracting gold and sodium sulfite restore golden five parts, specifically include Following steps:
(1) physics pretreatment: waste mobile phone 11 bought from market, through disassembling to obtain useless circuit board manually, using height Circuit board of mobile phone is broken into powder by fast multifunctional crusher.It is screened with 35 mesh unification of the motherland standard inspection sieves, after screening The powder sample 200g that partial size is less than 0.500mm is obtained, as containing golden object powder.
(2) chemical pretreatment: will contain golden object powder 1.0000g in small beaker, and excess HNO is added3Solution is placed in 30 DEG C It reacts in digital display thermostat water bath and filters afterwards for 24 hours, filter residue is washed, obtains gold-containing residue after drying.
(3) chloroazotic acid leaching gold: being added excessive chloroazotic acid for gold-containing residue, and the liquid-solid ratio of gold-containing residue and chloroazotic acid is 140ml/g, and 35 It DEG C heating in water bath for reaction 21 hours, is sealed during reaction with preservative film, aperture exhaust is opened on film.Sample filtering after resolution, obtains To containing golden filtrate and filter residue, golden filtrate will be contained in deionized water constant volume 200mL volumetric flask.Wherein the chloroazotic acid presses volume basis Than for concentrated hydrochloric acid (HCl): concentrated nitric acid (HNO3)=3:1.
(4) golden filtrate and extract liquor hybrid extraction, the extraction extraction of DBC- Isopropanol Solvent DBC- isopropyl alcohol extraction: will be contained Liquid is taken to carry out extracting gold, wherein DBC- isopropyl alcohol extraction system includes 70% DBC, 30% isopropanol by percent by volume, It is stirred under 300r/min blender under room temperature, liquid separation is stood after 5min.It is obtained after extraction liquid separation for the first time containing golden organic phase, separation Raffinate out, level-one extraction yield are 88%.It adds and is sufficiently mixed carry out reextraction with the extract liquor of raffinate same volume, Second level extraction yield is 95%.
(5) multiple saturated organic phase extracted sodium sulfite extraction reduction gold: is entered into the sulfurous that mass concentration is 5% In acid sodium solution reduction reactor, 90S is stirred to react under room temperature, wherein the stream of organic phase and water phase compares for 5:2, i.e. O/A=5: 2。
The extraction rate of the gold of the present embodiment is about 96%, extracts reduction rate 95%, overall recovery is about 93%.
Embodiment 2
A method of extracting gold from useless circuit board, process flow chart is as shown in Figure 1, including physics pretreatment, changing Pretreatment, chloroazotic acid leaching gold are learned, DBC- isopropyl alcohol extraction system extracting gold and sodium sulfite restore golden five parts, specifically include Following steps:
(1) physics pretreatment: waste mobile phone 11 bought from market, through disassembling to obtain useless circuit board manually, using height Circuit board of mobile phone is broken into powder by fast multifunctional crusher.It is screened with 35 mesh unification of the motherland standard inspection sieves, after screening The powder sample 200g that partial size is less than 0.500mm is obtained, as containing golden object powder.
(2) chemical pretreatment: will contain golden object powder 1.0000g in small beaker, and excess HNO is added3Solution is placed in 30 DEG C It reacts in digital display thermostat water bath and filters afterwards for 24 hours, filter residue is washed, obtains gold-containing residue after drying.
(3) chloroazotic acid leaching gold: by the excessive chloroazotic acid of gold-containing residue addition, the liquid-solid ratio of gold-containing residue and chloroazotic acid is 80ml/g, often Temperature reaction 24 hours, is sealed during reaction with preservative film, and aperture exhaust is opened on film.Sample filtering after resolution obtains filter containing gold Liquid and filter residue will contain golden filtrate in deionized water constant volume 200mL volumetric flask.Wherein the chloroazotic acid is dense salt by percent by volume Sour (HCl): concentrated nitric acid (HNO3)=3:1.
(4) golden filtrate and extract liquor hybrid extraction, the extraction extraction of DBC- Isopropanol Solvent DBC- isopropyl alcohol extraction: will be contained Liquid is taken to carry out extracting gold, wherein DBC- isopropyl alcohol extraction system includes 60% DBC, 40% isopropanol by percent by volume, It is stirred under 300r/min blender under room temperature, liquid separation is stood after 5min.It is obtained after extraction liquid separation for the first time containing golden organic phase, separation Raffinate out, level-one extraction yield are 85%.It adds and is sufficiently mixed carry out reextraction with the extract liquor of raffinate same volume, Second level extraction yield is 92%.
(5) multiple saturated organic phase extracted sodium sulfite extraction reduction gold: is entered into the Asia that mass concentration is 10% In metabisulfite solution reduction reactor, 60S is stirred to react under room temperature, wherein the stream of organic phase and water phase compares for 6:2.
The extraction rate of the gold of the present embodiment is about 94%, extracts reduction rate 96%, overall recovery is about 92%.
Embodiment 3
A method of extracting gold from useless circuit board, process flow chart is as shown in Figure 1, including physics pretreatment, changing Pretreatment, chloroazotic acid leaching gold are learned, DBC- isopropyl alcohol extraction system extracting gold and sodium sulfite restore golden five parts, specifically include Following steps:
(1) physics pretreatment: waste mobile phone 11 bought from market, through disassembling to obtain useless circuit board manually, using height Circuit board of mobile phone is broken into powder by fast multifunctional crusher.It is screened with 35 mesh unification of the motherland standard inspection sieves, after screening The powder sample 200g that partial size is less than 0.500mm is obtained, as containing golden object powder.
(2) chemical pretreatment: golden object powder 1.0000g will be contained in small beaker, excessive HNO is added3Solution is placed in 30 It reacts in DEG C digital display thermostat water bath and filters afterwards for 24 hours, filter residue is washed, obtains gold-containing residue after drying.
(3) chloroazotic acid leaching gold: being added excessive chloroazotic acid for gold-containing residue, and the liquid-solid ratio of gold-containing residue and chloroazotic acid is 80ml/g, and 30 It DEG C heating in water bath for reaction 27 hours, is sealed during reaction with preservative film, aperture exhaust is opened on film.Sample filtering after resolution, obtains To containing golden filtrate and filter residue, golden filtrate will be contained in deionized water constant volume 200mL volumetric flask.Wherein the chloroazotic acid presses volume basis Than for concentrated hydrochloric acid (HCl): concentrated nitric acid (HNO3)=3:1.
(4) golden filtrate and extract liquor hybrid extraction, the extraction extraction of DBC- Isopropanol Solvent DBC- isopropyl alcohol extraction: will be contained Liquid is taken to carry out extracting gold, wherein DBC- isopropyl alcohol extraction system includes 80% DBC, 20% isopropanol by percent by volume, It is stirred under 300r/min blender under room temperature, liquid separation is stood after 5min.It is obtained after extraction liquid separation for the first time containing golden organic phase, separation Raffinate out, level-one extraction yield are 83%.It adds and is sufficiently mixed carry out reextraction with the extract liquor of raffinate same volume, Second level extraction yield is 91%.
(5) multiple saturated organic phase extracted sodium sulfite extraction reduction gold: is entered into the sulfurous that mass concentration is 5% In acid sodium solution reduction reactor, 120S is stirred to react under room temperature, wherein the stream of organic phase and water phase compares for 4:2.
The extraction rate of the gold of the present embodiment is about 95%, extracts reduction rate 91%, overall recovery is about 89%.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.

Claims (9)

1. a kind of method for extracting gold from useless circuit board, which comprises the following steps:
(1) useless circuit board is crushed, crosses sieve, obtained containing golden object powder;
(2) step (1) the object powder obtained containing gold is pre-processed with nitric acid, obtains gold-containing residue;
(3) gold-containing residue made from the step (2) is added in chloroazotic acid and is cleared up, obtained containing Jin Wangshui;
(4) step (3) is obtained containing golden chloroazotic acid and extract liquor hybrid extraction, at least extracted twice;Extraction is used The extract liquor of DBC- Isopropanol Solvent carries out extracting gold, obtains isolating raffinate containing golden organic phase after extracting liquid separation for the first time, It adds and is sufficiently mixed carry out reextraction with the extract liquor of raffinate same volume;Wherein, in the DBC- Isopropanol Solvent It include: DBC the and 20-40% isopropanol of 60-80%, room temperature extraction by percent by volume;
(5) containing sodium sulfite reduction is added in golden organic phase, cake of gold will be obtained in the step (6).
2. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that crush electricity in step (1) 35-100 mesh is crossed after the plate of road.
3. it is according to claim 1 extracted from useless circuit board gold method, which is characterized in that in step (3) chloroazotic acid with The liquid-solid ratio of gold-containing residue is 60-140ml/g.
4. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that filter containing gold in step (3) The reaction temperature of slag and chloroazotic acid is 25-45 DEG C.
5. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that step (3) gold-containing residue Reaction with chloroazotic acid is normal-temperature reaction 21-27 hours.
6. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that the processing of step (3) chloroazotic acid Afterwards, golden chloroazotic acid filtering will be contained, obtained containing golden filtrate and filter residue, then filter residue is subjected to extracting gold with extract liquor.
7. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that DBC- is different in step (4) It include: DBC the and 20-40% isopropanol of 60-80% by percent by volume in propyl alcohol system.
8. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that step (5) sulfite The mass concentration of sodium solution is 5-10%.
9. the method according to claim 1 for extracting gold from useless circuit board, which is characterized in that step has in (5) containing gold The time of machine phase and sodium sulfite reduction reaction is 60-120S, and the stream of organic phase and water phase compares for 4-6:2.
CN201910380498.1A 2019-05-08 2019-05-08 Method for extracting gold from waste circuit board Active CN110106354B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112662885A (en) * 2021-01-07 2021-04-16 广州云伊科技有限公司 Device for extracting gold from batched waste memory cards

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CN103757246A (en) * 2014-01-02 2014-04-30 紫金矿业集团股份有限公司 Method for producing high-purity gold
CN105441690A (en) * 2015-11-18 2016-03-30 金川集团股份有限公司 Method for extracting gold from material liquid with high gold content

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112662885A (en) * 2021-01-07 2021-04-16 广州云伊科技有限公司 Device for extracting gold from batched waste memory cards
CN112662885B (en) * 2021-01-07 2022-07-01 深圳还珠科技有限公司 Device for extracting gold from batched waste memory cards

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