CN112725633A - Negative pressure type gold chlorination and separation process - Google Patents

Negative pressure type gold chlorination and separation process Download PDF

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Publication number
CN112725633A
CN112725633A CN202110169192.9A CN202110169192A CN112725633A CN 112725633 A CN112725633 A CN 112725633A CN 202110169192 A CN202110169192 A CN 202110169192A CN 112725633 A CN112725633 A CN 112725633A
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gold
reaction kettle
negative pressure
reaction
chlorination
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CN112725633B (en
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黄苍林
马千里
蓝振坤
谢炳生
陈亮华
龙彬
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Xiamen Strait Gold Jewelry Industrial Park Co ltd
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Xiamen Strait Gold Jewelry Industrial Park Co ltd
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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
    • C22B11/06Chloridising
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a negative pressure type chlorination gold separation process, which comprises the following steps: s110, preparing a liquid reaction material, adding pure water and concentrated hydrochloric acid into a reaction kettle, and uniformly mixing to obtain the liquid reaction material; s120, pretreating a gold-containing material, namely mixing the gold-containing material with sodium chlorate according to the weight ratio of 1: 0.5-1 to obtain a gold-containing pretreatment material; s130, preheating a reaction kettle, and introducing hot water into a jacket of the reaction kettle; s140, feeding and reacting; s150, chlorine is removed under negative pressure; and S160, cooling and filtering. Has the advantages that: compared with the traditional gold chlorination and separation method, the phenomenon of tube explosion or kettle explosion caused by the increase of the pressure in the closed reaction container due to the generation of chlorine gas when sodium chlorate is put in is reduced, and the safety of the gold chlorination and separation process is improved; the material can be fed simultaneously, so that the feeding time is saved, the reaction efficiency of the chlorination and the gold separation is improved, and the operation time is shortened; after single feeding, the reaction operation can be carried out by one person, so that the number of operators is reduced compared with the traditional process, and the labor cost can be reduced.

Description

Negative pressure type gold chlorination and separation process
Technical Field
The invention relates to the technical field of metallurgy, in particular to a negative pressure type gold chlorination and separation process.
Background
The gold hydrometallurgical process mainly adopts a cyanidation method, replacement gold mud obtained in the gold extraction process of the cyanidation method is an intermediate raw material for gold extraction, gold and silver are generally recovered by adopting a wet refining process, and finished gold powder is generally obtained by carrying out a plurality of procedures of replacing gold mud pre-immersion dezincification, pre-immersion slag primary chlorination leaching, crude gold reduction, secondary chlorination leaching, primary gold reduction refining and the like on the wet refined gold. Excessive zinc powder and partial impurities in the gold mud are removed through a pre-soaking process, the obtained pre-leaching residue is subjected to chlorination leaching again, Au and other impurity metals in the residue are dissolved into a chlorination leaching solution, and silver enters the chlorination leaching residue in an AgCl form. And replacing AgCl in the chloridized leaching residues with iron powder to obtain crude silver powder, and casting the crude silver powder on an anode plate for electrolysis to obtain finished silver powder. And Au is put into the chlorination leaching solution to obtain crude gold with gold grade of 60-98% through a reduction process, and the crude gold is subjected to secondary chlorine leaching to obtain a solution to be reduced to obtain a primary gold finished product. However, the following problems exist in the gold separation process by using the above process: 1. the sodium chlorate has strong oxidizing property under the acidic condition, is easy to dissolve in water, and cannot complete the whole process of the gold separation operation by one-time investment in the gold separation operation; 2. after sodium chlorate is put into the reactor, the reaction is severe, a large amount of chlorine is generated, the pressure is continuously increased in a closed space, the sectional dosing is inconvenient, and the danger coefficient is increased. Therefore, the applicant provides a gold chlorination and separation process which is good in safety and convenient to operate.
Disclosure of Invention
The invention aims to solve the problems and provide a negative pressure type gold chlorination and separation process, and the preferable technical scheme in the technical schemes provided by the invention comprises the following steps: the safety is good, and the technical effects of one-time feeding for reaction, production efficiency improvement and the like can be achieved, and the details are described in the following.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a negative pressure type chlorination gold separation process, which comprises the following steps:
s110, preparing a liquid reaction material, adding pure water and concentrated hydrochloric acid into a reaction kettle, and uniformly mixing to obtain the liquid reaction material;
s120, pretreating a gold-containing material, namely mixing the gold-containing material with sodium chlorate according to the weight ratio of 1: 0.5-1 to obtain a gold-containing pretreatment material;
s130, preheating the reaction kettle, introducing hot water into a jacket of the reaction kettle until the temperature in the reaction kettle is increased to 75-85 ℃, and closing a hot water pipeline;
s140, feeding reaction, namely adding the gold-containing pretreatment material into the preheated reaction kettle, carrying out chlorination leaching reaction, observing the melting state of the gold-containing pretreatment material after the feeding is finished until the gold-containing pretreatment material is completely dissolved, opening an emptying valve of the reaction kettle in the reaction process, and extracting chlorine generated by the reaction;
s150, chlorine is removed under negative pressure, hot water is introduced into the jacket of the reaction kettle again, the temperature of the reaction kettle is raised to 85-95 ℃, materials in the reaction kettle are stirred until the materials are uniformly mixed, and negative pressure equipment is used for communicating the reaction kettle to remove chlorine under negative pressure;
s160, cooling and filtering, discharging hot water in a jacket of the reaction kettle, adjusting the pH value of liquid materials in the reaction kettle to 3-4, introducing cold water into the jacket of the reaction kettle to cool to normal temperature, and finally sending the gold-separating pregnant solution cooled to normal temperature into a filtering device by using extraction equipment to filter.
Preferably, in step S110, the weight ratio of the gold-containing material to the liquid reaction material is 1: 3-6.
Preferably, in step S110, the weight ratio of the gold-containing material to the liquid reaction material is 1: 4.5.
preferably, the reaction kettle is a double-layer reaction kettle, wherein a jacket connected with a water supply and drainage pipeline is arranged between the inner layer and the outer layer.
Preferably, the reaction kettle is provided with an emptying valve connected with negative pressure equipment.
Preferably, the reaction kettle is provided with a thermometer, and the temperature measuring end of the thermometer is inserted into the inner layer of the reaction kettle.
Preferably, in step S140, the feeding time of the gold-containing pretreatment material is completed within 1 hour.
Preferably, in the step S150, after the reaction kettle is heated, the stirring time is not less than 10 minutes.
Preferably, in step S120, the weight ratio of the gold-containing material to the sodium chlorate is 1: 0.75.
preferably, in step S160, the pumping device is a pneumatic pump.
In conclusion, the beneficial effects of the invention are as follows: 1. compared with the traditional gold chlorination and separation method, the phenomenon of tube explosion or kettle explosion caused by the increase of the pressure in the closed reaction container due to the generation of chlorine gas when sodium chlorate is put in is reduced, and the safety of the gold chlorination and separation process is improved;
2. the material can be fed simultaneously, so that the feeding time is saved, the reaction efficiency of the chlorination and the gold separation is improved, and the operation time is shortened;
3. after single feeding, the reaction operation can be carried out by one person, so that the number of operators is reduced compared with the traditional process, and the labor cost can be reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Referring to fig. 1, the invention provides a negative pressure type gold chlorination and separation process, which comprises the following steps:
s110, preparing a liquid reaction material, adding pure water and concentrated hydrochloric acid into a reaction kettle, and uniformly mixing to obtain the liquid reaction material, wherein the weight ratio of the gold-containing material to the liquid reaction material is 1: 4.5;
s120, pretreating a gold-containing material, wherein the weight ratio of the gold-containing material to sodium chlorate is 1: 0.75 to obtain a gold-containing pretreatment material;
s130, preheating the reaction kettle, introducing hot water into a jacket of the reaction kettle until the temperature in the reaction kettle is increased to 75-85 ℃, and closing a hot water pipeline;
s140, adding a gold-containing pretreatment material into the preheated reaction kettle, wherein the adding time of the gold-containing pretreatment material is finished within 1 hour, carrying out chlorination leaching reaction, observing the melting state of the gold-containing pretreatment material after the adding is finished until the gold-containing pretreatment material is completely melted, opening an emptying valve of the reaction kettle in the reaction process, extracting chlorine generated by the reaction, and opening the emptying valve to be not too large so as to avoid too fast pumping due to too large negative pressure;
s150, removing chlorine under negative pressure, introducing hot water into a jacket of the reaction kettle again, heating the reaction kettle to 85-95 ℃, stirring the materials in the reaction kettle until the materials are uniformly mixed, stirring for not less than 10 minutes after heating, and communicating the reaction kettle with negative pressure equipment to remove chlorine under negative pressure;
s160, cooling and filtering, discharging hot water in a jacket of the reaction kettle, adjusting the pH value of liquid materials in the reaction kettle to 3-4, introducing cold water into the jacket of the reaction kettle to cool to normal temperature, and finally sending the gold-separating pregnant solution cooled to normal temperature into a filtering device by using a pneumatic pump for filtering.
As an optional implementation mode, the reaction kettle is a double-layer reaction kettle made of titanium materials to meet the acid resistance requirement in the reaction process, wherein a jacket connected with a water supply and drainage pipeline is arranged between the inner layer and the outer layer; an emptying valve connected with negative pressure equipment is arranged on the reaction kettle; the reaction kettle is provided with a thermometer, and the temperature measuring end of the thermometer is inserted into the inner layer of the reaction kettle.
By adopting the structure, compared with the traditional chlorination and gold separation method, the phenomenon of tube explosion or kettle explosion caused by the increase of the pressure in the closed reaction container due to the generation of chlorine gas when sodium chlorate is put in is reduced, and the safety of the chlorination and gold separation process is improved; the material can be fed simultaneously, so that the feeding time is saved, the reaction efficiency of the chlorination and the gold separation is improved, and the operation time is shortened; after single feeding, the reaction operation can be carried out by one person, so that the number of operators is reduced compared with the traditional process, and the labor cost can be reduced.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (10)

1. A negative pressure type gold chlorination and separation process is characterized by comprising the following steps:
s110, preparing a liquid reaction material, adding pure water and concentrated hydrochloric acid into a reaction kettle, and uniformly mixing to obtain the liquid reaction material;
s120, pretreating a gold-containing material, namely mixing the gold-containing material with sodium chlorate according to the weight ratio of 1: 0.5-1 to obtain a gold-containing pretreatment material;
s130, preheating the reaction kettle, introducing hot water into a jacket of the reaction kettle until the temperature in the reaction kettle is increased to 75-85 ℃, and closing a hot water pipeline;
s140, feeding reaction, namely adding the gold-containing pretreatment material into the preheated reaction kettle, carrying out chlorination leaching reaction, and observing the melting state of the gold-containing pretreatment material after the feeding is finished until the gold-containing pretreatment material is completely dissolved;
s150, chlorine is removed under negative pressure, hot water is introduced into the jacket of the reaction kettle again, the temperature of the reaction kettle is raised to 85-95 ℃, materials in the reaction kettle are stirred until the materials are uniformly mixed, and negative pressure equipment is used for communicating the reaction kettle to remove chlorine under negative pressure;
s160, cooling and filtering, discharging hot water in a jacket of the reaction kettle, adjusting the pH value of liquid materials in the reaction kettle to 3-4, introducing cold water into the jacket of the reaction kettle to cool to normal temperature, and finally sending the gold-separating pregnant solution cooled to normal temperature into a filtering device by using extraction equipment to filter.
2. The negative pressure type chlorination gold separation process according to claim 1, characterized in that: in the step S110, the weight ratio of the gold-containing material to the liquid reaction material is 1: 3-6.
3. The negative pressure type chlorination gold separation process according to claim 2, characterized in that: in the step S110, the weight ratio of the gold-containing material to the liquid reaction material is 1: 4.5.
4. the negative pressure type chlorination gold separation process according to claim 1, characterized in that: the reaction kettle is a double-layer reaction kettle, wherein a jacket connected with a water supply pipeline and a water discharge pipeline is arranged between the inner layer and the outer layer.
5. The negative pressure type chlorination gold separation process according to claim 4, wherein: and an exhaust valve connected with negative pressure equipment is arranged on the reaction kettle.
6. The negative pressure type chlorination gold separation process according to claim 4, wherein: the reaction kettle is provided with a thermometer, and the temperature measuring end of the thermometer is inserted into the inner layer of the reaction kettle.
7. The negative pressure type chlorination gold separation process according to claim 1, characterized in that: in step S140, the charging time of the gold-containing pretreatment material is completed within 1 hour.
8. The negative pressure type chlorination gold separation process according to claim 1, characterized in that: in the step S150, the stirring time is not less than 10 minutes after the reaction kettle is heated.
9. The negative pressure type chlorination gold separation process according to claim 1, characterized in that: in the step S120, the weight ratio of the gold-containing material to the sodium chlorate is 1: 0.75.
10. the negative pressure type chlorination gold separation process according to claim 1, characterized in that: in step S160, the pumping device is a pneumatic pump.
CN202110169192.9A 2021-02-07 2021-02-07 Negative pressure type gold chlorination and separation process Active CN112725633B (en)

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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB795790A (en) * 1955-04-20 1958-05-28 Electro Chimie Metal Improvements in or relating to the recovery of gold
US20050118081A1 (en) * 2003-09-30 2005-06-02 Jaguar Nickel Inc. Process for the recovery of value metals from base metal sulfide ores
CN101451190A (en) * 2007-11-30 2009-06-10 灵宝市金源矿业有限责任公司 Novel method for separating gold and silver from gold mud
CN102274978A (en) * 2011-08-26 2011-12-14 山东黄金矿业(莱州)有限公司三山岛金矿 Method for quickly wet-process refining non-standard coarse gold powder
CN103305699A (en) * 2013-06-20 2013-09-18 山东恒邦冶炼股份有限公司 Method for extracting platinum-palladium out of copper anode mud
CN104084026A (en) * 2014-07-18 2014-10-08 贵州大龙银星汞业有限责任公司 Processing method of chlorine-containing tail gas produced by mercuric chloride production
CN105567992A (en) * 2015-12-19 2016-05-11 中国地质科学院矿产综合利用研究所 Method for reducing neutralization cost of refractory gold ore hot-pressing oxidation acid
CN105648231A (en) * 2016-01-19 2016-06-08 中国有色桂林矿产地质研究院有限公司 Quick hot pressing oxidation pretreatment technology for microgranular sulfide type gold ore
CN106244820A (en) * 2016-08-29 2016-12-21 金川集团股份有限公司 A kind of method of chlorine pressure rapid solution complexity rare precious metal concentrate
CN106282555A (en) * 2016-08-31 2017-01-04 胡中 Recycling tail gas equipment and technique during a kind of dissolving gold, platinum, palladium
CN109848179A (en) * 2019-01-15 2019-06-07 长春黄金研究院有限公司 A kind of gold industry hot-pressure oxidation cyaniding tailing processing method
CN211848093U (en) * 2020-01-06 2020-11-03 烟台市金奥环保科技有限公司 Industrial test device for chlorination gold extraction of arsenic-containing gold concentrate

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB795790A (en) * 1955-04-20 1958-05-28 Electro Chimie Metal Improvements in or relating to the recovery of gold
US20050118081A1 (en) * 2003-09-30 2005-06-02 Jaguar Nickel Inc. Process for the recovery of value metals from base metal sulfide ores
US20090013829A1 (en) * 2003-09-30 2009-01-15 Harris G Bryn Process for the recovery of value metals from base metal sulfide ores
CN101451190A (en) * 2007-11-30 2009-06-10 灵宝市金源矿业有限责任公司 Novel method for separating gold and silver from gold mud
CN102274978A (en) * 2011-08-26 2011-12-14 山东黄金矿业(莱州)有限公司三山岛金矿 Method for quickly wet-process refining non-standard coarse gold powder
CN103305699A (en) * 2013-06-20 2013-09-18 山东恒邦冶炼股份有限公司 Method for extracting platinum-palladium out of copper anode mud
CN104084026A (en) * 2014-07-18 2014-10-08 贵州大龙银星汞业有限责任公司 Processing method of chlorine-containing tail gas produced by mercuric chloride production
CN105567992A (en) * 2015-12-19 2016-05-11 中国地质科学院矿产综合利用研究所 Method for reducing neutralization cost of refractory gold ore hot-pressing oxidation acid
CN105648231A (en) * 2016-01-19 2016-06-08 中国有色桂林矿产地质研究院有限公司 Quick hot pressing oxidation pretreatment technology for microgranular sulfide type gold ore
CN106244820A (en) * 2016-08-29 2016-12-21 金川集团股份有限公司 A kind of method of chlorine pressure rapid solution complexity rare precious metal concentrate
CN106282555A (en) * 2016-08-31 2017-01-04 胡中 Recycling tail gas equipment and technique during a kind of dissolving gold, platinum, palladium
CN109848179A (en) * 2019-01-15 2019-06-07 长春黄金研究院有限公司 A kind of gold industry hot-pressure oxidation cyaniding tailing processing method
CN211848093U (en) * 2020-01-06 2020-11-03 烟台市金奥环保科技有限公司 Industrial test device for chlorination gold extraction of arsenic-containing gold concentrate

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