CN106916961A - Vacuum drying oven produces thick silver process - Google Patents
Vacuum drying oven produces thick silver process Download PDFInfo
- Publication number
- CN106916961A CN106916961A CN201710268435.8A CN201710268435A CN106916961A CN 106916961 A CN106916961 A CN 106916961A CN 201710268435 A CN201710268435 A CN 201710268435A CN 106916961 A CN106916961 A CN 106916961A
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- CN
- China
- Prior art keywords
- vacuum drying
- drying oven
- silver
- tin
- metal
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to one kind thick silver process is produced using vacuum drying oven.The present invention it comprise the following steps：(1) metal requirement：Vacuum drying oven there are certain requirements to charging metal, tin<0.1%th, antimony<5%th, copper<0.1%, other metals in alloy are first blown into the pretreatment of the early stages such as antimony, decopper(ing), detin；(2) metal handled well only remains lead, silver-colored and micro other metals, first time enrichment is carried out during metal is added into vacuum drying oven, lead pipe metal out is substantially that lead can directly arrive lead electrowinning process, and tin-tube metal out is exactly the silver alloy of silver content 30% 40%；(3) silver alloy of silver content 30% 40% carries out secondary vacuum distillation, it is possible to obtain the silver alloy of content more than 90.Thick silver process is produced the invention provides a kind of process is simple, production efficiency utilization vacuum drying oven high.
Description
Technical field
It is more particularly to a kind of to produce thick silver process using vacuum drying oven the present invention relates to one kind thick silver process of production.
Background technology
Noble metal production both at home and abroad at present is all wet underwater welding, and wet processing is a large amount of useless due to that can be produced in production process
Water, it is difficult to process and seriously polluted.This inventive method is that using vacuum drying oven under high temperature, reduced pressure, different metal saturation is steamed
The different principle of vapour pressure comes separation of Silver and other metals.Whole process is carried out in the stove of sealing, using Electric heating, so
The technique has technological process short, and environmentally friendly good energy consumption is low substantially pollution-free, the advantages of metal recovery rate is high.
The content of the invention
Thick silver process is produced it is an object of the invention to provide a kind of process is simple, production efficiency utilization vacuum drying oven high.
The present invention is to solve by the following technical programs：The technique is comprised the following steps:
（1）Decopper(ing) treatment
Alloy lead is put into pot and is melted, temperature control is slowly added to sulphur at 320~280 DEG C, opened mixer and stir strongly
Mix, wherein 1Kg copper adds 1Kg sulphur, to add continue after sulphur and stir, wait liquid level surface yellow-gray dope gradually become it is black
Color powder, as reaction terminate, and pull scum silica frost out, stop stirring, and decopper(ing) terminates, and copper content is about less than 0.1%；
（2）Except tin treatment
Metal in step 1 is heated up to 400-450 DEG C, mixer is opened, constantly to adding solid NuaO, hydroxide in pot
Sodium consumption is 2-3 times of tin metal amount, and at this temperature, alloy is in molten condition, is passed through compressed air, more active using tin
The characteristics of, make itself and air oxidation into tin ash, then sodium stannate slag is obtained with alkali reaction, no longer produced when NaOH is added
During scum silica frost, show that tin has been totally separated, pull scum silica frost out, be extracted into cooling in mould；
（3）Vacuum drying oven distills for the first time
After adding vacuum drying oven material pot to dissolve alloy after detin, open vavuum pump and start for pressure in stove to be extracted into below 5MPa,
Control vacuum drying oven three electric currents of heater are 3600A, voltage 32V, treat that body of heater is warmed up to 1200~1300 DEG C, start charging,
Feed rate is controlled in 1100g/10s, and material volatilizees in drip pan in stove, the different original of the saturated vapor pressure according to each metal
Reason, liquid metal silver alloy by go out tin-tube flow out, and metallic lead, antimony, etc. then volatilize to the cold condenser condensation after by lead pipe flow out, warp
After vacuum drying oven distillation, the silver content in silver alloy is about in 20%-40% or so；
（4）Vacuum drying oven distills for second
Step（3）In first time distillation silver alloy, second distillation is carried out again, control condition is electric current：3600A, voltage
32V, flow control between 500-600g/10s, silver alloy content out between 90%-95%, argentiferous 10%- in metal
Between 30%, return to time distillation and do raw material, go out tin-tube and be out thick silver content>90%, can be with Direct Electrolysis or wet purification.
The technique of the thick silver of utilization vacuum drying oven production that the present invention is provided has advantages below relative to existing technology：（1）
Reduce pollution：Reduce wet method and put forward the intractable problem of waste water in silver, while also reducing pollution；（2）Improve metal recovery rate：Silver is wet
Many metals can be molten in the middle of waste water in method production, causes to reclaim difficult.Using waste of the vacuum drying oven without these materials, improve
Metal recovery rate.
Brief description of the drawings Fig. 1 is that the embodiment of the present invention produces thick silver process schematic flow sheet using vacuum drying oven.
Specific embodiment as shown in figure 1, vacuum drying oven to charging metal there are certain requirements, tin<0.1%th, antimony<5%th, copper<
0.1%, therefore other metals in alloy are first blown into the pretreatment of the early stages such as antimony, decopper(ing), detin.
Embodiment 1
The embodiment is comprised the following steps：
（1）Decopper(ing) treatment
Alloy lead is put into pot and is melted, temperature control is slowly added to sulphur at 320 DEG C, opens mixer strong agitation, its
Middle 1Kg copper adds 1Kg sulphur, continues to stir after adding sulphur, waits the yellow-gray dope on liquid level surface to gradually become black powder
End, as reaction are terminated, and pull scum silica frost out, stop stirring, and decopper(ing) terminates, and copper content is about less than 0.1%；
（2）Except tin treatment
Metal in step 1 is heated up to 400 DEG C.Mixer is opened, constantly to solid NuaO is added in pot, NaOH is used
It is 2.5 times of tin metal amount to measure, and at this temperature, alloy is in molten condition, compressed air is passed through, using the spy that tin is more active
Point, makes itself and air oxidation into tin ash, then obtains sodium stannate slag with alkali reaction, and scum silica frost is no longer produced when NaOH is added
When, show that tin has been totally separated, pull scum silica frost out, it is extracted into cooling in mould；
（3）Vacuum drying oven distills for the first time
After adding vacuum drying oven material pot to dissolve alloy after detin, open vavuum pump and start for pressure in stove to be extracted into below 5MPa,
Control vacuum drying oven three electric currents of heater are 3600A, voltage 32V, treat that body of heater is warmed up to 1200 DEG C, start charging, enter stream
In 1100g/10s, material volatilizees in drip pan in stove, the different principle of the saturated vapor pressure according to each metal, liquid for amount control
State metal silver alloy by go out tin-tube flow out, and metallic lead, antimony, etc. then volatilize to the cold condenser condensation after by lead pipe flow out, through vacuum
After stove distillation, the silver content in silver alloy is about in 20%-40%；
（4）Vacuum drying oven distills for second
Step（3）In first time distillation silver alloy, second distillation is carried out again, control condition is electric current：3600A, voltage
32V, flow control between 500-600g/10s, silver alloy content out between 90%-95%, argentiferous 10%- in metal
Between 30%, return to time distillation and do raw material, go out tin-tube and be out thick silver content>90%, can be with Direct Electrolysis or wet purification.
Embodiment 2
The embodiment is comprised the following steps：
（1）Decopper(ing) treatment
Alloy lead is put into pot and is melted, temperature control is slowly added to sulphur at 300 DEG C, opens mixer strong agitation, its
Middle 1Kg copper adds 1Kg sulphur, continues to stir after adding sulphur, waits the yellow-gray dope on liquid level surface to gradually become black powder
End, as reaction are terminated, and pull scum silica frost out, stop stirring, and decopper(ing) terminates, and copper content is about less than 0.1%；
（2）Except tin treatment
Metal in step 1 is heated up to 450 DEG C, mixer is opened, constantly to adding solid NuaO, NaOH to use in pot
It is 3 times of tin metal amount to measure, and at this temperature, alloy is in molten condition, compressed air is passed through, using the spy that tin is more active
Point, makes itself and air oxidation into tin ash, then obtains sodium stannate slag with alkali reaction, and scum silica frost is no longer produced when NaOH is added
When, show that tin has been totally separated, pull scum silica frost out, it is extracted into cooling in mould；
（3）Vacuum drying oven distills for the first time
After adding vacuum drying oven material pot to dissolve alloy after detin, open vavuum pump and start for pressure in stove to be extracted into below 5MPa,
Control vacuum drying oven three electric currents of heater are 3600A, voltage 32V, treat that body of heater is warmed up to 1300 DEG C, start charging, enter stream
In 1100g/10s, material volatilizees in drip pan in stove, the different principle of the saturated vapor pressure according to each metal, liquid for amount control
State metal silver alloy by go out tin-tube flow out, and metallic lead, antimony, etc. then volatilize to the cold condenser condensation after by lead pipe flow out, through vacuum
After stove distillation, the silver content in silver alloy is about in 20%-40%；
（4）Vacuum drying oven distills for second
Step（3）In first time distillation silver alloy, second distillation is carried out again, control condition is electric current：3600A, voltage
32V, flow control between 500-600g/10s, silver alloy content out between 90%-95%, argentiferous 10%- in metal
Between 30%, return to time distillation and do raw material, go out tin-tube and be out thick silver content>90%.Can be with Direct Electrolysis or wet purification.
Claims (1)
1. a kind of vacuum drying oven produces thick silver process, it is characterised in that：It is comprised the following steps：
（1）Decopper(ing) treatment
Alloy lead is put into pot and is melted, temperature control is slowly added to sulphur at 320~280 DEG C, opened mixer and stir strongly
Mix, wherein 1Kg copper adds 1Kg sulphur, to add continue after sulphur and stir, wait liquid level surface yellow-gray dope gradually become it is black
Color powder, as reaction terminate, and pull scum silica frost out, stop stirring, and decopper(ing) terminates, and copper content is about less than 0.1%；
（2）Except tin treatment
Metal in step 1 is heated up to 400-450 DEG C, mixer is opened, constantly to adding solid NuaO, hydroxide in pot
Sodium consumption is 2-3 times of tin metal amount, and at this temperature, alloy is in molten condition, is passed through compressed air, more active using tin
The characteristics of, make itself and air oxidation into tin ash, then sodium stannate slag is obtained with alkali reaction, no longer produced when NaOH is added
During scum silica frost, show that tin has been totally separated, pull scum silica frost out, be extracted into cooling in mould；
（3）Vacuum drying oven distills for the first time
After adding vacuum drying oven material pot to dissolve alloy after detin, open vavuum pump and start for pressure in stove to be extracted into below 5MPa,
Control vacuum drying oven three electric currents of heater are 3600A, voltage 32V, treat that body of heater is warmed up to 1200~1300 DEG C, start charging,
Feed rate is controlled in 1100g/10s, and material volatilizees in drip pan in stove, the different original of the saturated vapor pressure according to each metal
Reason, liquid metal silver alloy by go out tin-tube flow out, and metallic lead, antimony, etc. then volatilize to the cold condenser condensation after by lead pipe flow out, warp
After vacuum drying oven distillation, the silver content in silver alloy is about in 20%-40%；
（4）Vacuum drying oven distills for second
Step（3）In first time distillation silver alloy, second distillation is carried out again, control condition is electric current：3600A, voltage
32V, flow control between 500-600g/10s, silver alloy content out between 90%-95%, argentiferous 10%- in metal
Between 30%, return to time distillation and do raw material, go out tin-tube and be out thick silver content>90%, can be with Direct Electrolysis or wet purification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710268435.8A CN106916961A (en) | 2017-04-23 | 2017-04-23 | Vacuum drying oven produces thick silver process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710268435.8A CN106916961A (en) | 2017-04-23 | 2017-04-23 | Vacuum drying oven produces thick silver process |
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| CN106916961A true CN106916961A (en) | 2017-07-04 |
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Family Applications (1)
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| CN201710268435.8A Pending CN106916961A (en) | 2017-04-23 | 2017-04-23 | Vacuum drying oven produces thick silver process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2693670C1 (en) * | 2018-05-07 | 2019-07-03 | Акционерное общество "Уралэлектромедь" | Method of processing silicate reduced slag by vacuum distillation, containing antimony, lead and silver |
| CN112210672A (en) * | 2020-10-20 | 2021-01-12 | 昆明理工大学 | Method for purifying crude silver |
| CN114657389A (en) * | 2022-03-11 | 2022-06-24 | 紫金矿业集团黄金冶炼有限公司 | Method for processing high-silver-content low-grade alloy gold |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4350524A (en) * | 1981-05-15 | 1982-09-21 | Kennecott Corporation | Process for removal of base metal impurities from molten silver with sulfur hexafluoride |
| CN87104574A (en) * | 1987-06-27 | 1988-03-30 | 昆明工学院 | New technique of fire refining method for bullion lead |
| CN101560606A (en) * | 2009-05-19 | 2009-10-21 | 昆明鼎邦科技有限公司 | Deleading method through vacuum distillation of noble lead materials |
| CN102168179A (en) * | 2011-04-07 | 2011-08-31 | 赵志强 | Technology for producing Au and Ag from precious Pb by vacuum distillation |
-
2017
- 2017-04-23 CN CN201710268435.8A patent/CN106916961A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4350524A (en) * | 1981-05-15 | 1982-09-21 | Kennecott Corporation | Process for removal of base metal impurities from molten silver with sulfur hexafluoride |
| CN87104574A (en) * | 1987-06-27 | 1988-03-30 | 昆明工学院 | New technique of fire refining method for bullion lead |
| CN101560606A (en) * | 2009-05-19 | 2009-10-21 | 昆明鼎邦科技有限公司 | Deleading method through vacuum distillation of noble lead materials |
| CN102168179A (en) * | 2011-04-07 | 2011-08-31 | 赵志强 | Technology for producing Au and Ag from precious Pb by vacuum distillation |
Non-Patent Citations (1)
| Title |
|---|
| 技术市场专栏编者: "粗铅火法精炼新技术", 《有色冶炼》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2693670C1 (en) * | 2018-05-07 | 2019-07-03 | Акционерное общество "Уралэлектромедь" | Method of processing silicate reduced slag by vacuum distillation, containing antimony, lead and silver |
| CN112210672A (en) * | 2020-10-20 | 2021-01-12 | 昆明理工大学 | Method for purifying crude silver |
| CN112210672B (en) * | 2020-10-20 | 2021-12-07 | 昆明理工大学 | Method for purifying crude silver |
| CN114657389A (en) * | 2022-03-11 | 2022-06-24 | 紫金矿业集团黄金冶炼有限公司 | Method for processing high-silver-content low-grade alloy gold |
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Application publication date: 20170704 |
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