CN107557585B - A kind of method of gold-tin alloy separation - Google Patents
A kind of method of gold-tin alloy separation Download PDFInfo
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- CN107557585B CN107557585B CN201710802841.8A CN201710802841A CN107557585B CN 107557585 B CN107557585 B CN 107557585B CN 201710802841 A CN201710802841 A CN 201710802841A CN 107557585 B CN107557585 B CN 107557585B
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- vulcanizing agent
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Abstract
The present invention relates to a kind of methods of gold-tin alloy separation, belong to non-ferrous metal field of thermometallurgical technology.Gold-tin alloy is put into closed container after mixing with vulcanizing agent and is sealed, vulcanization reaction is carried out under anaerobic, stirring condition, the tin in gold-tin alloy is vulcanized as stannous sulfide.Material is evaporated in vacuo under certain condition after vulcanization, and stannous sulfide is made to volatilize, to realize the separation of gold and tin.Present invention process process is short, and gold-tin alloy is i.e. separable by vulcanizing and two processing steps being evaporated in vacuo.
Description
Technical field
The present invention relates to a kind of methods of gold-tin alloy separation, belong to non-ferrous metal field of thermometallurgical technology.
Background technique
The gold-tin alloy of different composition ratio has high thermal conductivity, low vapour pressure, excellent corrosion resistance, good leaching
Lubricant nature and mobility are used for the soldering of gold-plated or plating billon lead frame and lead.Gold-tin alloy solder has pricker
It welds moderate temperature, high intensity, be not necessarily to the features such as scaling powder, good wellability, low viscosity, thermal fatigue resistance, be widely used
In great power LED, electricity strives forward the microelectronic fields such as automobile and laser and optic communication and field of photoelectric devices.In gold-tin alloy
Gold-tin alloy waste material can be generated in process of manufacture and use process, during copper, lead, tin anode mud synthetical recovery and
Also the gold-tin alloy containing impurity can be generated in electronic component removal process.Every gram of price of gold lattice are approximately 2000 times of tin, therefore
Fitting in recycling gold-tin alloy has great economic value.
Currently, the method for recycling gold from gold-tin alloy is mainly wet process, main method has: the (1) direct dissolution method of chloroazotic acid,
Gold-tin alloy material is directlyed adopt into aqua regia dissolution, so that gold is entered solution in the form of gold chloride, reusing reducing agent will be in solution
Gold chloride be reduced to metallic gold.This method tin during molten gold is easily oxidized to insoluble stannic oxide by chloroazotic acid, hinders
Gold dissolution, while filtration difficulty is caused, cause gold recovery low.(2) electrochemical solution, according to noble metal in material and low-priced gold
Belong to electrode potential difference, by electrolysis, makes expensive, base metal separation.This method can handle the material of any shape, but treating capacity
It is small, low efficiency.(3) metal fragmentation-dissolution method, roasting forms it at a certain temperature after gold-tin alloy is mixed with metallic aluminium
New alloy, then removes tin, aluminium using diluted acid dissolution, and insoluble matter uses aqua regia dissolution to recycle gold again.It is main existing for this method
It wants problem to be the introduction of new impurity aluminum, needs successive depths impurity and purification, process flow is longer, and tin is not returned effectively
It receives.
The above-mentioned Method for extracting gold from stanniferous material is finally to dissolve gold in the solution, then gold is extracted from solution.
There is golden recovery process long flow path in these methods, tin element is easy in golden course of dissolution and solution forms colloid, cause filtering tired
Difficulty can generate a large amount of waste water in wet-treating process, also contain a small amount of gold in waste water, need to be recycled to waste water
Disadvantage.
One kind, which is disclosed, application No. is 201410270455.5 Chinese patent recycles Jin Jixi from gold-tin alloy waste material
Method, this method mixes gold-tin alloy waste material with oxidisability sodium (potassium) salt in mass ratio, is packed into nickel or iron crucible, is placed in
In high temperature furnace, 500~700 DEG C roasting temperature 1~3 hour, after reaction, cooling, water logging after separation of solid and liquid, obtains
Sodium stannate (potassium) solution and insoluble slag；Sodium stannate (potassium) product is obtained after the purified removal of impurities of sodium stannate solution, condensing crystallizing；It is insoluble
Slag uses hydrochloric acid+oxidant dissolution again, obtains gold-containing solution, and after purification, addition reducing agent obtains high-purity cake of gold.This method mentions
Gold needs to add plurality of reagents, long flow path.
Summary of the invention
It is an object of the present invention to provide a kind of methods of gold-tin alloy separation, it is simple, easily operated.
The invention is realized by the following technical scheme:
Step 1: becoming 1.0~1.2 times of additions of vulcanizing agent molar fraction needed for sulphided state by tin element in gold-tin alloy
Vulcanizing agent；
Step 2: gold-tin alloy is put into closed container after mixing and is sealed with vulcanizing agent, in anaerobic, stirring bar
Under part, controlling heating temperature vulcanizes material at 200 DEG C~500 DEG C；
Step 3: sulfur product obtained by step 2 is put into vacuum drying oven, at 1100 DEG C~1400 DEG C of temperature, vacuum degree 1
It under~100Pa, is evaporated in vacuo, sulfide is made to volatilize, realize the purpose of golden tin separation.
Vulcanizing agent used in the present invention is sulphur.
Gold-tin alloy of the present invention can also contain a small amount of other metallic elements in addition to containing gold and tin element.
Working mechanism of the present invention: the boiling point of tin and gold is difficult to point at 2600 DEG C or more if directlying adopt vacuum distillation
From.Its volatility is greater than corresponding metal after tin metal is become sulfide, within the scope of 900 DEG C to 1200 DEG C, at identical temperature
The saturated vapour pressure of stannous sulfide is the 10 of metallic tin5~106Times.And other higher boiling metallic elements, as gold will not and vulcanizing agent
Directly reaction generates sulfide.Therefore, after gold-tin alloy and sulfurizing agent, tin element, which cures, becomes sulfide, and golden
Element will not cure, which can make tin sulfide volatilize by the way that control condition is evaporated in vacuo, and gold is non-volatile.Copper, iron are contour
Boiling contaminants are stored in slag phase with oxide morphology and gold is layered, and realize separation；The low boiling impurities such as lead, antimony are with sulphided state or simple substance
State is volatilized with stannous sulfide, to realize the separation of gold and tin.
The relationship of 1 metal of table and sulfide saturated vapour pressure and temperature
The invention has the advantages that
(1) process flow is short, and gold, tin point can be realized by vulcanizing and being evaporated in vacuo two processing steps in stanniferous material
From.
(2) present invention process is full thermal process, will not generate waste water, and cost for wastewater treatment is not present.
(3) for containing only the golden material with tin element, proof gold can be directly obtained using this technique；For containing other miscellaneous
Gold can be enriched in a product by the material of prime element using this technique, be conducive to subsequent gold purification.
(4) stannous sulfide of this technique output can be used as tin metallurgy raw material and return to tin process, or use as friction material.
Specific embodiment
Combined with specific embodiments below, the invention will be further described.
Embodiment 1
By the tin of unvulcanised state in gold-tin alloy (mass percentage: Sn98.22%, Au1.49%, other < 0.3%)
Become 1.2 times of addition sulphur of vulcanizing agent molar fraction needed for sulphided state.
Gold-tin alloy is put into closed container after mixing and is sealed with sulphur, under conditions of anaerobic, stirring, is risen
Temperature carries out vulcanizing treatment.Temperature is controlled at 200 DEG C~250 DEG C first, is reacted 60 minutes.Then anaerobic, stirring condition are kept,
380 DEG C~400 DEG C are warming up to, material and vulcanizing agent is made to carry out depth vulcanization reaction.After reaction, stop heating, to material
Sulfur product is taken out after cooling.
Material is evaporated in vacuo 90 minutes under the conditions of 1400 DEG C of temperature, 5~50Pa of vacuum degree after vulcanization, obtain volatile matter and
Residue.Through detection volatile constituent be Sn80.76%, S 19.18%, Au5g/t, residue ingredient be Sn1.81%,
Au97.33%.
Embodiment 2
Become sulphided state by the tin of unvulcanised state in gold-tin alloy (mass percentage: Sn89.66%, Au10.32%)
1.1 times of addition sulphur of required vulcanizing agent molar fraction.
Gold-tin alloy is put into closed container after mixing and is sealed with sulphur, under conditions of anaerobic, stirring, is risen
Temperature carries out vulcanizing treatment.Temperature is controlled at 230 DEG C~280 DEG C first, is reacted 30 minutes.Then anaerobic, stirring condition are kept,
350 DEG C~400 DEG C are warming up to, material and vulcanizing agent is made to carry out depth vulcanization reaction.After reaction, stop heating, to material
Sulfur product is taken out after cooling.
Material is evaporated in vacuo 60 minutes under the conditions of 1100 DEG C of temperature, 1~20Pa of vacuum degree after vulcanization, obtain volatile matter and
Residue.Through detection volatile constituent be Sn78.32%, S 21.46%, Au3g/t, residue ingredient be Sn1.05%,
Au98.86%.
Embodiment 3
Become sulphided state by the tin of unvulcanised state in gold-tin alloy (mass percentage: Sn57.66%, Au42.32%)
1.15 times of addition sulphur of required vulcanizing agent molar fraction.
Gold-tin alloy is put into closed container after mixing and is sealed with sulphur, under conditions of anaerobic, stirring, is risen
Temperature carries out vulcanizing treatment.Temperature is controlled at 250 DEG C~300 DEG C first, is reacted 30 minutes.Then anaerobic, stirring condition are kept,
450 DEG C~500 DEG C are warming up to, material and vulcanizing agent is made to carry out depth vulcanization reaction.After reaction, stop heating, to material
Sulfur product is taken out after cooling.
Material is evaporated in vacuo 60 minutes under the conditions of 1300 DEG C of temperature, 30~100Pa of vacuum degree after vulcanization, obtains volatile matter
And residue.Through detection volatile constituent be Sn78.67%, S21.25%, Au8g/t, residue ingredient be Sn0.19%,
Au99.80%.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Various change out.
Claims (1)
1. a kind of method of gold-tin alloy separation, it is characterised in that specific step is as follows:
Step 1: vulcanizing by 1.0~1.2 times of additions that tin element in gold-tin alloy becomes vulcanizing agent molar fraction needed for sulphided state
Agent；
Step 2: gold-tin alloy is put into closed container after mixing and is sealed with vulcanizing agent, in anaerobic, stirring condition
Under, controlling heating temperature vulcanizes material at 200 DEG C~500 DEG C；
Step 3: sulfur product obtained by step 2 is put into vacuum drying oven, at 1100 DEG C~1400 DEG C of temperature, vacuum degree 1~
It under 100Pa, is evaporated in vacuo, sulfide is made to volatilize, realize the purpose of golden tin separation；
The vulcanizing agent is sulphur.
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| CN109628746B (en) * | 2019-01-03 | 2021-02-26 | 江西铜业技术研究院有限公司 | Method for extracting tin from silver separating slag |
| CN109777966B (en) * | 2019-03-04 | 2020-11-17 | 昆明理工大学 | Method for separating indium-copper alloy by vacuum distillation |
| CN111020197B (en) * | 2019-12-09 | 2021-04-16 | 北京有色金属与稀土应用研究所 | Separation and recovery method of gold-tin alloy waste |
| CN114959277B (en) * | 2022-01-17 | 2024-03-26 | 昆明理工大学 | Method for separating and purifying tin and copper from tin refining sulfur slag |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792858A (en) * | 2009-11-16 | 2010-08-04 | 云南锡业集团（控股）有限责任公司 | Method for processing tin-iron-titanium material by using DC electric furnace |
| CN103589870A (en) * | 2013-11-08 | 2014-02-19 | 昆明理工大学 | Method for processing tin refining sulfur slag |
| CN103614555A (en) * | 2013-09-12 | 2014-03-05 | 昆明理工大学 | Method for efficiently separating and enriching tin from nickel-tin-iron alloy scrap |
| CN104232904A (en) * | 2014-09-18 | 2014-12-24 | 龙济时代(北京)新能源科技有限公司 | Method for Ni-Fe alloy production and Sn recovery from Ni-Sn ferroalloy scrap by high-sulfur coal sulfuration volatilization and oxidation slagging |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792858A (en) * | 2009-11-16 | 2010-08-04 | 云南锡业集团（控股）有限责任公司 | Method for processing tin-iron-titanium material by using DC electric furnace |
| CN103614555A (en) * | 2013-09-12 | 2014-03-05 | 昆明理工大学 | Method for efficiently separating and enriching tin from nickel-tin-iron alloy scrap |
| CN103589870A (en) * | 2013-11-08 | 2014-02-19 | 昆明理工大学 | Method for processing tin refining sulfur slag |
| CN104232904A (en) * | 2014-09-18 | 2014-12-24 | 龙济时代(北京)新能源科技有限公司 | Method for Ni-Fe alloy production and Sn recovery from Ni-Sn ferroalloy scrap by high-sulfur coal sulfuration volatilization and oxidation slagging |
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