CN107557585A - 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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- CN107557585A CN107557585A CN201710802841.8A CN201710802841A CN107557585A CN 107557585 A CN107557585 A CN 107557585A CN 201710802841 A CN201710802841 A CN 201710802841A CN 107557585 A CN107557585 A CN 107557585A
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- gold
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- vulcanizing agent
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Abstract
The present invention relates to a kind of method of gold-tin alloy separation, belong to non-ferrous metal field of thermometallurgical technology.It is put into closed container and seals after gold-tin alloy is well mixed with vulcanizing agent, vulcanization reaction is carried out under anaerobic, stirring condition, is stannous sulfide by the tin vulcanization in gold-tin alloy.Material is evaporated in vacuo under certain condition after vulcanization, stannous sulfide is volatilized, so as to realize the separation of gold and tin.Present invention process flow is short, and gold-tin alloy is i.e. separable by vulcanizing and being evaporated in vacuo two processing steps.
Description
Technical field
The present invention relates to a kind of method of gold-tin alloy separation, belong to non-ferrous metal field of thermometallurgical technology.
Background technology
The gold-tin alloy of different proportion of composing has high thermal conductivity, low vapour pressure, excellent corrosion resistance, good leaching
Lubricant nature and mobility, it is used for the soldering of gold-plated or plating billon lead frame and lead.Gold-tin alloy solder has pricker
Weld moderate temperature, high intensity, without scaling powder, good wellability, low viscosity, thermal fatigue resistance the features such as, be widely used
In great power LED, electricity strives forward the microelectronics such as automobile and laser, and optic communication and field of photoelectric devices.In gold-tin alloy
Gold-tin alloy waste material can be produced during process of manufacture and use, during copper, lead, tin anode mud synthetical recovery and
Also the gold-tin alloy containing impurity can be produced in electronic component removal process.Every gram of price of gold lattice are approximately 2000 times of tin, therefore
Gold utensil in recovery gold-tin alloy has great economic value.
At present, the method that gold is reclaimed from gold-tin alloy is mainly wet method, and main method has：(1) the direct dissolution method of chloroazotic acid,
Gold-tin alloy material is directly used into aqua regia dissolution, gold is entered solution in the form of gold chloride, reuses reducing agent by solution
Gold chloride be reduced to metallic gold.This method tin during molten gold is easily oxidized to insoluble tin ash by chloroazotic acid, hinders
Gold dissolving, 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, make expensive, base metal separation.This method can handle the material of any shape, but treating capacity
Small, efficiency is low.(3) metal fragmentation-dissolution method, roasting forms it at a certain temperature after gold-tin alloy is mixed with metallic aluminium
New alloy, then dissolved using diluted acid and remove tin, aluminium, insoluble matter is again using aqua regia dissolution recovery gold.It is main existing for this method
Problem is wanted to be the introduction of new impurity aluminum, it is necessary to which successive depths impurity and purification, technological process is longer, and tin is not returned effectively
Receive.
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 easily in golden course of dissolution and solution forms colloid, causes filtering to be stranded
Difficulty, substantial amounts of waste water can be produced in wet-treating flow, also contain a small amount of gold in waste water, waste water need to be recycled etc.
Shortcoming.
The Chinese patent of Application No. 201410270455.5 discloses one kind and reclaims 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, loads in nickel or iron crucible, is placed in
In high temperature furnace, in 500~700 DEG C of roasting temperatures 1~3 hour, after reaction terminates, cooling, water logging, after separation of solid and liquid, obtain
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 using hydrochloric acid+oxidant dissolving, obtains gold-containing solution again, and after purification, addition reducing agent obtains high-purity cake of gold.This method carries
Gold needs to add plurality of reagents, long flow path.
The content of the invention
It is an object of the present invention to provide a kind of method of gold-tin alloy separation, it is simple, easily operated.
The present invention is achieved through the following technical solutions：
Step 1: 1.0~1.2 times of vulcanizing agent molar fraction as needed for tin element in gold-tin alloy is changed into sulphided state are added
Vulcanizing agent；
Step 2: it is put into closed container and seals after gold-tin alloy is well mixed with vulcanizing agent, in anaerobic, stirring bar
Under part, control heating-up temperature is vulcanized material at 200 DEG C~500 DEG C；
Step 3: sulfur product obtained by step 2 is put into vacuum drying oven, in 1100 DEG C~1400 DEG C of temperature, vacuum 1
Under~100Pa, it is evaporated in vacuo, sulfide is volatilized, realizes the purpose of golden tin separation.
The 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 more than 2600 DEG C, if be directly difficult to point using vacuum distillation
From.Its volatility is more than corresponding metal after tin metal is changed into sulfide, in the range 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 generation sulfide.Therefore, after gold-tin alloy and sulfurizing agent, tin element, which cures, is changed into sulfide, and golden
Element will not cure, and the material 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 are layered with gold, realize separation；The low boiling impurities such as lead, antimony are with sulphided state or simple substance
State is volatilized with stannous sulfide, so as to realize the separation of gold and tin.
The metal of table 1 and the relation of sulfide saturated vapour pressure and temperature
It is an advantage of the invention that：
(1) technological process is short, and gold, tin point can be achieved by vulcanizing and being evaporated in vacuo two processing steps in stanniferous material
From.
(2) present invention process is full thermal process, waste water will not be produced, in the absence of cost for wastewater treatment.
(3) for comprising only the golden material with tin element, proof gold can be directly obtained using this technique；For containing other miscellaneous
The material of prime element, gold can be enriched in a product using this technique, be advantageous to follow-up gold purification.
(4) stannous sulfide of this technique output can be used as tin metallurgy raw material to return to tin flow, or be used as friction material.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
By gold-tin alloy (weight/mass percentage composition：It is Sn98.22%, Au1.49%, other<0.3%) tin of unvulcanised state in
It is changed into 1.2 times of addition sulphur of vulcanizing agent molar fraction needed for sulphided state.
It is put into closed container and seals after gold-tin alloy is well mixed with sulphur, under conditions of anaerobic, stirring, rises
Temperature carries out vulcanizing treatment.First by temperature control at 200 DEG C~250 DEG C, react 60 minutes.Then anaerobic, stirring condition are kept,
380 DEG C~400 DEG C are warming up to, material and vulcanizing agent is carried out depth vulcanization reaction.After reaction terminates, stop heating, treat 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 after vulcanization, obtain volatile matter and
Residue.Volatile constituent is Sn80.76%, S 19.18%, Au5g/t after testing, residue composition be Sn1.81%,
Au97.33%.
Embodiment 2
By gold-tin alloy (weight/mass percentage composition：Sn89.66%, Au10.32%) in the tin of unvulcanised state be changed into sulphided state
1.1 times of addition sulphur of required vulcanizing agent molar fraction.
It is put into closed container and seals after gold-tin alloy is well mixed with sulphur, under conditions of anaerobic, stirring, rises
Temperature carries out vulcanizing treatment.First by temperature control at 230 DEG C~280 DEG C, react 30 minutes.Then anaerobic, stirring condition are kept,
350 DEG C~400 DEG C are warming up to, material and vulcanizing agent is carried out depth vulcanization reaction.After reaction terminates, stop heating, treat 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 after vulcanization, obtain volatile matter and
Residue.Volatile constituent is Sn78.32%, S 21.46%, Au3g/t after testing, residue composition be Sn1.05%,
Au98.86%.
Embodiment 3
By gold-tin alloy (weight/mass percentage composition：Sn57.66%, Au42.32%) in the tin of unvulcanised state be changed into sulphided state
1.15 times of addition sulphur of required vulcanizing agent molar fraction.
It is put into closed container and seals after gold-tin alloy is well mixed with sulphur, under conditions of anaerobic, stirring, rises
Temperature carries out vulcanizing treatment.First by temperature control at 250 DEG C~300 DEG C, react 30 minutes.Then anaerobic, stirring condition are kept,
450 DEG C~500 DEG C are warming up to, material and vulcanizing agent is carried out depth vulcanization reaction.After reaction terminates, stop heating, treat 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 after vulcanization, obtains volatile matter
And residue.Volatile constituent is Sn78.67%, S21.25%, Au8g/t after testing, residue composition 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, in those of ordinary skill in the art's possessed knowledge, it can also make on the premise of present inventive concept is not departed from
Go out various change.
Claims (2)
- A kind of 1. method of gold-tin alloy separation, it is characterised in that comprise the following steps that：Step 1: 1.0~1.2 times of additions of vulcanizing agent molar fraction as needed for tin element in gold-tin alloy is changed into sulphided state vulcanize Agent；Step 2: it is put into closed container and seals after gold-tin alloy is well mixed with vulcanizing agent, in anaerobic, stirring condition Under, control heating-up temperature is vulcanized material at 200 DEG C~500 DEG C；Step 3: sulfur product obtained by step 2 is put into vacuum drying oven, in 1100 DEG C~1400 DEG C of temperature, vacuum 1~ Under 100Pa, it is evaporated in vacuo, sulfide is volatilized, realizes the purpose of golden tin separation.
- A kind of 2. method of gold-tin alloy separation according to claim 1, it is characterised in that：The vulcanizing agent is sulphur.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109628746A (en) * | 2019-01-03 | 2019-04-16 | 江西铜业技术研究院有限公司 | The extracting method of tin in a kind of silver separating residues |
| CN109777966A (en) * | 2019-03-04 | 2019-05-21 | 昆明理工大学 | A method of vacuum distillation separating indium copper alloy |
| CN111020197A (en) * | 2019-12-09 | 2020-04-17 | 北京有色金属与稀土应用研究所 | Separation and recovery method of gold-tin alloy waste |
| WO2023134017A1 (en) * | 2022-01-17 | 2023-07-20 | 昆明理工大学 | Method for separating and purifying tin and copper from tin refining sulfur slag |
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| 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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2017
- 2017-09-07 CN CN201710802841.8A patent/CN107557585B/en active Active
Patent Citations (4)
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| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109628746A (en) * | 2019-01-03 | 2019-04-16 | 江西铜业技术研究院有限公司 | The extracting method of tin in a kind of silver separating residues |
| 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 |
| CN109777966A (en) * | 2019-03-04 | 2019-05-21 | 昆明理工大学 | A method of vacuum distillation separating indium copper alloy |
| CN109777966B (en) * | 2019-03-04 | 2020-11-17 | 昆明理工大学 | Method for separating indium-copper alloy by vacuum distillation |
| CN111020197A (en) * | 2019-12-09 | 2020-04-17 | 北京有色金属与稀土应用研究所 | Separation and recovery method of gold-tin alloy waste |
| 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 |
| WO2023134017A1 (en) * | 2022-01-17 | 2023-07-20 | 昆明理工大学 | Method for separating and purifying tin and copper from tin refining sulfur slag |
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| CN107557585B (en) | 2019-03-15 |
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