CN115011814A - Method for efficiently recovering tin from tin slag generated in wave soldering - Google Patents
Method for efficiently recovering tin from tin slag generated in wave soldering Download PDFInfo
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- CN115011814A CN115011814A CN202210646961.4A CN202210646961A CN115011814A CN 115011814 A CN115011814 A CN 115011814A CN 202210646961 A CN202210646961 A CN 202210646961A CN 115011814 A CN115011814 A CN 115011814A
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- tin
- wave soldering
- reducing agent
- dross
- carbonaceous reducing
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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
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
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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
- C22B25/00—Obtaining tin
- C22B25/02—Obtaining tin by dry processes
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- 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
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for efficiently recovering tin from tin slag generated in wave soldering, which comprises the following steps: placing tin slag generated by wave soldering and a carbonaceous reducing agent into a reactor, and heating and reacting under atmospheric conditions, wherein the heating temperature is 850-; the tin dross produced by wave soldering comprises: metallic tin and tin dioxide; the tin dioxide is wrapped on the outer layer of the metal tin. The method is simple and convenient, environment-friendly, strong in operability and high in tin recovery rate, and the obtained recovered tin can meet the requirement of recycling and producing wave soldering tin-based brazing materials.
Description
Technical Field
The invention belongs to the field of tin recovery methods, and particularly relates to a method for efficiently recovering tin from tin slag generated in wave soldering.
Background
Tin wave soldering is a brazing process which is adopted in the electronic industry at present, and generates a large amount of tin slag every year. The wave soldering mechanism is that molten liquid solder forms a solder wave with a specific shape on the liquid surface of a solder tank under the action of a power pump, a PCB inserted with components is placed on a conveyor belt and penetrates through the solder wave through a certain specific angle and a certain immersion depth to realize the process of soldering a welding point. During the brazing processSolder with high Sn content is easily oxidized in high-temperature soldering, so that oxide residue SnO is formed on the liquid surface of a tin furnace 2 The welding quality is affected and waste is caused. Particularly, due to the environmental protection requirement, the usage amount of the lead-free solder is greatly increased in recent years, and the lead-free solder with high Sn content is more easily oxidized in high-temperature welding compared with Sn-Pb alloy solder, so that a large amount of tin dross with high tin content is generated every year. The tin dross produced in this industry is characterized by high tin content, typical dross structure is about 90% of available tin metal distributed in the center, and tin oxide wrapped in the outer layer, in powder form.
The tin price continues to increase in the last two years, and on the basis, it is very important to develop a special environment-friendly, simple and economic production and recovery process aiming at the characteristics of tin dross generated by tin wave soldering.
Disclosure of Invention
Based on the technical problems, the invention provides a method for efficiently recovering tin from tin slag generated by wave soldering, which is simple, environment-friendly and economical and is beneficial to realizing resource utilization of the tin slag generated by the wave soldering.
The specific scheme of the invention is as follows:
the invention provides a method for efficiently recovering tin from tin slag generated in wave soldering, which comprises the following steps: placing tin slag generated by wave soldering and a carbonaceous reducing agent into a reactor, and heating and reacting under atmospheric conditions, wherein the heating temperature is 850-; the tin dross produced by wave soldering comprises: metallic tin and tin dioxide; the tin dioxide is wrapped on the outer layer of the metallic tin.
According to the invention, a carbonaceous reducing agent reacts at a high temperature to generate carbon monoxide, and the carbon monoxide further reduces tin dioxide in tin slag generated by wave soldering into simple substance tin.
Preferably, the tin dross generated by wave soldering and the carbonaceous reducing agent are alternately distributed in layers in the reactor.
Preferably, the thickness of the carbonaceous reducing agent layer is 30-50 mm/layer, and the thickness of the tin dross layer is 100-200 mm/layer.
The alternating layered cloth of the invention means that the carbonaceous reducing agent and the tin dross are not mixed, but a layer of carbonaceous reducing agent and a layer of tin dross are arranged in an alternating and layered way. By adopting the material distribution mode, on one hand, the carbonaceous reducing agent can be insufficiently combusted to generate carbon monoxide; on the other hand, the generated carbon monoxide is fully contacted with the tin dioxide in the tin slag, the dynamic condition of the reduction reaction is improved, the reduction speed and the sufficiency are greatly improved, and the recovery rate is favorably improved.
Preferably, the carbonaceous reducing agent is 5-20% by weight of the dross produced by wave soldering.
Preferably, the carbonaceous reducing agent is selected from the group consisting of one or more of charcoal, chemical coke, metallurgical coke, and combinations thereof.
Preferably, the carbonaceous reducing agent has a particle size of 5 to 50 mm.
Preferably, the carbonaceous reducing agent is charcoal, which has a particle size of 25-35 mm.
The charcoal with the granularity of 25-35mm is used as a preferable scheme of the carbonaceous reducing agent, the charcoal with the granularity has higher fixed carbon content, more excellent chemical activity and good air permeability, and is beneficial to the full reaction.
Preferably, the method also comprises the steps of naturally cooling the metallic tin liquid to 250-300 ℃, pouring the metallic tin liquid into a cast iron mold, and cooling to obtain the metallic tin ingot.
Preferably, the reactor is a graphite crucible; and (3) placing the graphite crucible in a medium-frequency induction furnace, and carrying out heating reaction under the atmospheric condition.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for recovering tin from tin slag generated by wave soldering, which is simple, convenient, environment-friendly, strong in operability and high in tin recovery rate.
1. And (3) environmental protection: compared with the wet metallurgy recovery technology, the invention does not generate wastewater, thereby greatly improving the environmental protection level; 2. the investment is less: the method does not need to be carried out under the vacuum condition, can be realized only under the atmospheric and normal pressure conditions, and has low requirements on production equipment; 3. high recovery rate and high purity: the tin recovery rate of the invention can reach more than 95 percent at most, the purity of the recovered tin can reach more than 99.00 percent at most, and the invention can meet the requirement of producing the tin-based brazing material for wave soldering by recovering tin for reuse.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
The tin dross aimed at in the following examples and comparative examples is the tin dross generated by wave soldering, and comprises the following components in percentage by weight: 85% of metallic tin, 0.7% of copper, less than 0.1% of impurities and the balance of tin dioxide; the tin dioxide is wrapped on the outer layer of the metal tin; the trace impurities are lead, antimony and bismuth. The reactor adopts a No. 200 graphite crucible, the graphite crucible is placed in a medium-frequency induction furnace with 150KVA power, and heating reaction is carried out under the atmospheric condition.
Example 1
A method for efficiently recovering tin from tin slag generated in wave soldering comprises the following steps:
(1) placing 100kg of tin slag generated by wave soldering and 10kg of charcoal in a graphite crucible, and alternately distributing the tin slag and the charcoal in layers, namely laying a layer of charcoal at the bottom of the graphite crucible, then laying a layer of tin slag on the charcoal, and alternately distributing two layers; the thickness of the tin slag layer is 150 mm/layer, and the thickness of the charcoal layer is 40 mm/layer; the particle size of the charcoal is 30 mm;
(2) placing the loaded graphite crucible in a medium-frequency induction furnace, raising the temperature to 900 ℃ by induction, and keeping the temperature for 15min, wherein the graphite crucible is stirred by a graphite rod;
(3) stopping heating, removing carbon ash floating on the surface, naturally cooling to 300 ℃, pouring molten metal tin into a cast iron mold, cooling, and taking out a metal tin ingot.
Example 2
A method for efficiently recovering tin from tin slag generated in wave soldering comprises the following steps:
(1) placing 100kg of tin slag generated by wave soldering and 10kg of charcoal in a graphite crucible, and alternately distributing the tin slag and the charcoal in layers, namely laying a layer of charcoal at the bottom of the graphite crucible, then laying a layer of tin slag on the charcoal, and alternately distributing two layers; the thickness of the tin slag layer is 100 mm/layer, and the thickness of the charcoal layer is 30 mm/layer; the particle size of the charcoal is 25 mm;
(2) placing the loaded graphite crucible in a medium-frequency induction furnace, raising the temperature to 1000 ℃ by induction, and keeping the temperature for 10min, wherein the graphite crucible is stirred by a graphite rod;
(3) stopping heating, removing carbon ash floating on the surface, naturally cooling to 300 ℃, pouring molten metal tin into a cast iron mold, cooling, and taking out a metal tin ingot.
Example 3
Compared with the method in the embodiment 1, the method for efficiently recovering tin from tin slag generated in wave soldering only replaces the carbonaceous reducing agent with metallurgical coke, the granularity of the metallurgical coke is 30mm, and the rest is the same as that in the embodiment 1.
Example 4
Compared with the method in the embodiment 1, the method for efficiently recovering tin from tin slag generated in wave soldering only replaces the carbonaceous reducing agent with chemical coke, wherein the particle size of the chemical coke is 10mm, and the rest is the same as that in the embodiment 1.
Example 5
A method for efficiently recovering tin from tin slag generated in wave soldering comprises the following steps:
(1) uniformly mixing 100kg of tin slag generated by wave soldering and 10kg of charcoal, and then placing the mixture into a graphite crucible;
(2) placing the loaded graphite crucible in a medium-frequency induction furnace, raising the temperature to 900 ℃ by induction, and keeping the temperature for 15min, wherein the graphite crucible is stirred by a graphite rod;
(3) stopping heating, removing carbon ash floating on the surface, naturally cooling to 300 ℃, pouring molten metal tin into a cast iron mold, cooling, and taking out a metal tin ingot.
Comparative example 1
Compared with the method of example 1, the method for recovering tin from tin slag generated by wave soldering only adjusts the particle size of charcoal from 30mm to 2mm, and the rest is the same as that of example 1.
Comparative example 2
Compared with the method of example 1, the method for recovering tin from tin slag generated by wave soldering is the same as the method of example 1 except that the particle size of charcoal is adjusted to 55mm from 30 mm.
Weighing the weights of the metal tin ingots obtained in the embodiment and the comparative proportion, and calculating the recovery rate; the purity of the tin was then determined by chemical analysis with sampling and the results are shown in table 1 below:
TABLE 1 recovery and purity of recovered tin
Weight/kg of metallic tin ingot | Percent recovery% | Purity of Sn/%) | |
Example 1 | 95.86 | 95.86 | 99.26 |
Example 2 | 95.25 | 95.25 | 99.25 |
Example 3 | 92.55 | 92.55 | 98.65 |
Example 4 | 91.48 | 91.48 | 98.45 |
Example 5 | 90.68 | 90.68 | 99.20 |
Comparative example 1 | 88.76 | 88.76 | 98.31 |
Comparative example 2 | 87.55 | 87.55 | 99.12 |
Note that the recovery rate is a ratio calculated by dividing "the weight of metallic tin ingot" by "the weight of dross generated by wave soldering" and expressing the ratio in percentage.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (9)
1. A method for efficiently recovering tin from tin slag generated in wave soldering is characterized by comprising the following steps: placing tin slag generated by wave soldering and a carbonaceous reducing agent into a reactor, and heating and reacting under atmospheric conditions, wherein the heating temperature is 850-; the tin dross produced by wave soldering comprises: metallic tin and tin dioxide; the tin dioxide is wrapped on the outer layer of the metal tin.
2. The method for efficiently recovering tin from tin dross generated in wave soldering according to claim 1, wherein the tin dross generated in wave soldering and the carbonaceous reducing agent are alternately layered and distributed in the reactor.
3. The method for efficiently recovering tin from tin dross generated in wave soldering as recited in claim 1 or 2, wherein the thickness of the carbonaceous reducing agent layer is 30-50 mm/layer, and the thickness of the tin dross layer is 100-200 mm/layer.
4. The method for recovering tin from tin dross produced in wave soldering as recited in any one of claims 1 to 3, wherein the carbonaceous reducing agent is 5 to 20% by weight of the tin dross produced in wave soldering.
5. The method for recovering tin from tin dross generated in wave soldering as recited in any one of claims 1 to 4, wherein the carbonaceous reducing agent is selected from the group consisting of charcoal, chemical coke, and metallurgical coke.
6. The method for efficiently recovering tin from tin slag generated by wave soldering as recited in any one of claims 1 to 5, wherein the carbonaceous reducing agent has a particle size of 5 to 50 mm.
7. A method for recovering tin from tin dross produced in wave soldering as claimed in any one of claims 1 to 6, wherein the carbonaceous reducing agent is charcoal having a particle size of 25 to 35 mm.
8. The method for recovering tin from tin slag generated in wave soldering as recited in any one of claims 1 to 7, further comprising naturally cooling the molten tin to 250-300 ℃, pouring the molten tin into a cast iron mold, and cooling to obtain a tin ingot.
9. A method for efficient recovery of tin from solder dross produced by wave soldering as claimed in any one of claims 1 to 8, wherein the reactor is a graphite crucible; and (3) placing the graphite crucible into a medium-frequency induction furnace, and carrying out heating reaction under the atmospheric condition.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115558810A (en) * | 2022-10-29 | 2023-01-03 | 内蒙古新雨稀土功能材料有限公司 | Method and device for extracting rare earth from bastnaesite |
Citations (6)
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GB776602A (en) * | 1952-09-20 | 1957-06-12 | Billiton Mij Nv | Process for the recovery of tin or tin dioxide from materials containing tin in an oxidic form |
CN85101919A (en) * | 1984-02-07 | 1987-01-10 | 波利顿股份公司 | By contain tin and/reclaim the method for precious metals in the zinc raw material |
RU2115747C1 (en) * | 1997-09-08 | 1998-07-20 | Санкт-Петербургский государственный горный институт им.Г.В.Плеханова (технический университет) | Method for reducing metals from mixture of their oxides |
KR101619340B1 (en) * | 2015-03-16 | 2016-05-11 | 한국생산기술연구원 | Recovery method of Sn from Sn containing dross using dry reduction process |
CN110699558A (en) * | 2019-04-02 | 2020-01-17 | 柳州光华科技有限公司 | Method for extracting high-purity tin from industrial waste |
CN113512645A (en) * | 2021-07-13 | 2021-10-19 | 桂林金格电工电子材料科技有限公司 | Method for mixing and recycling silver tin oxide waste and silver graphite waste |
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2022
- 2022-06-09 CN CN202210646961.4A patent/CN115011814B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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GB776602A (en) * | 1952-09-20 | 1957-06-12 | Billiton Mij Nv | Process for the recovery of tin or tin dioxide from materials containing tin in an oxidic form |
CN85101919A (en) * | 1984-02-07 | 1987-01-10 | 波利顿股份公司 | By contain tin and/reclaim the method for precious metals in the zinc raw material |
RU2115747C1 (en) * | 1997-09-08 | 1998-07-20 | Санкт-Петербургский государственный горный институт им.Г.В.Плеханова (технический университет) | Method for reducing metals from mixture of their oxides |
KR101619340B1 (en) * | 2015-03-16 | 2016-05-11 | 한국생산기술연구원 | Recovery method of Sn from Sn containing dross using dry reduction process |
CN110699558A (en) * | 2019-04-02 | 2020-01-17 | 柳州光华科技有限公司 | Method for extracting high-purity tin from industrial waste |
CN113512645A (en) * | 2021-07-13 | 2021-10-19 | 桂林金格电工电子材料科技有限公司 | Method for mixing and recycling silver tin oxide waste and silver graphite waste |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115558810A (en) * | 2022-10-29 | 2023-01-03 | 内蒙古新雨稀土功能材料有限公司 | Method and device for extracting rare earth from bastnaesite |
CN115558810B (en) * | 2022-10-29 | 2023-08-15 | 内蒙古新雨稀土功能材料有限公司 | Method and device for extracting rare earth from bastnaesite |
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