CN115011814B - Method for efficiently recycling tin from tin slag generated in wave soldering - Google Patents
Method for efficiently recycling tin from tin slag generated in wave soldering Download PDFInfo
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- CN115011814B CN115011814B CN202210646961.4A CN202210646961A CN115011814B CN 115011814 B CN115011814 B CN 115011814B CN 202210646961 A CN202210646961 A CN 202210646961A CN 115011814 B CN115011814 B CN 115011814B
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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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- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for efficiently recycling 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 the atmospheric condition, wherein the heating temperature is 850-1050 ℃, and the heat preservation time is 10-30min, so as to obtain a metal tin liquid; the tin slag generated by wave soldering comprises: metallic tin and tin dioxide; the tin dioxide is coated 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 requirements of the reuse production of the wave soldering tin-based brazing material.
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 soldering process adopted in the electronic industry in large quantities at present, and a large amount of tin slag is generated annually. The wave soldering mechanism is to form a solder wave with a specific shape on the liquid surface of a solder tank under the action of a power pump, and the PCB with the components inserted on the conveying belt passes through the solder wave crest at a specific angle and a specific immersion depth to realize the welding process of the solder point. During the soldering process, the solder with high Sn content is easily oxidized in high-temperature soldering, thereby forming oxide residues SnO on the liquid surface of the tin furnace 2 The welding quality is affected, and meanwhile, the waste is caused. Particularly, due to the environmental protection requirement, the use amount of the lead-free solder is greatly increased in recent years, and compared with the Sn-Pb alloy solder, the lead-free solder with high Sn content is easier to oxidize in high-temperature welding, so that a large amount of tin slag with high Sn content is generated every year. The tin slag produced in the industry is characterized by high tin content, and a typical tin slag structure is characterized in that about 90% of available tin metal is distributed in the center, and the outer layer is coated with tin oxide in a powdery state.
In recent two years, the price of tin is continuously increased, and on the basis, how to develop a special environment-friendly, simple and economic production and recovery process aiming at the characteristics of tin slag generated by tin wave soldering is very important.
Disclosure of Invention
Based on the technical problems, the invention provides a method for efficiently recycling tin from tin slag generated in wave soldering, which is simple, environment-friendly and economical and is beneficial to realizing the recycling utilization of the tin slag generated in wave soldering.
The specific scheme of the invention is as follows:
the invention provides a method for efficiently recycling 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 the atmospheric condition, wherein the heating temperature is 850-1050 ℃, and the heat preservation time is 10-30min, so as to obtain a metal tin liquid; the tin slag generated by wave soldering comprises: metallic tin and tin dioxide; the tin dioxide is coated on the outer layer of the metal tin.
The invention uses carbonaceous reducing agent to react at high temperature to generate carbon monoxide, and the carbon monoxide further reduces the tin dioxide in the tin slag generated by wave soldering into elemental tin.
Preferably, tin dross produced by wave soldering is layered alternately with carbonaceous reducing agent in the reactor.
Preferably, the carbonaceous reducing agent layer has a thickness of 30-50 mm/layer and the tin slag layer has a thickness of 100-200 mm/layer.
The alternate layered cloth refers to the alternate layered arrangement of one layer of carbonaceous reducing agent and one layer of tin slag without mixing the carbonaceous reducing agent and the tin slag. On the one hand, the distribution mode can lead the carbonaceous reducing agent to burn insufficiently 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 improved.
Preferably, the carbonaceous reducing agent is 5-20% by weight of the tin dross produced in wave soldering.
Preferably, the carbonaceous reducing agent is selected from one or more of charcoal, chemical coke, metallurgical coke.
Preferably, the carbonaceous reductant particle size is from 5 to 50mm.
Preferably, the carbonaceous reducing agent is charcoal having a charcoal particle size of 25-35mm.
The charcoal with the granularity of 25-35mm is used as a preferable scheme of the carbonaceous reducing agent, and the charcoal with the granularity has higher fixed carbon content, more excellent chemical activity and good air permeability, and is favorable for fully carrying out the reaction.
Preferably, the method further comprises the steps of naturally cooling the molten tin to 250-300 ℃, pouring the molten tin into a cast iron mold, and cooling to obtain a molten tin ingot.
Preferably, the reactor is a graphite crucible; and placing the graphite crucible in an intermediate frequency induction furnace, and performing 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 in wave soldering, which is simple, environment-friendly, high in operability and high in tin recovery rate.
1. Environmental protection: compared with the hydrometallurgical recovery technology, the invention does not generate waste water, and greatly improves the environmental protection level; 2. the investment is low: the method is not required to be carried out under the vacuum condition, can be realized under the atmospheric pressure condition, and has low requirements on production equipment; 3. high recovery rate and purity: the recovery rate of tin can reach more than 95%, the purity of recovered tin can reach more than 99.00%, and the method can meet the requirements of recovering tin for recycling and producing tin-based brazing materials for wave soldering.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
The tin dross for the following examples and comparative examples are tin dross produced in wave soldering, and comprise in weight percent: 85% of metallic tin, 0.7% of copper, less than 0.1% of impurities and the balance of tin dioxide; tin dioxide is coated on the outer layer of the metal tin; the trace impurities are lead, antimony and bismuth. The reactor adopts a No. 200 graphite crucible, and the graphite crucible is placed in a medium-frequency induction furnace with 150KVA power to carry out heating reaction 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, alternately layering and distributing the tin slag and the charcoal, namely paving a layer of charcoal at the bottom of the graphite crucible, paving 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 granularity of the charcoal is 30mm;
(2) Heating the medium frequency induction furnace in which the loaded graphite crucible is placed to 900 ℃ through induction, and preserving heat for 15min, and stirring by a graphite rod during the heating;
(3) Stopping heating, removing carbon ash floating on the surface, naturally cooling to 300 ℃, pouring molten tin into a cast iron mold, cooling, and taking out the molten 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, alternately layering and distributing the tin slag and the charcoal, namely paving a layer of charcoal at the bottom of the graphite crucible, paving 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 granularity of the charcoal is 25mm;
(2) Heating the medium frequency induction furnace in which the loaded graphite crucible is placed to 1000 ℃ through induction, and preserving heat for 10min, and stirring by a graphite rod during the heating;
(3) Stopping heating, removing carbon ash floating on the surface, naturally cooling to 300 ℃, pouring molten tin into a cast iron mold, cooling, and taking out the molten tin ingot.
Example 3
A method for efficiently recovering tin from tin dross produced in wave soldering, in which the carbonaceous reducing agent was replaced by "charcoal" only with "metallurgical coke" having a metallurgical coke particle size of 30mm, as compared with example 1, was the same as in example 1.
Example 4
In comparison with example 1, the method for efficiently recovering tin from tin dross produced in wave soldering only replaces carbonaceous reducing agent with "charcoal" and chemical coke "and the chemical coke has a particle size of 10mm, and all the other steps are the same as in example 1.
Example 5
A method for efficiently recovering tin from tin slag generated in wave soldering comprises the following steps:
(1) Uniformly mixing tin slag generated by 100kg wave soldering with 10kg charcoal, and then placing the mixture in a graphite crucible;
(2) Heating the medium frequency induction furnace in which the loaded graphite crucible is placed to 900 ℃ through induction, and preserving heat for 15min, and stirring by a graphite rod during the heating;
(3) Stopping heating, removing carbon ash floating on the surface, naturally cooling to 300 ℃, pouring molten tin into a cast iron mold, cooling, and taking out the molten tin ingot.
Comparative example 1
A method for recovering tin from tin dross produced in wave soldering, which is similar to example 1 except that the grain size of charcoal was adjusted from 30mm to 2mm only as compared with example 1.
Comparative example 2
A method for recovering tin from tin dross produced in wave soldering, which is similar to example 1 except that the grain size of charcoal was adjusted from 30mm to 55mm only as compared with example 1.
Weighing the weight of the metal tin ingots obtained in the examples and the comparative examples, and calculating the recovery rate; the tin purity was then checked by chemical analysis sampling and the results are shown in table 1 below:
TABLE 1 recovery and purity of recovered tin
| Weight/kg of metallic tin ingot | Recovery/% | Sn purity/% | |
| 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 recovery is calculated as a percentage by dividing "weight of metallic tin ingot" by "weight of tin dross produced by wave soldering".
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. A method for efficiently recovering tin from tin dross produced in wave soldering, comprising: placing tin slag generated by wave soldering and a carbonaceous reducing agent into a reactor, and heating and reacting under the atmospheric condition, wherein the heating temperature is 850-1050 ℃, and the heat preservation time is 10-30min, so as to obtain a metal tin liquid; the tin slag generated by wave soldering comprises: metallic tin and tin dioxide; tin dioxide is coated on the outer layer of the metal tin;
tin slag generated by wave soldering and a carbonaceous reducing agent are alternately layered and distributed in a reactor; the granularity of the carbonaceous reducing agent is 5-50mm.
2. The method for efficiently recovering tin from wave soldering tin dross in accordance with claim 1, wherein the carbonaceous reducing agent layer has a thickness of 30-50 mm/layer and the tin dross layer has a thickness of 100-200 mm/layer.
3. The method for efficiently recovering tin from wave-soldering tin dross according to claim 1 or 2, wherein the carbonaceous reducing agent is 5-20% by weight of the wave-soldering tin dross.
4. The method for efficiently recovering tin from wave soldering tin dross according to claim 1 or 2, wherein the carbonaceous reducing agent is selected from the group consisting of charcoal, chemical coke, and metallurgical coke.
5. The method for efficiently recovering tin from tin dross produced in wave soldering according to claim 1 or 2, wherein the carbonaceous reducing agent is charcoal having a grain size of 25-35mm.
6. The method for efficiently recovering tin from tin dross produced in wave soldering according to claim 1 or 2, further comprising naturally cooling molten tin to 250-300 ℃, pouring into a cast iron mold, and cooling to obtain a metallic tin ingot.
7. The method for efficiently recovering tin from tin dross produced in wave soldering according to claim 1 or 2, wherein the reactor is a graphite crucible; and placing the graphite crucible in an intermediate frequency induction furnace, and performing heating reaction under the atmospheric condition.
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| CN202210646961.4A CN115011814B (en) | 2022-06-09 | 2022-06-09 | Method for efficiently recycling tin from tin slag generated in wave soldering |
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| CN202210646961.4A CN115011814B (en) | 2022-06-09 | 2022-06-09 | Method for efficiently recycling tin from tin slag generated in wave soldering |
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| CN115011814B true CN115011814B (en) | 2023-08-22 |
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| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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- 2022-06-09 CN CN202210646961.4A patent/CN115011814B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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