CN116904793B - Purifying remelting method for gold-tin alloy return material - Google Patents
Purifying remelting method for gold-tin alloy return material Download PDFInfo
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- JVPLOXQKFGYFMN-UHFFFAOYSA-N gold tin Chemical compound [Sn].[Au] JVPLOXQKFGYFMN-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 76
- 239000000463 material Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000012535 impurity Substances 0.000 claims abstract description 38
- 230000008018 melting Effects 0.000 claims abstract description 34
- 238000002844 melting Methods 0.000 claims abstract description 34
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010931 gold Substances 0.000 claims abstract description 5
- 229910052737 gold Inorganic materials 0.000 claims abstract description 5
- 239000000155 melt Substances 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 4
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 20
- 239000000956 alloy Substances 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 3
- 230000002950 deficient Effects 0.000 abstract description 3
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 238000005476 soldering Methods 0.000 abstract description 3
- 235000021190 leftovers Nutrition 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 67
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002893 slag Substances 0.000 description 7
- 238000005266 casting Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003353 gold alloy Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- 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
- C22B9/023—By filtering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/02—Alloys based on gold
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Casting Support Devices, Ladles, And Melt Control Thereby (AREA)
Abstract
The invention discloses a purifying remelting method of a gold-tin alloy return material, and relates to the technical field of metal alloy treatment. The invention carries out purification treatment on the return materials such as defective products, leftovers and the like generated in the production of gold-tin soldering flakes, melts and covers the alloy surface by using the covering agent to carry out adsorption, controls the melting temperature and the aperture of the ceramic filter, ensures that the covering agent and impurities on the covering agent are completely separated from gold-tin alloy melt, realizes the effect of purifying the return materials of gold-tin alloy, ensures that the material index is qualified, and can be put into use again, thereby realizing the recycling of gold and tin which are high-value metal elements. The purifying remelting method has high impurity removal rate of 43.3% on the gold-tin alloy return material.
Description
Technical Field
The invention relates to the technical field of metal alloy treatment, in particular to a purifying remelting method of a gold-tin alloy return material.
Background
The gold tin soldering lug is a key packaging interconnection material in the semiconductor micro-assembly industry, and has wide application in the fields of photoelectrons, microwave radio frequency and the like. As a noble metal solder, the material cost occupies a large proportion of the production cost of the product. The gold-tin soldering lug can generate scraps such as scraps and appearance defective products in the processing process, and the scraps can be used as return materials after remelting in order to improve the utilization rate of noble metal materials. However, the return material is inevitably mixed with trace impurities, for example, if no purification measures are taken during remelting, the content of impurities in the prepared gold-tin alloy is increased, and the usability of the material is possibly deteriorated.
At present, the main treatment object of the metal return material purifying remelting technology is mainly high-temperature alloys such as nickel base alloy, and the like, as disclosed in the prior art, is a purifying treatment method for casting the high-temperature alloy return material, which is characterized in that the surface of molten steel after the return material and new material are mixed and refined is covered with specific covering slag CaO-Al 2 O 3 -CaF 2 MgO to capture floating inclusions for purification, but wherein the covering slag is not easily separated from the metal melt, the impurity removal is poor, metal losses are easily caused, and the covering slag has a high melting temperature, mainly for high temperature alloys (capable of long-term operation at temperatures above 600 ℃ C.), and is not suitable for low Wen Gui metal alloys, such as gold-tin alloyGold.
Disclosure of Invention
The invention provides a purifying remelting method for a gold-tin alloy return material, which aims to overcome the defects and defects that the existing purifying remelting technology is not suitable for processing the gold-tin alloy return material and has poor impurity removing effect, and utilizes a covering agent to melt and cover the surface of an alloy for adsorption, and simultaneously controls the melting temperature well, so as to ensure that the covering agent and impurities on the covering agent are completely separated from the gold-tin alloy melt, thereby realizing the effect of purifying the gold-tin alloy return material.
The above object of the present invention is achieved by the following technical scheme:
a purifying remelting method of a gold-tin alloy return material comprises the following steps:
s1, heating a covering agent to a molten state, then adding a gold-tin alloy return material, melting into a melt, and then preserving heat;
s2, reducing the temperature, and separating the mixture of the gold-tin alloy return material melt and the covering agent through a filter after the covering agent is solidified to obtain a purified gold-tin alloy return material;
the covering agent is one of covering agent A, covering agent B and covering agent C; wherein the mass fraction of each component in the covering agent A is Bi 2 O 3 70~80 wt%、B 2 O 3 1-10wt%, 10-20wt% ZnO and 1-10wt% SnO; the mass fraction of each component in the covering agent B is V 2 O 5 60~70 wt%、P 2 O 5 15~30 wt%、TeO 2 1~10 wt%、B 2 O 3 0~5 wt%、ZnO 0~5 wt%、Li 2 0-5 wt% of O; the mass fraction of each component in the covering agent C is P 2 O 5 40~60 wt%、ZnO 30~50 wt%、B 2 O 3 5~15 wt%、Na 2 O 1~10 wt%、Li 2 O 0~5 wt%；
The density of the covering agent is lower than that of the gold-tin alloy;
the melting temperature of the covering agent is higher than that of the gold-tin alloy;
the temperature of the step S2 is reduced to be higher than the melting temperature of the gold-tin alloy and lower than the melting temperature of the covering agent.
The following are to be described:
the density of the covering agent used for smelting the gold-tin alloy return material is lower than that of the gold-tin alloy, and the covering agent can completely cover alloy melt during smelting, thereby playing a role in isolating air and preventing alloy oxidation, and simultaneously adsorbing impurities in the gold-tin alloy return material.
The melting temperature of the covering agent needs to be higher than that of the gold-tin alloy return material, when the temperature in the step S2 is reduced to be between the melting temperature of the covering agent and that of the gold-tin alloy, the covering agent floating on the surface of the alloy melt is solidified, so that the covering agent and impurities adsorbed on the covering agent are blocked by the ceramic filter when the covering agent passes through the ceramic filter, thereby realizing the separation of the impurities and the gold-tin alloy return material and achieving the purpose of purifying the gold-tin alloy return material.
The covering agent comprises B 2 O 3 、SiO 2 、SnO、ZnO、Al 2 O 3 、Na 2 O、Bi 2 O 3 、ZrO 2 、La 2 O 3 、CaO、MgO、P 2 O 5 、V 2 O 5 、TeO 2 、Li 2 At least 4 components in O, and by controlling the components of the covering agent, the melting temperature of the covering agent is adjusted, and meanwhile, the successful adsorption of impurities in the gold-tin alloy return material can be ensured.
Specifically, the density of the gold-tin alloy is 14-15 g/cm 3 。
Specifically, the melting temperature of the gold-tin alloy return material is 280-320 ℃.
Specifically, after the temperature is reduced in step S2, the covering agent is solidified into a block shape, and can be fully intercepted when passing through the ceramic filter.
Specifically, the covering agent is glass.
Specifically, the melting temperature of the covering agent is 400 to 600 ℃, for example, 400 ℃, 430 ℃, 450 ℃, 460 ℃, 500 ℃, 550 ℃, 600 ℃, more specifically 430 to 460 ℃.
The covering agent has too low melting temperature, and is not easy to separate from the alloy melt due to incomplete solidification during casting; the covering agent has too high melting temperature, correspondingly higher melting temperature is adopted, the production cost is increased, and the production efficiency is reduced. Therefore, the melting temperature of the covering agent is controlled, which is beneficial to further improving the purifying effect.
Specifically, in the step S1, the container of the covering agent and the gold-tin alloy return material is a crucible, and the crucible is made of one of stainless steel, titanium alloy, quartz and graphite.
Specifically, the heat preservation time in the step S1 is 10 to 60 minutes, for example, 10 minutes, 15 minutes, 30 minutes, and 60 minutes.
The proper heat preservation time is favorable for promoting the adsorption of the covering agent to impurities, ensuring the uniformity of the components of the alloy melt, and the longer heat preservation time is favorable for removing the impurities, but long-time standing can lead to the tendency of phase separation of the components of the alloy melt, so that the components of the alloy melt are uneven, and the production efficiency can be reduced.
Preferably, the heat preservation time of the step S1 is 15-30 min.
Specifically, in the step S1, the melted tin-gold alloy return material may be stirred by mechanical force or electromagnetic force.
Specifically, the temperature in the step S2 is reduced to 350 to 450 ℃, for example, 350 to 320 ℃, 400 to 420 ℃, 450 ℃, and preferably 370 to 400 ℃.
The temperature in the step S2 is too high, which is not beneficial to the solidification of the covering agent, and the situation that the covering agent is not easy to separate from the alloy melt due to incomplete solidification is more easy to occur during casting; when the temperature is too low, the fluidity of the alloy melt is poor and the casting quality is poor.
Specifically, the difference between the temperature of the step S2 and the melting temperature of the covering agent is 60 to 120 ℃, for example, 60 ℃, 80 ℃, 100 ℃, 110 ℃, more specifically 80 to 110 ℃.
Specifically, in the step S2, the mixture is poured into a mold through a ceramic filter having holes, and recasting of the tin alloy return is performed. The casting mould is made of one of stainless steel, copper alloy and graphite.
Preferably, the covering agent contains 4-5 components.
Specifically, the ceramic filter is cylindrical or cuboid in shape, and holes penetrating through the upper surface and the lower surface are densely distributed.
Specifically, the diameter of the filtering holes of the ceramic filter is less than or equal to 2mm.
The filter pore size is too large, which is not conducive to filtering out residues, and as the alloy melt passes through the filter, some residues may pass through together.
More specifically, the filter is a ceramic filter, and the diameter of the filtering hole is 0.5-2 mm.
When the pore diameter of the filter is too small, the alloy melt is not easy to pass through.
Specifically, the ceramic filter is made of one or more of cordierite, mullite, aluminum titanate, aluminum oxide, zirconium oxide and silicon nitride.
Specifically, the gold-tin alloy return material in the step S1 contains 77-81 wt% of gold.
Specifically, the balance of the gold-tin alloy return material is tin and trace impurities.
Specifically, the mass fraction of the impurity in the gold-tin alloy return material in the step S1 is 0.02 to 0.05%, more specifically 0.03 to 0.04%, for example, 0.03%, 0.031%, 0.032%, 0.033%, 0.035%, 0.04%.
The invention has low equipment requirement for purifying remelting, simple and convenient operation, adaptability to flexible production, small material loss in the remelting process, good purifying effect, and effective control of purifying cost while ensuring low impurity content of the obtained gold-tin alloy.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a purifying and remelting method for gold-tin alloy return materials, which is characterized in that the return materials such as defective products, leftover materials and the like generated in gold-tin solder sheet production are purified, the surface of the alloy is covered by a covering agent in a melting way for adsorption, the melting temperature and the pore diameter of a ceramic filter are controlled, the covering agent and impurities on the covering agent are ensured to be completely separated from gold-tin alloy melt, the effect of purifying the gold-tin alloy return materials is realized, the material index is ensured to be qualified, and the gold and tin which are high-value metal elements can be recycled.
The purifying remelting method has high impurity removal rate of 43.3% to the gold-tin alloy return material.
Detailed Description
Some of the raw materials of the following examples and comparative examples of the present invention are described below:
covering agent 1: covering agent A, the component is Bi 2 O 3 、B 2 O 3 ZnO and SnO with the mass ratio of 72:8:15:5 and the melting temperature of 460 ℃;
covering agent 2: covering agent B containing component V 2 O 5 、P 2 O 5 、TeO 2 、B 2 O 3 、ZnO、Li 2 O, the mass ratio is 64:25:5:2:1.5:2.5, and the melting temperature is 430 ℃;
covering agent 3: covering agent C containing ZnO and B 2 O 3 、P 2 O 5 、Na 2 O、Li 2 O, wherein the mass ratio is 40:8:45:5:2, and the melting temperature is 450 ℃;
the density of the covering agent is lower than that of the gold-tin alloy;
the components of the covering agents are uniformly mixed according to a proportion and then used;
ceramic filter 1: mullite is used as a material, and the pore diameter is 2mm;
ceramic filter 2: the material is alumina, and the aperture is 0.5mm;
ceramic filter 3: the material is zirconia, and the aperture is 4mm.
The elemental content of the gold-tin alloy return used in particular is shown in table 1 below:
TABLE 1 content of elements before treatment of gold-tin alloy return
The mass fraction of gold in the gold-tin alloy return material is 80wt%, and the alloy density is 14.52 g/cm 3 The melting temperature was 280 ℃.
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
Example 1
A purifying remelting method of a gold-tin alloy return material comprises the following steps:
s1, firstly, putting the covering agent 1 into a graphite crucible, heating to 500 ℃ to melt the covering agent, then putting a gold-tin alloy return material into the crucible, and carrying out heat preservation after the return material is completely melted into a melt; the heat preservation time is 15min;
s2, reducing the temperature to 380 ℃, and pouring the mixture of the gold-tin alloy return material melt and the covering agent in the crucible into a casting mould (steel) through a ceramic filter 1 filled with holes after the covering agent is solidified to obtain the purified gold-tin alloy return material.
Example 2
A purifying remelting method for a gold-tin alloy return material, which is the same as that of example 1, is different in that a covering agent 1 is replaced with a covering agent 2.
Example 3
A purifying remelting method for a gold-tin alloy return material, which is the same as that of example 1, is different in that a covering agent 1 is replaced with a covering agent 3.
Example 4
A purifying remelting method for a gold-tin alloy return material is the same as in example 1, except that a ceramic filter 1 is replaced with a ceramic filter 2.
Example 5
A purifying remelting method of a gold-tin alloy return material is the same as in example 1, except that a ceramic filter 1 is replaced with a ceramic filter 3.
Example 6
A purifying remelting method for a gold-tin alloy return material is the same as in example 1, except that step S2 is reduced to a temperature of 350 ℃.
Example 7
A purifying and remelting method for a gold-tin alloy return material is the same as that of example 1, except that step S2 is reduced to 450 ℃.
Example 8
A purifying and remelting method for a gold-tin alloy return material is similar to that of the embodiment 1, and is different in that the heat preservation time of the step S1 is 10min.
Example 9
A purifying and remelting method for a gold-tin alloy return material is similar to that of the embodiment 1, and is different in that the heat preservation time of the step S1 is 30min.
Example 10
A purifying and remelting method for a gold-tin alloy return material is similar to that of the embodiment 1, and is different in that the heat preservation time of the step S1 is 60min.
Comparative example 1
A purifying remelting method for gold-tin alloy return material, the steps are the same as those of example 1, the difference is that covering agent 1 in step S1 is replaced by covering slag CaO-Al 2 O 3 -CaF 2 -MgO, in a mass ratio of 5:2:2:1, said covering slag melting temperature being 1500 ℃.
Comparative example 2
A purifying remelting method for a gold-tin alloy return material is the same as in example 1, except that no covering agent is added in step S1.
Result detection
Impurity removal rate test of purified gold-tin alloy return materials obtained in examples and comparative examples: detecting the impurity content by ICP-OES;
the impurity removal rate is calculated by the following steps:
(total content of impurities before treatment-total content of impurities after treatment)/total content of impurities before treatment.
The results are shown in Table 2.
TABLE 2 impurity removal Rate in gold-tin alloy returns
As can be seen from Table 2, the impurity removal rate of the purifying remelting method for the gold-tin alloy return material is not lower than 26.1%. It can be seen from examples 1 to 3 that the change of the components of the covering agent causes the change of the melting temperature, and the combined action influences the adsorption effect on impurities, so that the impurity removal rate is changed; as can be seen from examples 1, 4 and 5, when the pore diameter of the ceramic filter is 0.5-2 mm, the filtering effect is better and the impurity removal rate is higher than that when the pore diameter is 4 mm; as can be seen from examples 1, 6 and 7, the reduced temperature in step S2 also affects the impurity removal rate, and the low removal rate in example 7 is mainly due to the fact that the temperature is close to the temperature of the covering agent, so that the solidification effect of the covering agent is poor, and the difference between the temperature in step S2 and the melting temperature of the covering agent is preferably 80-110 ℃; it can be seen from examples 1 and 8-10 that the change of the heat preservation time also causes the change of the removal rate, and the impurity removal rate is lower when the heat preservation time is shorter; the effect of removing impurities from the gold-tin alloy return material is significantly reduced by changing the composition of the covering agent or not adding the covering agent in comparative examples 1 and 2, and the effect of removing impurities is rather inferior to that of comparative example 2 after adding the covering slag in comparative example 1, because the covering slag added in comparative example 1 is not easily separated from the alloy melt and has a high melting temperature, and impurities cannot be melt-adsorbed under the conditions of the present invention, resulting in lower impurity removal rate.
TABLE 3 impurity element content (wt%) of gold-tin alloy returns after treatment of example 1 and comparative example 1
As can be seen from Table 3, the gold-tin alloy return material is purified and remelted by adopting the technical scheme of the invention, and the content of each impurity element in the obtained gold-tin alloy return material is obviously reduced, so that the gold-tin alloy return material has better removal effect compared with the scheme of adopting other covering agents in comparative example 1.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (9)
1. The purifying and remelting method for the gold-tin alloy return material is characterized by comprising the following steps of:
s1, heating a covering agent to a molten state, then adding a gold-tin alloy return material, melting into a melt, and then preserving heat;
s2, reducing the temperature, and separating the mixture of the gold-tin alloy return material melt and the covering agent through a filter after the covering agent is solidified to obtain a purified gold-tin alloy return material;
the covering agent is one of covering agent A, covering agent B and covering agent C; wherein the mass fraction of each component in the covering agent A is Bi 2 O 3 70~80 wt%、B 2 O 3 1-10wt%, 10-20wt% ZnO and 1-10wt% SnO; the mass fraction of each component in the covering agent B is V 2 O 5 60~70 wt%、P 2 O 5 15~30 wt%、TeO 2 1~10 wt%、B 2 O 3 0~5 wt%、ZnO 0~5 wt%、Li 2 0-5 wt% of O; the mass fraction of each component in the covering agent C is P 2 O 5 40~60 wt%、ZnO 30~50 wt%、B 2 O 3 5~15 wt%、Na 2 O 1~10 wt%、Li 2 O 0~5 wt%；
The density of the covering agent is lower than that of the gold-tin alloy; the melting temperature of the covering agent is higher than that of the gold-tin alloy; the temperature of the step S2 is reduced to be higher than the melting temperature of the gold-tin alloy and lower than the melting temperature of the covering agent; the melting temperature of the gold-tin alloy return material is 280-320 ℃; the melting temperature of the covering agent is 430-600 ℃.
2. The purifying remelting method of claim 1, wherein the heat preservation time in the step S1 is 10-60 min.
3. The purifying remelting method of claim 1, wherein the heat preservation time in the step S1 is 15-30 min.
4. The method of claim 1, wherein the temperature in step S2 is reduced to 350-450 ℃.
5. The method of claim 1, wherein the difference between the temperature of step S2 and the melting temperature of the covering agent is 60 to 120 ℃.
6. The method of claim 1, wherein the filter is a ceramic filter, and the diameter of the filtering holes is less than or equal to 2mm.
7. The method of purifying and remelting as claimed in claim 6, wherein the ceramic filter has a filtration pore diameter of 0.5 to 2mm.
8. The method of claim 1, wherein the gold-tin alloy return in step S1 contains 77 to 81wt% gold.
9. The purifying remelting method of claim 1, wherein the mass fraction of impurities in the gold-tin alloy return material in the step S1 is 0.02 to 0.05%.
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| JP4949353B2 (en) * | 2008-11-06 | 2012-06-06 | 株式会社タムラ製作所 | How to remove lead |
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| GB347222A (en) * | 1930-01-24 | 1931-04-24 | Alexander Henderson | A new or improved process of refining metals and alloys of low melting points |
| JP2003147453A (en) * | 2001-11-13 | 2003-05-21 | Shirogane:Kk | Low temperature flow-down refining to tin, lead and solder and recycle system for these metal |
| CN104017994A (en) * | 2014-06-17 | 2014-09-03 | 昆明贵金属研究所 | Method for recovering gold and tin from gold-tin alloy scrap |
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