JP5950103B2 - Separation of precious metals and sulfate impurities - Google Patents
Separation of precious metals and sulfate impurities Download PDFInfo
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- JP5950103B2 JP5950103B2 JP2012147408A JP2012147408A JP5950103B2 JP 5950103 B2 JP5950103 B2 JP 5950103B2 JP 2012147408 A JP2012147408 A JP 2012147408A JP 2012147408 A JP2012147408 A JP 2012147408A JP 5950103 B2 JP5950103 B2 JP 5950103B2
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims description 41
- 238000000926 separation method Methods 0.000 title claims description 15
- 239000012535 impurity Substances 0.000 title claims description 14
- 239000010970 precious metal Substances 0.000 title claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 58
- 229910000510 noble metal Inorganic materials 0.000 claims description 36
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims description 23
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 20
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 20
- 235000011152 sodium sulphate Nutrition 0.000 claims description 20
- 239000007791 liquid phase Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 230000005484 gravity Effects 0.000 claims description 13
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 9
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 9
- 235000011151 potassium sulphates Nutrition 0.000 claims description 9
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002893 slag Substances 0.000 description 14
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052788 barium Inorganic materials 0.000 description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 101000601610 Drosophila melanogaster Heparan sulfate N-sulfotransferase Proteins 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052956 cinnabar Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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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- Manufacture And Refinement Of Metals (AREA)
Description
本発明は、貴金属等の乾式精製を行う際に、不純物成分である鉛やバリウムを溶融塩として分離除去する方法に関する。 The present invention relates to a method for separating and removing lead and barium, which are impurity components, as a molten salt when dry purification of noble metals and the like is performed.
銅の電解精製によって生じる陽極泥（スライム）には銀等の貴金属が含まれており、湿式製錬または乾式製錬によって貴金属が分離され回収されている。従来、乾式製錬ではスライム中に含まれる不純物成分である鉛やバリウムを酸化物にし、これをシリケート系のスラグにして分離除去していた。 Anode mud (slime) generated by electrolytic refining of copper contains noble metals such as silver, and the noble metals are separated and recovered by wet smelting or dry smelting. Conventionally, in dry smelting, lead and barium, which are impurity components contained in slime, are converted into oxides, which are separated and removed as silicate slag.
例えば、銅電解スライムを硫酸浴に浸漬して銅電解スライム中の銅を溶出させて残渣と分離し、該残渣を焙焼してＳｅ等を揮発分離し、この焙焼澱物を各種の貴金属含有繰返し物と混合し、さらに硅石と鉄屑とコ−クスとを加え、電気炉にて加熱熔融して、還元反応により貴金属を含む貴鉛とＦｅＯ−ＳｉＯ2系のスラグとを生成させる乾式処理方法が知られている〔特開２００４−７６１４２号公報、特開２００４−９１８９８号公報〕。 For example, copper electrolytic slime is immersed in a sulfuric acid bath to elute the copper in the copper electrolytic slime and separate from the residue. The residue is roasted to separate Se and the like by volatilization, and the roasted starch is converted into various precious metals. A dry type that mixes with the containing repeating product, further adds meteorite, iron scrap and coke, heats and melts in an electric furnace, and generates noble lead containing noble metal and FeO-SiO 2 slag by reduction reaction Processing methods are known [Japanese Patent Laid-Open Nos. 2004-76142 and 2004-91898].
貴金属が含まれる陽極泥には鉛やバリウムが硫酸塩の形で含まれている。これらを乾式処理法において分離除去するには、硫酸塩を酸化物に還元した後に、硅砂等の溶剤を添加してシリケート系のスラグを生成させ、このスラグに酸化鉛や酸化バリウムを含有させる。このスラグは比重差によって貴金属相の上側に浮くので、スラグを掻き出して貴金属相と分離される。 Anode mud containing precious metals contains lead and barium in the form of sulfate. In order to separate and remove these in a dry processing method, after reducing the sulfate to an oxide, a solvent such as cinnabar is added to produce a silicate-based slag, and the slag contains lead oxide or barium oxide. Since this slag floats above the noble metal phase due to the specific gravity difference, the slag is scraped out and separated from the noble metal phase.
従来の上記乾式処理において、陽極スライムに含まれる鉛やバリウムなどの硫酸塩を酸化物にするためには、還元剤としてコークスやメタル鉄等を加えて加熱する。このため、熱源はもちろんのこと、還元剤や溶剤が必要であり、反応も長時間かかる。また、陽極スライムに含まれる硫酸バリウムは、銅アノードを鋳造する際に使用される離型剤に由来しており、スライム中の含有量が多い。さらに、硫酸バリウムは非常に安定であるため酸化物にするのは容易ではない。この硫酸バリウムを還元せずに、そのまま固体の硫酸塩の形態で排出しようとすると、スラグ中に懸垂し、極めて高粘性で流動性の劣るスラグになり、スラグ中への銀の懸垂ロスを招き操業にも支障をきたすことになる。 In the conventional dry treatment, in order to convert sulfates such as lead and barium contained in the anode slime into oxides, coke and metal iron are added as a reducing agent and heated. For this reason, not only a heat source but also a reducing agent and a solvent are required, and the reaction takes a long time. Moreover, the barium sulfate contained in the anode slime is derived from the release agent used when casting the copper anode, and the content in the slime is large. Furthermore, since barium sulfate is very stable, it is not easy to make it an oxide. If this barium sulfate is not reduced and is discharged in the form of solid sulfate as it is, it will be suspended in the slag, resulting in a slag with extremely high viscosity and poor fluidity, leading to silver suspension loss in the slag. This will also hinder operations.
本発明は、従来の上記乾式処理における上記問題を解決したものであり、陽極スライムなどに含まれる貴金属を、硫酸鉛や硫酸バリウム等の不純物から乾式処理によって分離する際に、従来の方法よりも低い加熱温度で処理することができ、スラグ化の時間も短く、作業効率が大幅に改善された処理方法を提供する。 The present invention solves the above-mentioned problems in the conventional dry processing, and when separating the noble metal contained in the anode slime from impurities such as lead sulfate and barium sulfate by dry processing, than the conventional method. Provided is a processing method which can be processed at a low heating temperature, has a short slag time, and has greatly improved work efficiency.
本発明は、以下に示す構成によって上記問題を解決した分離方法に関する。
〔１〕貴金属と共に硫酸鉛および硫酸バリウムを含む貴金属含有原料に、硫酸ナトリウムまたは硫酸カリウムを加えて加熱することによって、８００℃において液相の硫酸鉛と硫酸バリウムと硫酸ナトリウムまたは硫酸カリウムの三元系硫酸塩を生成させ、この三元系硫酸塩と貴金属とを比重差によって分離することを特徴とする貴金属と硫酸塩不純物の分離方法。
〔２〕上記[１] に記載する分離方法において、硫酸鉛５０質量％〜８５質量％、硫酸バリウム３０質量％、および硫酸ナトリウム１０質量％〜４５質量％からなる８００℃において液相の三元系硫酸塩を生成させる貴金属と硫酸塩不純物の分離方法。
上記[１]に記載する貴金属と硫酸塩不純物の分離方法。
〔３〕上記[１]または上記[２]に記載する分離方法において、坩堝内で、８００℃において液相の硫酸鉛と硫酸バリウムと硫酸ナトリウムまたは硫酸カリウムの三元系硫酸塩を生成させ、坩堝を傾けて上記液相の三元系硫酸塩を流れ出させる貴金属と硫酸塩不純物の分離方法。
The present invention relates to a separation method that solves the above problem by the following configuration.
[1] A ternary of lead sulfate, barium sulfate, sodium sulfate or potassium sulfate in liquid phase at 800 ° C. by adding sodium sulfate or potassium sulfate to a noble metal-containing raw material containing lead sulfate and barium sulfate together with the noble metal and heating. A method for separating a noble metal and a sulfate impurity, characterized in that a sulfate is produced and the ternary sulfate and the noble metal are separated by a difference in specific gravity.
[2] In the separation method described in [1 ] above, a liquid phase ternary is formed at 800 ° C., comprising 50% by mass to 85% by mass of lead sulfate, 30% by mass of barium sulfate, and 10% by mass to 45% by mass of sodium sulfate. For separating precious metals and sulfate impurities to form sulfates.
The method for separating a noble metal and a sulfate impurity as described in [1] above.
[3] In the separation method described in [1] or [2] above, in a crucible, liquid phase lead sulfate, barium sulfate, sodium sulfate or potassium sulfate ternary sulfate is produced at 800 ° C., A method for separating noble metal and sulfate impurities by tilting the crucible and allowing the liquid phase ternary sulfate to flow out.
〔具体的な説明〕
本発明の処理方法は、貴金属と共に硫酸鉛および硫酸バリウムを含む貴金属含有原料に、硫酸ナトリウムまたは硫酸カリウムを加えて加熱することによって、８００℃において液相の硫酸鉛と硫酸バリウムと硫酸ナトリウムまたは硫酸カリウムの三元系硫酸塩を生成させ、この三元系硫酸塩と貴金属とを比重差によって分離することを特徴とする貴金属と硫酸塩不純物の分離方法である。
[Specific description]
In the treatment method of the present invention, sodium sulfate or potassium sulfate is added to a noble metal-containing raw material containing lead sulfate and barium sulfate together with a noble metal, and heated, thereby liquid lead sulfate, barium sulfate, sodium sulfate or sulfuric acid at 800 ° C. This is a method for separating a noble metal and a sulfate impurity, characterized in that a ternary sulfate of potassium is produced and the ternary sulfate and the noble metal are separated by a difference in specific gravity.
本発明の分離方法において、貴金属と共に硫酸鉛および硫酸バリウムを含む貴金属含有原料とは、例えば、銅の電解精製によって生じる陽極スライム、工程内で発生する煙灰や澱物などである。該原料に含まれている貴金属とは銀等である。また、該原料に含まれている硫酸鉛および硫酸バリウムは融点が１１００℃以上の硫酸塩であり、具体的には、例えば、硫酸鉛の融点は１１７５℃、硫酸バリウムの融点は１５８０℃であり、何れも融点１１００℃以上の高融点物質である。
In the separation method of the present invention, the noble metal-containing raw material containing lead sulfate and barium sulfate together with the noble metal is, for example, anode slime generated by electrolytic refining of copper, smoke ash and starch generated in the process, and the like. The noble metal contained in the raw material is silver or the like. In addition, lead sulfate and barium sulfate contained in the raw material are sulfates having a melting point of 1100 ° C. or higher. Specifically, for example, lead sulfate has a melting point of 1175 ° C. and barium sulfate has a melting point of 1580 ° C. These are high-melting-point substances having a melting point of 1100 ° C. or higher.
本発明の分離方法は、硫酸鉛や硫酸バリウムと共に三元系溶融硫酸塩を形成する硫酸ナトリウムまたは硫酸カリウムを上記貴金属含有原料に加えて加熱し、８００℃において液相の低融点の三元系溶融硫酸塩を生成させる。
In the separation method of the present invention, sodium sulfate or potassium sulfate that forms a ternary molten sulfate together with lead sulfate or barium sulfate is added to the above-mentioned noble metal-containing raw material and heated, and at 800 ° C., a liquid phase low melting point ternary system A molten sulfate is formed.
本発明の分離方法は、例えば、貴金属と共に硫酸鉛および硫酸バリウムを含む貴金属含有原料に硫酸ナトリウムを添加して加熱することにっよって、硫酸鉛５０質量％〜８５質量％、硫酸バリウム３０質量％、および硫酸ナトリウム１０質量％〜４５質量％からなる８００℃において液相の三元系硫酸塩を生成させ、この三元系硫酸塩と貴金属とを比重差によって分離する方法である。In the separation method of the present invention, for example, sodium sulfate is added to a noble metal-containing raw material containing lead sulfate and barium sulfate together with the noble metal and heated, so that lead sulfate is 50 mass% to 85 mass%, barium sulfate is 30 mass%. In addition, a ternary sulfate in a liquid phase is produced at 800 ° C. composed of 10% by mass to 45% by mass of sodium sulfate, and the ternary sulfate and noble metal are separated by a difference in specific gravity.
硫酸鉛、硫酸バリウム、および硫酸ナトリウムを加えて加熱溶融して形成した三元系硫酸塩の状態図を図１に示す。図示するように、硫酸鉛３０質量％〜９０質量％、硫酸ナトリウム１０質量％〜６０質量％、および残余が硫酸バリウムの領域は概ね１０００℃において液相の三元系硫酸塩であり、硫酸鉛５０質量％〜８５質量％、硫酸ナトリウム１０質量％〜４５質量％、および残余が硫酸バリウムの領域は概ね８００℃において液相の三元系硫酸塩である。
FIG. 1 shows a phase diagram of a ternary sulfate formed by adding lead sulfate, barium sulfate, and sodium sulfate and heating and melting them. As shown in the figure,
本発明は、例えば、貴金属と共に硫酸鉛および硫酸バリウムを含む貴金属含有原料について、硫酸鉛５０質量％〜８５質量％、硫酸ナトリウム１０質量％〜４５質量％、および硫酸バリウムが３０質量％未満の組成になるように硫酸ナトリウムを加えて加熱し、８００℃において液相の三元系溶融硫酸塩を形成する。
In the present invention, for example, a noble metal-containing raw material containing lead sulfate and barium sulfate together with a noble metal,
なお、図１の状態図に示すように、硫酸バリウムの含有量が５０質量％以上になると、三元系硫酸塩の融点が１０００℃を上回るので、原料に加える硫酸ナトリウムの量は、生成される三元系硫酸塩において硫酸バリウムが５０質量未満、好ましくは３０質量％未満になる量を用いる。 As shown in the phase diagram of FIG. 1, when the barium sulfate content is 50% by mass or more, the melting point of the ternary sulfate exceeds 1000 ° C., so the amount of sodium sulfate added to the raw material is generated. In such a ternary sulfate, an amount that makes barium sulfate less than 50 mass%, preferably less than 30 mass%, is used.
一般に銀等の貴金属の比重よりも上記三元系硫酸塩の比重は小さいので、上記三元系硫酸塩を生成させることによって硫酸塩のままスラグ化し、比重差によって貴金属と硫酸塩を分離することができる。本発明の分離方法は、貴金属と共に原料に含まれる高融点の硫酸鉛および硫酸バリウムを８００℃において液相の三元系溶融硫酸塩に変えて溶融状態にし、比重差によって貴金属と分離するので、原料に含まれる貴金属は金属の状態でもよく、化合物の状態でもよい。
In general, the specific gravity of the ternary sulfate is smaller than the specific gravity of noble metals such as silver. Therefore, by producing the ternary sulfate, it is converted into slag as sulfate, and the noble metal and sulfate are separated by the specific gravity difference. Can do. In the separation method of the present invention, the high melting point lead sulfate and barium sulfate contained in the raw material together with the noble metal are changed to a liquid phase ternary molten sulfate salt at 800 ° C., and separated from the noble metal due to the difference in specific gravity. The noble metal contained in the raw material may be in a metal state or a compound state.
本発明の分離方法は、原料の陽極スライム等に含まれる不純物成分の鉛やバリウムを硫酸塩の形態のまま、硫酸ナトリウム及び/または硫酸カリウム等の硫酸塩を添加して加熱し、８００℃において液相の三元系溶融硫酸塩にするので、貴金属を含む相と不純物成分の鉛やバリウムを比重差によって容易に分離することができる。
In the separation method of the present invention, lead or barium, which is an impurity component contained in the anode slime as a raw material, is heated in the form of a sulfate while adding a sulfate such as sodium sulfate and / or potassium sulfate at 800 ° C. Since the liquid phase ternary molten sulfate is used, the phase containing noble metal and the impurity components lead and barium can be easily separated by the difference in specific gravity.
また、本発明の分離方法では、スラグの組成を、シリケートスラグから溶融硫酸塩に変えることにより、溶融温度を、例えば従来の１１００℃から低下させることができ、重油等の燃料を削減でき、しかもスラグ化に要する時間が短時間になり、また、上記液相の三元系溶融硫酸塩は坩堝を傾けると流れ出すので分離が容易であり、作業効率も大幅に改善される。
In the separation method of the present invention, the melting temperature can be lowered from , for example, the conventional 1100 ° C. by changing the slag composition from silicate slag to molten sulfate, and fuel such as heavy oil can be reduced. The time required for slag formation is shortened, and the ternary molten sulfate in the liquid phase flows out when the crucible is tilted, so that the separation is easy and the working efficiency is greatly improved.
以下に本発明の実施例を示す。なお、融点は熱分析装置TG-DTAを用い、混合溶融塩のＤＴＡの吸熱ピークから溶融点を測定した。 Examples of the present invention are shown below. The melting point was measured from the endothermic peak of DTA of the mixed molten salt using a thermal analyzer TG-DTA.
〔実施例１〕
貴金属として銀を含み、不純物として硫酸鉛、硫酸バリウムを含む原料として、Ａｇを６ｇ(３２.４質量％)、ＰｂＳＯ4を１０.２ｇ(５５.１質量％)、ＢａＳＯ4を２.３ｇ(１２.５質量％)をよく混合して原料を調製した。この原料に添加剤としてＮａ2ＳＯ4を２.６ｇ加え、さらに混合した。その後、この混合した材料をマグネシア坩堝に入れ、空気中、温度１０００℃に加熱して溶融し、１時間保持した。その後、坩堝を常温に取り出し、水噴霧により急冷した。この坩堝を切断し断面を観察したところ、銀（比重１０.５）と溶融塩（比重３.５）は比重差により完全に分離しており、銀が回収された。
[Example 1]
As a raw material containing silver as a noble metal, lead sulfate and barium sulfate as impurities, 6 g (32.4 mass%) of Ag, 10.2 g (55.1 mass%) of PbSO 4 , and 2.3 g of BaSO 4 ( 12.5% by mass) was mixed well to prepare a raw material. To this raw material, 2.6 g of Na 2 SO 4 was added as an additive and further mixed. Thereafter, the mixed material was put in a magnesia crucible, heated and melted in air at a temperature of 1000 ° C. and held for 1 hour. Thereafter, the crucible was taken out to room temperature and quenched with water spray. When this crucible was cut and the cross section was observed, silver (specific gravity 10.5) and molten salt (specific gravity 3.5) were completely separated due to the difference in specific gravity, and silver was recovered.
〔実施例２〕
ＰｂＳＯ4：１０.２ｇ(６８wt％)、ＢａＳＯ4：２.３ｇ(１５wt％)、Ｎａ2ＳＯ4：２.６ｇ(１７wt％)を坩堝に入れて混合し、１０００℃に加熱して溶融し、１時間保持し、実施例１の溶融硫酸塩と同組成の三元系硫酸塩を調製した。この溶融状態の硫酸塩は坩堝を傾けると流れ出し、低粘性であり良好な流動性を有するものであった。
[Example 2]
PbSO 4 : 10.2 g (68 wt%), BaSO 4 : 2.3 g (15 wt%), Na 2 SO 4 : 2.6 g (17 wt%) are mixed in a crucible, heated to 1000 ° C. and melted. Holding for 1 hour, a ternary sulfate having the same composition as the molten sulfate of Example 1 was prepared. This molten sulfate flowed out when the crucible was tilted, and had a low viscosity and good fluidity.
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