JP3550537B2 - Extraction method of palladium - Google Patents
Extraction method of palladium Download PDFInfo
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- JP3550537B2 JP3550537B2 JP2000290365A JP2000290365A JP3550537B2 JP 3550537 B2 JP3550537 B2 JP 3550537B2 JP 2000290365 A JP2000290365 A JP 2000290365A JP 2000290365 A JP2000290365 A JP 2000290365A JP 3550537 B2 JP3550537 B2 JP 3550537B2
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- palladium
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Description
【０００１】
【発明の属する技術分野】
本発明は、パラジウムの溶媒抽出方法に関するもので、不純物として、セレン、テルル及び白金等が含有している塩酸溶液からパラジウムの抽出分離に関するものである。
【０００２】
【従来の技術】
パラジウムを含有するとともに、セレン、テルル及び白金等を含有する水溶液からパラジウムを選択的に抽出するための方法としてジアルキルスルファイドを抽出溶剤とする方法が知られている（特開平１０−１３０７４４号公報、特開平９−２７９２６４号公報参照）。
【０００３】
特開平１０−１３０７４４号公報には、金、セレン及び白金族金属の塩化物含有水溶液から金をジブチルカルビトール（ＤＢＣ）中へ抽出し、金を選択除去した溶液を塩酸で希釈して酸性溶液を得、この溶液中のパラジウムを硫化ジアルキル中に抽出し、塩酸を用いてスクラビングし、スクラビングを行った硫化ジアルキルからアンモニア水を用いてパラジウムを逆抽出する段階を含むパラジウムの抽出方法において、塩化物含有水溶液の塩酸濃度を４規定以上に調整し、かつ塩化浸出後液〔Ａ〕に対するジブチルカルビトール（ＢＤＣ）〔Ｏ〕の比率（Ｏ／Ａ）が１／２以上の条件で金の抽出を行うとともに、前記逆抽出後パラジウムを溶解したアンモニア水を濾過する段階を有することを特徴とする方法が記載されている。この方法は、鉄及びテルルによるパラジウムの純度低下を防止するものであって、その特徴とするところは、塩化物含有水溶液の塩酸濃度を４規定以上、好ましくは５規定以上に調整し、かつ塩化浸出の後液〔Ａ〕に対するジブチルカルビトール（ＤＢＣ）〔Ｏ〕の比率（Ｏ／Ａ）が１／２以上の条件で金の抽出を行うとともに、前記逆抽出後パラジウムを溶解したアンモニア水を濾過する点にある。
【０００４】
また、特開平９−２７９２６４号公報には、白金族元素を含有する貴金属溶液からパラジウムを連続的に選択抽出する方法であって、濃度４０％のジアルキルスルファイドを含有する抽出液を、単位時間あたり、上記貴金属溶液中のパラジウム量に対して４モル倍以上のジアルキルスルファイド量となる範囲で、かつ数分以内の接触を他の白金族元素から選択的に抽出する方法が記載されている。このように通液量と接触時間を選択することにより、抽出速度の遅いオスミウムやルテニウム等の抽出が抑制され、パラジウムが選択的に抽出されることが記載されている。
【０００５】
本発明者らは、従来のパラジウムの選択的抽出法によって得られたスポンジパラジウム中に、セレン、白金等の品位が高くなり、規格に合格できないことがあることを見出した。
前記の先行技術はいずれも、パラジウムのロスを抑制することは記載されていない。
また、本発明者らは、パラジウムを選択的に抽出するために成らされたもので、パラジウムを選択的に抽出するために硫化ジアルキルを含む有機溶媒で抽出、スクラビングした後、該抽出有機溶媒を逆抽出する際に、多量のスラッジが発生し、スラッジ中にパラジウムが移行するので、パラジウムを高収率で回収できないという問題点があることを見出した。
【０００６】
【発明が解決しようとする課題】
本発明は、セレン、テルル、及び白金等を含有するパラジウム含有水溶液から、硫化ジアルキルを用いてパラジウムを抽出した有機溶媒からパラジウムを逆抽出する際に、スラッジを多量に発生することなく、パラジウムを選択的に抽出・回収する方法を提供することを課題とする。
【０００７】：
【課題を解決するための手段】
本発明者らは、
（１）セレン、テルル及び白金からなる群の一種以上を含有するパラジウム含有水溶液より、硫化ジアルキルによりパラジウムを溶媒抽出した後、該パラジウムを抽出した有機溶媒相を３．５Ｍ以上の濃度の塩酸で洗浄した後、次いで３．０Ｍより薄い希塩酸で洗浄することを特徴とするパラジウムの抽出方法。を提供する。
【０００８】
【発明の実施の形態】
以下、本発明を、図１に示す貴金属回収フローチャートに沿って説明する。
銅製錬工程において副生する白金やパラジウムを含有する残滓に、塩化浸出を施し、貴金属を水溶液中に溶出させる。この浸出後液からＤＢＣによる金抽出を行う。金を抽出した抽出後液は純水を用いて酸調整してから、硫化ジアルキルによるパラジウム抽出を行う。パラジウムを抽出した硫化ジアルキルはＨＣｌ濃度を３．５Ｍ以上の塩酸溶液にてスクラビングして、その後希塩酸溶液にて洗浄することが本発明の特徴である。その後、アンモニア水で逆抽出すると、パラジウムはジクロロアンミンパラジウム（〔Ｐｄ（ＮＨ３）２〕Ｃｌ２）としてアンモニア水溶液中に溶解してくる。
硫化ジアルキルとしては、ジヘキシルスルフィド（ＤＨＳ）、ジオクチルスルフィドなどが用いられるが、ＤＨＳが好ましい。
【０００９】
以下、実施例により本発明をさらに詳しく説明する。
【実施例１】
ＤＨＳスクラビング時のＨＣｌ濃度（モル／Ｌ、以下単に「Ｍ」）を０．２〜７Ｍまで変化させた条件と、スクラビングを行わないでＤＨＳを逆抽出した時のスラッジ発生量の測定と分相性を観察した。
【００１０】
１）抽出工程
パラジウム抽出後のＤＨＳは図１に示すフローに沿って得たもので、５Ｃの濾紙にて濾過し、濾液を分析試料とした。試験に使用したＤＨＳは表１の組成を有するものである。
【表１】
２）スクラビング工程
表１の組成の抽出後ＤＨＳ４３０ｍｌと、ＨＣｌ濃度が０．２，１．０，３．５，７．０Ｍの塩酸溶液４３０ｍｌを混合して３０分間攪拌した。これによりＳｅ，Ｐｔの除去を行う。
その後、分液ロートに入れて、静置して塩酸相を分離し、次いで希塩酸をＤＨＳ量と同量加えて３０分間攪拌した後、分液ロートに入れて希塩酸相を分離する操作を２回繰り返した。ここで、希塩酸により洗浄するのは、Ｓｅ等の不純物を除去するためである。
【００１２】
３）逆抽出工程
〔００１１〕の各塩酸濃度で洗浄した後のＤＨＳ相（Ｏ）、及び洗浄しないＤＨＳ相（表１に示す抽出後ＤＨＳ）（Ｏ）に８％ＮＨ４ＯＨ（Ａ）をＯ／Ａ比＝１／１．５の混合割合で１時間攪拌して、分液ロートに入れて静置したのち、逆抽出後液を分離して分析した。また分相時に発生したスラッジを濾過分離して、その発生量を秤量した。
逆抽出後液の分析値、有機相と水相の中間に発生する中間相中のスラッジ発生量（有機相に対しての発生量を示す。）及び分相性の結果を表２に示す。
【表２】
表２より、スクラビングしない条件及びスクラビング時のＨＣｌ濃度が低いほど、逆抽出後液中のパラジウム濃度は低く、スラッジ発生量は多くなり、この時の逆抽出液中へのパラジウム回収率は塩酸濃度が高い方が高くなった。スクラビング塩酸濃度が１．０Ｍ以下にすると分相性が悪くなる。
またスクラビングの塩酸濃度が低いほど、逆抽出後液中のパラジウム濃度は低くなっていることから、スラッジへ移行するパラジウム量が多くなり、パラジウムロス量が多くなった。
従って、スクラビング時の塩酸濃度を高くするほど分相性が良く、かつパラジウムの回収率が高くなるが、分相性と塩酸使用量の経済性から判断すると塩酸濃度は３．５Ｍ以上が良いことがわかる。
【００１４】
【発明の効果】
本発明において、セレン、テルル、及び白金等を含有する水溶液からパラジウムを抽出した硫化ジアルキルをスクラビングする際に、３．５Ｍ以上の濃度の塩酸溶液にて洗浄した後、次いで希塩酸溶液にて洗浄することにより、逆抽出する際に、スラッジを大量に発生量することなく、パラジウムの回収率を向上させる効果がある。
【図面の簡単な説明】
【図１】本発明による貴金属回収フローチャートを示す。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a solvent extraction method for palladium, and more particularly to an extraction separation of palladium from a hydrochloric acid solution containing selenium, tellurium, platinum and the like as impurities.
[0002]
[Prior art]
As a method for selectively extracting palladium from an aqueous solution containing palladium and selenium, tellurium, platinum and the like, a method using a dialkyl sulfide as an extraction solvent is known (JP-A-10-130744). And JP-A-9-279264.
[0003]
JP-A-10-130744 discloses that gold is extracted from an aqueous solution containing gold, selenium and a platinum group metal chloride into dibutyl carbitol (DBC), and a solution obtained by selectively removing gold is diluted with hydrochloric acid to obtain an acidic solution. And extracting palladium in the solution into dialkyl sulfide, scrubbing with hydrochloric acid, and back-extracting palladium from the scrubbed dialkyl sulfide using aqueous ammonia. Extraction of gold under conditions that the hydrochloric acid concentration of the aqueous solution containing the substance is adjusted to 4N or more, and the ratio (O / A) of dibutyl carbitol (BDC) [O] to liquid [A] after chlorination and leaching is 1/2 or more. And filtering the aqueous ammonia in which palladium is dissolved after the back-extraction. This method is for preventing the decrease in purity of palladium with iron and tellurium, and it is characterized, the hydrochloric acid concentration of chloride-containing aqueous solution of 4N or higher, preferably adjusted to 5 defined above, and chloride After the leaching , the extraction of gold was performed under the condition that the ratio (O / A) of dibutyl carbitol (DBC) [O] to the liquid [A] was 1/2 or more. The point is to filter.
[0004]
Japanese Patent Application Laid-Open No. 9-279264 discloses a method for continuously and selectively extracting palladium from a noble metal solution containing a platinum group element, wherein an extract containing a dialkyl sulfide having a concentration of 40% is prepared for a unit time. A method is described in which the amount of dialkyl sulfide is at least 4 mole times the amount of palladium in the noble metal solution, and the contact within several minutes is selectively extracted from other platinum group elements. . It is described that by selecting the flow rate and the contact time as described above, extraction of osmium, ruthenium, or the like having a low extraction rate is suppressed, and palladium is selectively extracted.
[0005]
The present inventors have found that in sponge palladium obtained by a conventional selective extraction method of palladium, the quality of selenium, platinum, and the like is high, and the sponge palladium may not be able to pass the standard.
None of the above prior art describes suppressing palladium loss.
Further, the present inventors have been made in order to selectively extract palladium, in order to selectively extract palladium, extracted with an organic solvent containing dialkyl sulfide, and after scrubbing, the extracted organic solvent is extracted. It has been found that a large amount of sludge is generated during back extraction and palladium migrates into the sludge, so that palladium cannot be recovered in a high yield.
[0006]
[Problems to be solved by the invention]
The present invention provides selenium, tellurium, and palladium-containing aqueous solutions containing platinum and the like, when back-extracting palladium from an organic solvent obtained by extracting palladium with dialkyl sulfide, without generating a large amount of sludge, It is an object to provide a method for selective extraction and recovery.
[0007]:
[Means for Solving the Problems]
We have:
(1) After extracting palladium with a dialkyl sulfide from a palladium-containing aqueous solution containing at least one of the group consisting of selenium, tellurium, and platinum, the organic solvent phase from which the palladium is extracted is treated with hydrochloric acid having a concentration of 3.5 M or more. A method for extracting palladium, comprising washing, followed by washing with dilute hydrochloric acid thinner than 3.0 M. I will provide a.
[0008]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, the present invention will be described with reference to the noble metal recovery flowchart shown in FIG.
The residue containing platinum and palladium by-produced in the copper smelting process is subjected to chlorination leaching to elute the noble metal into the aqueous solution. Gold extraction by DBC is performed from the leached liquid. After the extraction of the gold, the acid is adjusted using pure water, and then palladium is extracted with dialkyl sulfide. The feature of the present invention is that the dialkyl sulfide from which palladium is extracted is scrubbed with a hydrochloric acid solution having a HCl concentration of 3.5 M or more, and then washed with a dilute hydrochloric acid solution. Thereafter, when back-extracted with aqueous ammonia, palladium is dissolved in aqueous ammonia solution as dichloroammine palladium ([Pd (NH 3 ) 2 ] Cl 2 ).
As dialkyl sulfide, dihexyl sulfide (DHS), dioctyl sulfide and the like are used, and DHS is preferable.
[0009]
Hereinafter, the present invention will be described in more detail with reference to examples.
Embodiment 1
Conditions in which the HCl concentration (mol / L, hereinafter simply referred to as "M") during DHS scrubbing was changed from 0.2 to 7M, measurement of sludge generation amount when back-extracting DHS without scrubbing, and phase separation Was observed.
[0010]
1) Extraction Step DHS after palladium extraction was obtained according to the flow shown in FIG. 1 and was filtered through a 5C filter paper, and the filtrate was used as an analysis sample. The DHS used in the test has the composition shown in Table 1.
[Table 1]
2) Scrubbing process After extraction of the composition shown in Table 1, 430 ml of DHS and 430 ml of a hydrochloric acid solution having an HCl concentration of 0.2, 1.0, 3.5, or 7.0 M were mixed and stirred for 30 minutes. Thus, Se and Pt are removed.
Thereafter, the mixture was placed in a separating funnel and allowed to stand to separate the hydrochloric acid phase. Then, the same amount of dilute hydrochloric acid as the amount of DHS was added, and the mixture was stirred for 30 minutes. Repeated. Here, the cleaning with dilute hydrochloric acid is for removing impurities such as Se.
[0012]
3) 8% NH 4 OH (A) was added to the DHS phase (O) after washing with each hydrochloric acid concentration in the back extraction step [0011] and the DHS phase without washing (DHS after extraction shown in Table 1) (O). The mixture was stirred at a mixing ratio of O / A = 1 / 1.5 for 1 hour, placed in a separating funnel and allowed to stand, and after back extraction, the liquid was separated and analyzed. Further, sludge generated during the phase separation was separated by filtration, and the generated amount was weighed.
Table 2 shows the analytical values of the liquid after back extraction, the amount of sludge generated in the intermediate phase generated between the organic phase and the aqueous phase (the amount generated for the organic phase), and the results of phase separation.
[Table 2]
From Table 2, the conditions under which no scrubbing was performed and the lower the HCl concentration during scrubbing were, the lower the palladium concentration in the solution after back-extraction and the greater the amount of sludge generated. The higher the higher, the higher. When the concentration of the scrubbing hydrochloric acid is 1.0 M or less, the phase separation becomes poor.
Also, the lower the concentration of hydrochloric acid in the scrubbing, the lower the concentration of palladium in the solution after back-extraction, so that the amount of palladium transferred to the sludge increased, and the amount of palladium loss increased.
Therefore, the higher the hydrochloric acid concentration at the time of scrubbing, the better the phase separation property and the higher the recovery rate of palladium. However, judging from the phase separation property and the economy of the amount of hydrochloric acid used, it can be seen that the hydrochloric acid concentration is better than 3.5 M. .
[0014]
【The invention's effect】
In the present invention, when scrubbing a dialkyl sulfide obtained by extracting palladium from an aqueous solution containing selenium, tellurium, platinum, etc., after washing with a hydrochloric acid solution having a concentration of 3.5 M or more, then washing with a dilute hydrochloric acid solution This has the effect of improving the palladium recovery rate without generating a large amount of sludge during back extraction.
[Brief description of the drawings]
FIG. 1 shows a flowchart of a precious metal recovery according to the present invention.
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| JP2000290365A JP3550537B2 (en) | 2000-09-25 | 2000-09-25 | Extraction method of palladium |
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| JP2000290365A JP3550537B2 (en) | 2000-09-25 | 2000-09-25 | Extraction method of palladium |
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