JPH03166324A - Recovering method for platinum - Google Patents
Recovering method for platinumInfo
- Publication number
- JPH03166324A JPH03166324A JP30497089A JP30497089A JPH03166324A JP H03166324 A JPH03166324 A JP H03166324A JP 30497089 A JP30497089 A JP 30497089A JP 30497089 A JP30497089 A JP 30497089A JP H03166324 A JPH03166324 A JP H03166324A
- Authority
- JP
- Japan
- Prior art keywords
- platinum
- hydrochloric acid
- exchange resin
- acid solution
- ions
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 65
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims description 126
- 238000000034 method Methods 0.000 title claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 28
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 27
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract description 16
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 12
- 235000019270 ammonium chloride Nutrition 0.000 abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011347 resin Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- -1 platinum ion Chemical class 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、白金とイリジウムを含有する酸性溶液から白
金を分岬回醪する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for distilling platinum from an acidic solution containing platinum and iridium.
（従来技術とその問題点）
従来、イリジウムを含む白金の回収に於いて、イリジウ
ムを含む白金を王水等に溶解し脱硝酸したのち塩化アン
モニウムを加えて白金のアンモニウム錯塩を沈澱させ、
濾過し洗浄して白金を分離回収する方法が行われている
。(Prior art and its problems) Conventionally, in the recovery of platinum containing iridium, platinum containing iridium was dissolved in aqua regia, denitrified, and then ammonium chloride was added to precipitate an ammonium complex salt of platinum.
A method is used to separate and recover platinum by filtering and washing.
しかし、白金とイリジウムの分離が不十分であり純度の
高い白金を得るには上記の白金のアンモニウム錯塩の沈
澱を希塩化アンモニウム溶液で十分洗浄し、該沈澱を加
熱分解したのち、再度王水に溶解し脱硝酸して塩化アン
モニウムを加えて白金のアンモニウム錯塩を沈澱させ、
濾過、洗浄する操作を繰り返し行う必要があった。However, separation of platinum and iridium is insufficient, and in order to obtain high-purity platinum, the precipitate of the ammonium complex salt of platinum is thoroughly washed with a dilute ammonium chloride solution, the precipitate is thermally decomposed, and then it is poured into aqua regia again. Dissolve and denitrate, add ammonium chloride to precipitate ammonium complex salt of platinum,
It was necessary to repeat the filtration and washing operations.
また、白金をアンモニウム錯塩として沈澱させ濾過、洗
浄した際の濾過洗浄液中にはイリジウムと白金が存在し
てしまい白金の分離が不十分となる欠点があった。Furthermore, when platinum is precipitated as an ammonium complex salt, filtered, and washed, iridium and platinum are present in the filtration washing solution, resulting in insufficient separation of platinum.
（発明の目的）
本発明は、上記従来法の欠点を解決するために成された
もので、白金の分離回収を収率よく行うことのできる方
法を提供することを目的とする。(Objective of the Invention) The present invention was accomplished in order to solve the drawbacks of the above-mentioned conventional methods, and an object of the present invention is to provide a method that can separate and recover platinum with good yield.
（問題点を解決するための手段）
本発明は、白金を含有し、他にイリジウムを含む塩酸溶
液より白金を回収する方法に於いて、該塩酸溶液に還元
剤を加えて白金およびイリジウムのイオン価数を変え、
次いで陰イオン交換樹脂に接触させて白金を吸着させて
塩酸溶液中の白金を分離したのち、該陰イオン交換樹脂
を焼却して灰化し、灰化物を水素還元したのち、王水等
に溶解して脱硝酸したのち白金をアンモニウム錯塩とし
て沈澱生成し、濾過分離することを特徴とする白金の回
収方法で、前記還元剤がヒドラジン、亜硫酸水または亜
硫酸ガスである白金の回収方法である。(Means for Solving the Problems) The present invention provides a method for recovering platinum from a hydrochloric acid solution containing platinum and also iridium, in which a reducing agent is added to the hydrochloric acid solution to generate ions of platinum and iridium. change the valence,
Next, the platinum in the hydrochloric acid solution is separated by contacting with an anion exchange resin to adsorb platinum, and then the anion exchange resin is incinerated to ash, the ash is reduced with hydrogen, and then dissolved in aqua regia, etc. This is a method for recovering platinum, which is characterized in that after denitrification, platinum is precipitated as an ammonium complex salt and separated by filtration, and the reducing agent is hydrazine, sulfite water, or sulfite gas.
また、前記王水等に溶解して脱硝酸した溶液を上記に記
載の方法を繰り返し操作することを特徴とする白金の回
収方法である。Furthermore, the platinum recovery method is characterized in that the above-described method is repeatedly performed on a solution that has been dissolved in the aqua regia and denitrified.
まず、陰イオン交換樹脂に白金を吸着させるに先立ち、
還元剤を加えて白金およびイリジウムのイオン価数を変
えておくのは、白金は塩酸溶液中ではほとんどが■価の
イオンとして存在し、イリジウムも同様に■価のイオン
として存在しているが、陰イオン交換樹脂と接触させる
と白金とイリジウムがともに吸着されてしまうので、ヒ
ドラジン、亜硫酸水または亜硫酸ガスを加えて還元する
と白金はＨ価のイオンにイリジウムは■価のイオンにそ
れぞれ還元され、次いで、陰イオン交換樹脂と接触する
と白金のみが吸着し、イリジウムは塩酸溶液中にそのま
ま残る。First, before adsorbing platinum on the anion exchange resin,
The reason why the ionic valences of platinum and iridium are changed by adding a reducing agent is that platinum exists mostly as a valence ion in a hydrochloric acid solution, and iridium also exists as a valence ion. Platinum and iridium are both adsorbed when brought into contact with an anion exchange resin, so when hydrazine, sulfite water, or sulfur dioxide gas is added and reduced, platinum is reduced to H-valent ions and iridium is reduced to ■-valent ions, and then When it comes into contact with an anion exchange resin, only platinum is adsorbed, and iridium remains in the hydrochloric acid solution.
前記還元剤としてヒドラジン、亜硫酸水または亜硫酸ガ
スを用いるのはＳＢＨ等の還元力の強い還元剤では白金
およびイリジウムを金属まで還元してしまうことがあり
、他の還元力の弱い還元剤として重亜硫酸塩や亜硫酸塩
等あるが不純物や他の金属イオンが混入してしまうので
好ましくなく、ヒドラジン、亜硫酸水または亜硫酸ガス
は白金およびイリジウムの塩酸溶液中でそれぞれ価数を
変えるのに適しているものである。The reason for using hydrazine, sulfite water, or sulfur dioxide gas as the reducing agent is that strong reducing agents such as SBH may reduce platinum and iridium to metals, and other reducing agents with weak reducing power include bisulfite. Although there are salts and sulfites, they are undesirable because impurities and other metal ions are mixed in.Hydrazine, sulfite water, and sulfur dioxide gas are suitable for changing the valence of platinum and iridium in hydrochloric acid solutions, respectively. be.
前記陰イオン交換樹脂としては特に限定するものではな
いが、強塩基性の陰イオン交換樹脂で例えばダイヤイオ
ンＳＡＩＯＡ（三菱化成製）で良い。The anion exchange resin is not particularly limited, but a strongly basic anion exchange resin such as Diaion SAIOA (manufactured by Mitsubishi Kasei) may be used.
また、塩酸溶液と陰イオン交換樹脂との接触方法として
はとくに限定されるものではないが、該陰イオン交換樹
脂をカラムに充填し、塩酸溶液をＳＶで０． １〜５
で通液すればよいものである。Further, the method of contacting the hydrochloric acid solution with the anion exchange resin is not particularly limited, but the anion exchange resin is packed in a column and the hydrochloric acid solution is mixed at an SV of 0. 1-5
All you have to do is pass the liquid through it.
次いで、白金を吸着した陰イオン交換樹脂を焼却して灰
化させると吸着した白金はほとんど金属化するが一部酸
化しているので水素還元したのち、王水等で溶解し、必
要であれば濾過したのち、塩酸を加えて加熱脱硝酸して
白金溶液とし、塩化アンモニウムを加えて白金のアンモ
ニウム錯塩として沈澱させ、濾過し、塩化アンモニウム
溶液で洗浄し、乾燥したのち、加熱分解すると金属化し
た白金が得られる。Next, when the anion exchange resin that has adsorbed platinum is incinerated and incinerated, most of the adsorbed platinum becomes metallized, but since it is partially oxidized, it is reduced with hydrogen, and then dissolved with aqua regia, etc., and if necessary, After filtration, hydrochloric acid was added and heat denitrified to obtain a platinum solution, ammonium chloride was added to precipitate an ammonium complex salt of platinum, filtered, washed with an ammonium chloride solution, dried, and then heated and decomposed to metallize. Obtain platinum.
以上の方法によれば白金中のイリジウムを微量とするこ
とができるが、より白金中のイリジウムを除きたい場合
は、前記の水素還元したのち、王水等で溶解し塩酸を加
えて加熱脱硝酸して得た白金溶液を還元剤としてヒドラ
ジン、亜硫酸水または亜硫酸ガスを加えて白金イオンを
■価に還元し以下同様に操作することで可能である。According to the above method, iridium in platinum can be reduced to a trace amount, but if you want to remove even more iridium in platinum, after the hydrogen reduction described above, dissolve it in aqua regia, etc., and add hydrochloric acid to heat denitrification. This can be done by adding hydrazine, sulfite water, or sulfur dioxide gas as a reducing agent to the platinum solution obtained as a reducing agent to reduce the platinum ion to a valence of 2, and then proceeding in the same manner.
以下、本発明に係わる実施例を記載するが、該実施例は
本発明を限定するものではない。Examples related to the present invention will be described below, but the examples are not intended to limit the present invention.
（実施例ｌ）
Ｐ ｔ ２ ｇ／Ｃ Ｉ ｒ ２ ０ ０ｍｇ／Ｉ！
、が含有している３Ｎ塩酸溶液１００−にヒドラジンを
加え、９０℃で４時間反応させて還元し、陰イオン交換
樹Ｂｎ （ダイヤイオンＳＡ １ ０Ａ ：三菱化戒製
）を充填したカラムにＳＶ＝Ｉ．Ｏで通液した後の液中
の白金をＩＣＰで測定したところ、ｍｇ／Ａ以下でイリ
ジウムは１８０ｍｇ／ｌであった。(Example 1) P t 2 g/C I r 2 0 0 mg/I!
Hydrazine was added to a 3N hydrochloric acid solution containing 100% of hydrazine, and the mixture was reacted at 90°C for 4 hours to reduce the hydrazine. =I. When the platinum in the solution after passing with O was measured by ICP, it was less than mg/A and iridium was 180 mg/l.
白金の吸着した陰イオン交換樹脂を大気中８００℃で６
時間焼却し水素炎を当てて還元し、王水に溶解し、塩酸
を加えて加熱脱硝酸し、塩化アンモニウムを加えて白金
のアンモニウム錯塩を沈澱させ、濾過し塩化アンモニウ
ム溶液で洗浄したのち、該沈澱を乾燥し、８００℃で加
熱分解して、水素炎を当てて金属化した白金スポンジを
得た。The anion exchange resin with adsorbed platinum was heated at 800°C in the atmosphere.
After being incinerated for a period of time and reduced by applying a hydrogen flame, dissolved in aqua regia, heated to denitrate by adding hydrochloric acid, ammonium chloride was added to precipitate the ammonium complex salt of platinum, filtered and washed with an ammonium chloride solution. The precipitate was dried, thermally decomposed at 800° C., and metallized platinum sponge was obtained by applying hydrogen flame.
この白金スポンジ中のイリジウムを発光分光分析で測定
したところ４０ｐｐｍであった。Iridium in this platinum sponge was measured by emission spectrometry and was found to be 40 ppm.
（実施例２）
実施例ｌと同じ溶液を平行操作して還元剤として、亜硫
酸水を加えたものと亜硫酸ガスを加えてものの２種をそ
れぞれ陰イオン交換樹脂を充填したカラムにｓｖ＝ｔ．
ｏで通液した後の液中の白金をＩＣＰで測定したところ
、ｌｍｇ／ｆ以下であった、またイリジウムは１７０ｍ
ｇ／ｎと１７５ｍｇ／１であった。(Example 2) The same solution as in Example 1 was operated in parallel, and two types of solutions, one with sulfite water added and the other with sulfur dioxide gas added as a reducing agent, were added to a column packed with anion exchange resin at sv = t.
When the platinum in the liquid after passing at
g/n and 175 mg/1.
白金を吸着した陰イオン交換樹脂を実施例ｌと同様に操
作してそれぞれ白金スポンジを得た。The anion exchange resin adsorbed with platinum was operated in the same manner as in Example 1 to obtain platinum sponges.
その白金スポンジ中のイリジウムを発光分光分析で測定
したところ８０ｐｐｍと６０ｐｐｍであった。Iridium in the platinum sponge was measured by emission spectrometry and found to be 80 ppm and 60 ppm.
（実施例３）
実施例１と同様に操作して得た白金を吸着した陰イオン
交換樹月旨を実施例１と同様に焼却し水素炎を当てて還
元し、王水に溶解し塩酸を加えて加熱脱硝酸した白金溶
液を再度実施例ｌと同様にヒドラジンで還元し、以下同
様に操作して白金スポンジを得た。(Example 3) Anion exchange resin adsorbed with platinum obtained in the same manner as in Example 1 was incinerated in the same manner as in Example 1, reduced by applying a hydrogen flame, dissolved in aqua regia, and dissolved in hydrochloric acid. In addition, the heated platinum solution was reduced with hydrazine in the same manner as in Example 1, and the same procedure was repeated to obtain a platinum sponge.
この白金スポンジ中のイリジウムは検出できなかった。Iridium in this platinum sponge could not be detected.
（発明の効果）
以上のように、本発明の方法によれば従来法では分離回
収か困難であった、白金とイリジウムを含有している塩
酸溶液からの白金の分離回収が、陰イオン交換樹脂を用
いて効率よく行うことができ得られた白金中のイリジウ
ムを微量あるいは本発明の方法を繰り返すことで検出で
きない程度まで除去することができ得られた白金は高純
度のものとすることができ、貴金属という稀少な資源の
リサイクルに貢献すること大なるものである。(Effects of the Invention) As described above, according to the method of the present invention, it is possible to separate and recover platinum from a hydrochloric acid solution containing platinum and iridium, which was difficult to separate and recover using conventional methods. The iridium in the obtained platinum can be removed to trace amounts or to an undetectable level by repeating the method of the present invention, and the obtained platinum can be of high purity. , it is a great contribution to the recycling of rare resources such as precious metals.
Claims (3)
白金を回収する方法に於いて、該塩酸溶液に還元剤を加
えて白金およびイリジウムのイオン価数を変え、次いで
陰イオン交換樹脂に接触させて白金を吸着させて塩酸溶
液中の白金を分離したのち、該陰イオン交換樹脂を焼却
して灰化し、灰化物を水素還元したのち、王水等に溶解
して脱硝酸したのち白金をアンモニウム錯塩として沈澱
生成し、濾過分離することを特徴とする白金の回収方法
。(1) In a method for recovering platinum from a hydrochloric acid solution containing platinum and iridium, a reducing agent is added to the hydrochloric acid solution to change the ion valence of platinum and iridium, and then contact with an anion exchange resin. After separating the platinum in the hydrochloric acid solution by adsorbing the platinum, the anion exchange resin is incinerated to ash, the ash is reduced with hydrogen, and then dissolved in aqua regia etc. for denitrification, and the platinum is removed. A method for collecting platinum, which is characterized by forming a precipitate as an ammonium complex salt and separating it by filtration.
ガスである請求項１に記載の白金の回収方法。(2) The platinum recovery method according to claim 1, wherein the reducing agent is hydrazine, sulfite water, or sulfite gas.
に記載の方法を繰り返し操作することを特徴とする白金
の回収方法。(3) Claim 1: A denitrified solution dissolved in the aqua regia etc.
A method for collecting platinum, comprising repeatedly operating the method described in .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30497089A JPH03166324A (en) | 1989-11-24 | 1989-11-24 | Recovering method for platinum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30497089A JPH03166324A (en) | 1989-11-24 | 1989-11-24 | Recovering method for platinum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03166324A true JPH03166324A (en) | 1991-07-18 |
Family
ID=17939503
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30497089A Pending JPH03166324A (en) | 1989-11-24 | 1989-11-24 | Recovering method for platinum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03166324A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001098335A (en) * | 1999-08-05 | 2001-04-10 | Anglo American Platinum Corp Ltd | Separation of platinum group metal |
| JP2007302944A (en) * | 2006-05-11 | 2007-11-22 | Sumitomo Metal Mining Co Ltd | Method for recovering platinum group element from ion-exchange resin containing adsorbed platinum group element |
| CN111850565A (en) * | 2020-07-16 | 2020-10-30 | 昆山全亚冠环保科技有限公司 | Method for recovering gold and iodine from etching waste liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4945822A (en) * | 1972-08-10 | 1974-05-01 | ||
| JPS50105587A (en) * | 1973-11-19 | 1975-08-20 | ||
| JPS5183801A (en) * | 1974-12-12 | 1976-07-22 | Rhone Poulenc Ind | Aruminakeitantai hatsukin oyobi irijiumuyorinaru shokubaiseibun no kaishuhoho |
-
1989
- 1989-11-24 JP JP30497089A patent/JPH03166324A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4945822A (en) * | 1972-08-10 | 1974-05-01 | ||
| JPS50105587A (en) * | 1973-11-19 | 1975-08-20 | ||
| JPS5183801A (en) * | 1974-12-12 | 1976-07-22 | Rhone Poulenc Ind | Aruminakeitantai hatsukin oyobi irijiumuyorinaru shokubaiseibun no kaishuhoho |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001098335A (en) * | 1999-08-05 | 2001-04-10 | Anglo American Platinum Corp Ltd | Separation of platinum group metal |
| JP2007302944A (en) * | 2006-05-11 | 2007-11-22 | Sumitomo Metal Mining Co Ltd | Method for recovering platinum group element from ion-exchange resin containing adsorbed platinum group element |
| JP4715627B2 (en) * | 2006-05-11 | 2011-07-06 | 住友金属鉱山株式会社 | Method for recovering platinum group element from ion exchange resin adsorbed platinum group element |
| CN111850565A (en) * | 2020-07-16 | 2020-10-30 | 昆山全亚冠环保科技有限公司 | Method for recovering gold and iodine from etching waste liquid |
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