JPH04108618A - Production of hexaammine platinum (iv) tetrahydroxide - Google Patents
Production of hexaammine platinum (iv) tetrahydroxideInfo
- Publication number
- JPH04108618A JPH04108618A JP22754090A JP22754090A JPH04108618A JP H04108618 A JPH04108618 A JP H04108618A JP 22754090 A JP22754090 A JP 22754090A JP 22754090 A JP22754090 A JP 22754090A JP H04108618 A JPH04108618 A JP H04108618A
- Authority
- JP
- Japan
- Prior art keywords
- anion exchange
- solution
- exchange resin
- hexaammineplatinum
- tetrahydroxide
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- JTAFSELAEYLDJR-UHFFFAOYSA-J platinum(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Pt+4] JTAFSELAEYLDJR-UHFFFAOYSA-J 0.000 title abstract 3
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims abstract description 3
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 abstract description 14
- -1 chlorine ions Chemical class 0.000 abstract description 8
- 229910001923 silver oxide Inorganic materials 0.000 abstract description 7
- 239000000460 chlorine Substances 0.000 abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、ヘキサアンミン白金（ＩＶ）テトラハイドロ
オキサイド（以下ｒＨＡＰ ｔＴＨＪという。）の製造
方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing hexaammineplatinum (IV) tetrahydroxide (hereinafter referred to as rHAP tTHJ).
（従来技術とその問題点）
従来、ＨＡＰｔＴＨを製造する方法としては、ヘキサア
ンミン白金（ＩＶ）テトラクロライド溶液に酸化銀を加
えて塩素イオンを塩化銀の沈澱とし濾過分離してＨＡＰ
ｔＴＨ溶液としていたが、添加した銀と塩素イオンとの
反応が当量反応しに（いために添加する酸化銀量を確定
させに（く、添加した銀が残って混入してしまう欠点が
あった。(Prior art and its problems) Conventionally, HAPtTH was produced by adding silver oxide to a hexaammineplatinum (IV) tetrachloride solution, converting chlorine ions into silver chloride precipitates, and separating them by filtration.
Although a tTH solution was used, there was a drawback that the reaction between the added silver and chlorine ions did not occur in an equivalent manner (it was difficult to determine the amount of silver oxide to be added), and the added silver remained and was mixed in.
（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、陰イオン交換樹脂とヘキサアンミン白金（ＰＪ
）テトラクロライド溶液を接触させて塩素イオンとハイ
ドロオキサイドイオンを交換させることで、不純物の少
ないＨＡＰｔＴＨ溶液を製造する方法を提供することを
目的とする。(Purpose of the Invention) The present invention has been made to solve the drawbacks of the above-mentioned conventional methods.
) An object of the present invention is to provide a method for producing a HAPtTH solution with few impurities by contacting a tetrachloride solution to exchange chlorine ions and hydroxide ions.
（問題点を解決するための手段）
本発明は、塩化白金酸アンモニウムの結晶にアンモニア
水を加えて溶解して調製したヘキサアンミン白金（ＩＶ
）テトラクロライド溶液を陰イオン交換樹脂と接触させ
ることを特徴とするヘキサアンミン白金（ＩＶ）テトラ
ハイドロオキサイドの製造方法であり、前記陰イオン交
換樹脂を前以ってＯＨイオン型に処理しておく製造方法
で、前記接触させる陰イオン交換樹脂量が理論交換量の
２倍以上である製造方法である。(Means for Solving the Problems) The present invention provides hexaammineplatinum (IV
) A method for producing hexaammineplatinum (IV) tetrahydroxide, characterized in that a tetrachloride solution is brought into contact with an anion exchange resin, and the anion exchange resin is previously treated into an OH ion form. In the manufacturing method, the amount of the anion exchange resin brought into contact is at least twice the theoretical exchange amount.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
ヘキサアンミン白金（ＩＶ）テトラクロライド溶液の調
製方法は塩化白金酸溶液にアンモニア水を加えて塩化白
金酸アンモニウムの沈澱を生成し、濾過分離した後、該
沈澱にアンモニア水を加えて加圧で加熱しヘキサアンミ
ン白金（ＩＶ）テトラクロライド溶液（Ｐ ｔ （ＮＨ
３）６ ＣＡ４ ）を調製する。The method for preparing hexaammineplatinum (IV) tetrachloride solution is to add aqueous ammonia to a chloroplatinic acid solution to produce a precipitate of ammonium chloroplatinate, and after separation by filtration, add aqueous ammonia to the precipitate and heat under pressure. hexaammineplatinum(IV) tetrachloride solution (P t (NH
3) Prepare 6CA4).
次いで、前記陰イオン交換樹脂は強塩基陰イオン交換樹
脂を用いるのがよく、例えば三菱化成工業製ダイヤイオ
ンＳＡ Ｉ ＯＡ、またはダイヤイオン５Ａ１２Ａがあ
る。Next, it is preferable to use a strong base anion exchange resin as the anion exchange resin, such as Diaion SA I OA manufactured by Mitsubishi Chemical Industries, Ltd. or Diaion 5A12A.
陰イオン交換樹脂と調製したヘキサアンミン白金（ＩＶ
）テトラクロライド溶液を接触させる前に、陰イオン交
換樹脂をＯＨイオン型にしておく方法は、例えば］、ｌ
の陰イオン交換樹脂をカラムに充填しておき、５９６′
前後の水酸化ナトリウム溶液３１を空間速度５Ｖ＝２で
通液し、次いて純水を同じ＜５Ｖ＝２で通液して流出液
のｐＨが７になるまで行うことが必要である。Hexaammineplatinum (IV) prepared with anion exchange resin
) The method of converting the anion exchange resin into the OH ion form before contacting with the tetrachloride solution is, for example, ], l
The column was filled with anion exchange resin of 596'
It is necessary to pass the sodium hydroxide solutions 31 before and after each other at a space velocity of 5V=2, and then pass pure water at the same <5V=2 until the pH of the effluent reaches 7.
特に、純水を通液してｐＨ＝７まで行うのはナトリウム
イオンの除去をも含んでいる。In particular, passing pure water until pH=7 also includes the removal of sodium ions.
次いで、ＯＨイオン型にした陰イオン交換樹脂に調製し
たヘキサアンミン白金（ＩＶ）テトラクロライド溶液を
接触させる方法は、例えばビーカ内で混合して攪拌して
接触させてもよいが、前記ＯＨイオン型にする操作のよ
うにカラムに充填した陰イオン交換樹脂層に調製したヘ
キサアンミン白金（ＩＶ）テトラクロライド溶液を通液
させる方法が簡便であり分離等の手間も省けるもので、
連続操作を行うのにより好ましいものである。Next, the method of contacting the prepared hexaammineplatinum (IV) tetrachloride solution with the anion exchange resin in the OH ion type may be, for example, by mixing and stirring in a beaker. The method of passing the prepared hexaammineplatinum (IV) tetrachloride solution through the anion exchange resin layer packed in the column is simple and saves the trouble of separation.
This is more preferable for continuous operation.
また、前記通液速度５Ｖ＝Ｏ１１〜０．５でよく、より
好ましくは５Ｖ＝０．２である。Further, the liquid passing rate may be 5V=O11 to 0.5, and more preferably 5V=0.2.
なお、陰イオン交換樹脂の量を陰イオン交換理論量の２
倍以上とするのは、陰イオン交換平衡との関係によるも
ので、該白金化合物の塩素イオンとＯＨイオンとの交換
を完全に行わせるために欠くことのできないポイントで
ある。Note that the amount of anion exchange resin is 2 times the theoretical amount of anion exchange.
The reason why it is more than double is due to the relationship with the anion exchange equilibrium, and is an essential point in order to completely exchange the chlorine ions and OH ions of the platinum compound.
よって、陰イオン交換樹脂に通液する調製したヘキサア
ンミン白金（ＩＶ）テトラクロライド溶液の濃度は特に
限定されるものではないが、薄い液では濃縮操作が必要
になり、濃厚液では通液の際に結晶が発生する可能性が
あり、好ましくは１５ｇ／ｌ〜２０ ｇ／Ｉ！の範囲に
調製したものがよい。Therefore, the concentration of the prepared hexaammineplatinum (IV) tetrachloride solution to be passed through the anion exchange resin is not particularly limited, but a dilute solution requires a concentration operation, and a concentrated solution requires a concentration operation during passing. crystals may occur, preferably 15 g/l to 20 g/l! It is best to prepare it within this range.
以上の方法により、不純物の混入が極めて少ないＨＡＰ
ｔＴＨ溶液を製造することができるものである。By the above method, HAP with extremely low contamination of impurities
It is possible to produce a tTH solution.
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１）
塩化白金酸溶液（Ｐ ｔ ２００ ｇ／ｌ） １００
１ｎｌをＩ！！ビーカに入れ、塩化アンモニウムを加え
て塩化白金酸アンモニウムを沈澱させたのち、該沈澱を
パルプ濾紙を用いて濾過する。(Example 1) Chloroplatinic acid solution (P t 200 g/l) 100
1nl I! ! After placing the mixture in a beaker and adding ammonium chloride to precipitate ammonium chloroplatinate, the precipitate is filtered using pulp filter paper.
次いで、該沈澱をオートクレーブ中に移し入れアンモニ
ア水（２８％）３００ｒｎｌを加え１．８〜２．０ｋｇ
／ｃｒｒｆの圧力下で７３℃に加熱して３時間保持した
。Next, the precipitate was transferred to an autoclave, and 300 rnl of ammonia water (28%) was added thereto to give 1.8 to 2.0 kg.
The mixture was heated to 73°C under a pressure of /crrf and held for 3 hours.
次いで、オートクレーブから取り出した溶液をビー力に
移し、湯浴上で９５℃で加熱し、溶液のｐＨが７になっ
たところで加熱を止めてヘキサアンミン白金（ＩＶ）テ
トラクロライド溶液を調製した。Next, the solution taken out from the autoclave was transferred to a beaker and heated at 95° C. on a hot water bath. When the pH of the solution reached 7, heating was stopped to prepare a hexaammineplatinum (IV) tetrachloride solution.
次いで、該溶液を室温まで冷却し、前以ってＯＨイオン
型にした強塩基陰イオン交換樹脂（三菱化成工業型：ダ
イヤイオン５ＡＩＯＡ）３１を直径１００ｍｍのガラス
製カラムに充填した層に、空間速度５Ｖ＝０．２で通液
した。Next, the solution was cooled to room temperature, and a space was added to a glass column with a diameter of 100 mm filled with a strong base anion exchange resin (Mitsubishi Chemical Industries type: Diaion 5 AIOA) 31 which had been made into an OH ion type. The liquid was passed at a rate of 5V=0.2.
通液した後、陰イオン交換樹脂層に純水をＳ■−０，２
で通液し押出洗浄してＨＡＰｔＴＨ溶液１０４７を得た
。After passing the liquid, pure water was added to the anion exchange resin layer at S■-0,2
HAPtTH solution 1047 was obtained by passing a liquid through the solution and extrusion washing.
該ＨＡＰｔＴＨ溶液の２ｒｎ１分取し、Ｉ／１ ＯＮ塩
酸で電位差滴定したところ滴定に要した塩酸量から、白
金１ｍｏｌに対してＯＨイオンがほぼ４ｍｏｌとなりＨ
ＡＰｔＴＨであることを確認された。A 2rn1 fraction of the HAPtTH solution was titrated potentiometrically with I/1 ON hydrochloric acid. From the amount of hydrochloric acid required for the titration, the amount of OH ions was approximately 4 mol per mol of platinum.
It was confirmed to be APtTH.
なお、該溶液中の塩素イオン濃度は４０ｍｇ／ｌであっ
た。Note that the chloride ion concentration in the solution was 40 mg/l.
（従来例）
実施例１で用いたヘキサアンミン白金（ＩＶ）テトラク
ロライド溶液と同じ液に酸化銀粉末を攪拌下で加えて塩
化銀の白色沈澱の生じないことを確認したところで酸化
銀の添加を止め、濾過分離して純水洗浄した。(Conventional Example) Silver oxide powder was added under stirring to the same solution as the hexaammineplatinum (IV) tetrachloride solution used in Example 1, and after confirming that no white precipitate of silver chloride was formed, the addition of silver oxide was carried out. The mixture was stopped, filtered and washed with pure water.
濾過分離液は大部分はＨＡＰｔＴＨ溶液となっていたが
、溶液中の銀は１００ｍｇ／ｎ含有していた。Most of the filtrated solution was a HAPtTH solution, but the solution contained 100 mg/n of silver.
（発明の効果）
以上の説明で明らかのように、従来法では酸化銀を加え
て塩化銀の沈澱を濾過分離してＨＡＰｔＴＨ溶液を製造
していたが、溶液中に銀が残存することでＨＡＰｔＴＨ
溶液として不純物が多く含有するものであったが、本発
明の方法によれば、溶液中の塩素イオンを極めて少なく
でき、酸化銀を用いることもないので、溶液中の不純物
の少ない安定したものが製造できるというものである。(Effects of the Invention) As is clear from the above explanation, in the conventional method, a HAPtTH solution was produced by adding silver oxide and separating the silver chloride precipitate by filtration.
The solution contained many impurities, but according to the method of the present invention, the chlorine ions in the solution can be extremely reduced and silver oxide is not used, so a stable solution with few impurities can be obtained. It can be manufactured.
Claims (3)
加えて溶解して調製したヘキサアンミン白金（IV）テト
ラクロライド溶液を陰イオン交換樹脂と接触させること
を特徴とするヘキサアンミン白金（IV）テトラハイドロ
オキサイドの製造方法。(1) Hexaammineplatinum (IV) tetrahydro, which is characterized by contacting an anion exchange resin with a hexaammineplatinum (IV) tetrachloride solution prepared by adding ammonia water to crystals of ammonium chloroplatinate and dissolving them. Method for producing oxide.
処理しておく請求項１に記載の製造方法。(2) The manufacturing method according to claim 1, wherein the anion exchange resin is treated in advance into an OH ion type.
の２倍以上である請求項１または２に記載の製造方法。(3) The manufacturing method according to claim 1 or 2, wherein the amount of anion exchange resin brought into contact is at least twice the theoretical exchange amount.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2227540A JP3011747B2 (en) | 1990-08-29 | 1990-08-29 | Method for producing hexaammineplatinum (IV) tetrahydroxide |
| US08/007,871 US5244647A (en) | 1990-08-29 | 1993-01-22 | Process of preparing hexaamminerhodium trihydroxide, hexaammineplatinum (IV) tetrahydroxide, tetraammineplatinum (II) dihydroxide and tetraamminepalladium dihydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2227540A JP3011747B2 (en) | 1990-08-29 | 1990-08-29 | Method for producing hexaammineplatinum (IV) tetrahydroxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04108618A true JPH04108618A (en) | 1992-04-09 |
| JP3011747B2 JP3011747B2 (en) | 2000-02-21 |
Family
ID=16862504
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2227540A Expired - Lifetime JP3011747B2 (en) | 1990-08-29 | 1990-08-29 | Method for producing hexaammineplatinum (IV) tetrahydroxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3011747B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288147A (en) * | 2012-02-27 | 2013-09-11 | 陕西煤业化工技术开发中心有限责任公司 | Preparation method of ammonium chloroplatinate |
| JP2016502967A (en) * | 2012-12-12 | 2016-02-01 | ユミコア・アクチエンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフトＵｍｉｃｏｒｅ ＡＧ ＆ Ｃｏ．ＫＧ | Method for producing aqueous preparation of platinum group element complex |
| CN114349081A (en) * | 2021-12-22 | 2022-04-15 | 昆明贵金属研究所 | Hexaammine platinum compound, preparation method and application thereof in platinum plating on jewelry surface |
-
1990
- 1990-08-29 JP JP2227540A patent/JP3011747B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288147A (en) * | 2012-02-27 | 2013-09-11 | 陕西煤业化工技术开发中心有限责任公司 | Preparation method of ammonium chloroplatinate |
| JP2016502967A (en) * | 2012-12-12 | 2016-02-01 | ユミコア・アクチエンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフトＵｍｉｃｏｒｅ ＡＧ ＆ Ｃｏ．ＫＧ | Method for producing aqueous preparation of platinum group element complex |
| US11702437B2 (en) | 2012-12-12 | 2023-07-18 | Umicore Ag & Co. Kg | Method for producing aqueous preparations of complexes of platinum group metals |
| CN114349081A (en) * | 2021-12-22 | 2022-04-15 | 昆明贵金属研究所 | Hexaammine platinum compound, preparation method and application thereof in platinum plating on jewelry surface |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3011747B2 (en) | 2000-02-21 |
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