JPH03131529A - Production of potassium tetrachloroplatinate - Google Patents
Production of potassium tetrachloroplatinateInfo
- Publication number
- JPH03131529A JPH03131529A JP26759889A JP26759889A JPH03131529A JP H03131529 A JPH03131529 A JP H03131529A JP 26759889 A JP26759889 A JP 26759889A JP 26759889 A JP26759889 A JP 26759889A JP H03131529 A JPH03131529 A JP H03131529A
- Authority
- JP
- Japan
- Prior art keywords
- potassium
- crystals
- amount
- solution
- platinum
- 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 57
- 239000011591 potassium Substances 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 239000013078 crystal Substances 0.000 claims abstract description 62
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 22
- LIAWOTKNAVAKCX-UHFFFAOYSA-N hydrazine;dihydrochloride Chemical compound Cl.Cl.NN LIAWOTKNAVAKCX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 20
- 239000001103 potassium chloride Substances 0.000 claims description 15
- 235000011164 potassium chloride Nutrition 0.000 claims description 15
- 238000006722 reduction reaction Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 2
- 238000013019 agitation Methods 0.000 abstract 2
- 239000000706 filtrate Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000725 suspension Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005303 weighing 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、テトラクロロ白金酸カリウムの製造方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for producing potassium tetrachloroplatinate.
（従来技術とその問題点）
従来テトラクロロ白金酸カリウムの製造方法は、ヘキサ
クロロ白金酸溶液に塩化カリウムを加えて反応させ、水
浴中で冷却してヘキサクロロ白金酸カリウムの沈澱を生
成し、濾過したのち、熱エタノールを加えて該沈澱を溶
解し、熱時手早く濾過して濾波にジオキサンを加え、水
浴中で冷却して粗ヘキサクロロ白金酸カリウムの沈澱を
生成させ、濾過し少量の水に溶解し真空デシケータ中で
室温で放置し純度の良いヘキサクロロ白金酸カリウム結
晶を得る。(Prior art and its problems) The conventional method for producing potassium tetrachloroplatinate was to add potassium chloride to a hexachloroplatinic acid solution, react it, cool it in a water bath to form a precipitate of potassium hexachloroplatinate, and filter it. Afterwards, add hot ethanol to dissolve the precipitate, quickly filter while hot, add dioxane to the filter, cool in a water bath to form a precipitate of crude potassium hexachloroplatinate, filter and dissolve in a small amount of water. Leave to stand at room temperature in a vacuum desiccator to obtain potassium hexachloroplatinate crystals with good purity.
次いで、該結晶を少量の水に懸濁させて亜硫酸水を少量
づつ加えて還元反応させ、水蒸気浴上で結晶が生成しは
じめる迄濃縮し、次いで、これを室温まで冷却し結晶を
完全に生成させたのち、濾過し、結晶を分離し、冷水に
該結晶を溶解して未溶解物があれば濾過し、濾波にアセ
トン・エーテルの等全混合溶液を加えて急速攪拌してテ
トラクロロ白金酸カリウムを沈澱させる。Next, the crystals are suspended in a small amount of water, sulfurous acid water is added little by little to cause a reduction reaction, concentrated on a steam bath until crystals begin to form, and then cooled to room temperature to completely form crystals. After that, filter it to separate the crystals, dissolve the crystals in cold water, filter if there are any undissolved substances, add a mixed solution of acetone and ether to the filter, stir rapidly, and dissolve tetrachloroplatinic acid. Precipitates potassium.
次いで静置して上澄液をデカンテーションして除き、沈
澱をアセトン・エーテル混合溶液で洗浄し、次にエーテ
ルで洗浄してのち、結晶を濾紙上にて風乾するという方
法であるが極めて製造工程が長く工業生産」ニコスト高
となり、また製造に多（の労力がかかる欠点がある。The method is then left to stand, the supernatant liquid is removed by decantation, the precipitate is washed with a mixed solution of acetone and ether, then washed with ether, and then the crystals are air-dried on a filter paper. It has the disadvantage that the process is long, the cost of industrial production is high, and manufacturing requires a lot of labor.
また、他の方法として前記還元反応に用いた亜硫酸水に
変え蓚酸カリウムを還元し、次いで、はぼ同体積の塩酸
を加えて溶液が沸騰しない程度に加熱し、約半分の体積
のエタノールを加えて放冷しテトラクロロ白金酸カリウ
ムの結晶を生成させる方法は不純物が共存しゃすいく、
製造歩留りが低いという欠点がある。Another method is to reduce potassium oxalate by replacing the sulfurous acid water used in the reduction reaction, then add about the same volume of hydrochloric acid, heat the solution to the extent that it does not boil, and add about half the volume of ethanol. The method of forming crystals of potassium tetrachloroplatinate by leaving it to cool is a method in which impurities coexist.
It has the disadvantage of low manufacturing yield.
また、前記還元反応に二塩酸ヒドラジンを少量づつ加え
攪拌しながら反応温度を５０〜６５℃まで加熱してヘキ
サクロロ白金酸カリウムがわずか不溶のまま残る程度と
したのち約２時間温度を保ったのち、温度を８０〜９０
℃に」二げて反応を完全にし、水浴中で冷却し未反応の
ヘキサクロロ白金酸カリウムを濾過分離してテトラクロ
ロ白金酸カリウムと塩酸の混合溶液を得るというもので
テトラクロロ白金酸カリウムの結晶を得ることができな
いという欠点がある。Further, hydrazine dihydrochloride was added little by little to the reduction reaction, and the reaction temperature was heated to 50 to 65°C while stirring to such an extent that potassium hexachloroplatinate remained slightly insoluble, and the temperature was maintained for about 2 hours. Temperature 80-90
℃ to complete the reaction, cool in a water bath, and filter and separate unreacted potassium hexachloroplatinate to obtain a mixed solution of potassium tetrachloroplatinate and hydrochloric acid. The disadvantage is that it is not possible to obtain
（発明の目的）
本発明は、上記の従来法の欠点を解決するために成され
たもので、簡便な方法で製造歩留りも高く、純度の良い
テトラクロロ白金酸カリウムの結晶を製造する方法を提
供することを目的とするものである。(Objective of the Invention) The present invention was made to solve the above-mentioned drawbacks of the conventional method, and provides a method for producing potassium tetrachloroplatinate crystals with a simple method, high production yield, and good purity. The purpose is to provide
（問題点を解決するための手段）
本発明は、テトラクロロ白金酸カリウムの製造方法にお
いて、ヘキサクロロ白金酸溶液に塩化カリウム水溶液を
加えてヘキサクロロ白金酸カリウムの結晶を析出し、濾
過洗浄して６０〜８０℃で乾燥してヘキサクロロ白金酸
カリウムの結晶を得る工程（イ）と、前記ヘキサクロロ
白金酸カリウムの結晶を計り取り白金量を算出し、希塩
酸に懸濁して白金濃度を４０〜６０ｇ／ｌに調製し、該
算出した白金量から還元反応に必要とする二塩酸ヒドラ
ジン量を算出して計り取り、還元反応温度７０〜９０’
Ｃ攪拌下で二塩酸ヒドラジンを１０ｇ／分〜２０ｇ／分
の速さで加えたのち、該還元反応温度を維持し、攪拌を
継続して２〜３時間熟成させる工程（ロ）と、熟成した
溶液を白金濃度３５〜４５ ｇ／ｌに調製して液量を計
り、該液量の体積の１／２に相当する量の濃塩酸を加え
て攪拌し、一夜間静置したのち濾過して濾波を得る工程
（ハ）と、該濾波の量に等量のエタノールを加えて攪拌
しテトラクロロ白金酸カリウムの結晶を析出させ、濾過
し、エタノールで結晶を洗浄し、：３０℃で乾燥したの
ち１００℃に温度を」−昇させて乾燥する工程（ニ）か
ら成ることを特徴とするテトラクロロ白金酸カリウムの
製造方法である。(Means for Solving the Problems) The present invention provides a method for producing potassium tetrachloroplatinate, in which a potassium chloride aqueous solution is added to a hexachloroplatinic acid solution to precipitate crystals of potassium hexachloroplatinate, which are filtered and washed. Step (a) of obtaining crystals of potassium hexachloroplatinate by drying at ~80°C, and calculating the amount of platinum by weighing the crystals of potassium hexachloroplatinate, and suspending the crystals in dilute hydrochloric acid to give a platinum concentration of 40 to 60 g/l. The amount of hydrazine dihydrochloride required for the reduction reaction was calculated and measured from the calculated amount of platinum, and the reduction reaction temperature was 70-90'.
C. After adding hydrazine dihydrochloride at a rate of 10 g/min to 20 g/min under stirring, maintaining the reduction reaction temperature and continuing stirring for 2 to 3 hours (b), Prepare the solution to have a platinum concentration of 35 to 45 g/l, measure the volume of the solution, add concentrated hydrochloric acid in an amount equivalent to 1/2 of the volume of the solution, stir, let stand overnight, and then filter. Step (c) of obtaining a filter: Add an equal amount of ethanol to the filter and stir to precipitate potassium tetrachloroplatinate crystals, filter, wash the crystals with ethanol, and dry at 30°C. This method for producing potassium tetrachloroplatinate is characterized by comprising a step (d) of subsequently raising the temperature to 100° C. and drying.
以下、本発明の製造方法についてより詳しく説明する。Hereinafter, the manufacturing method of the present invention will be explained in more detail.
ヘキサクロロ白金酸カリウムの結晶を析出させるにおい
て、塩化カリウム水溶液として加え反応を速やかに行わ
せ、しかも反応に必要とする塩化カリウム量より過剰の
塩化カリウムを水溶液で加え、濾過し、２ｗｔ％塩化カ
リウム水溶液で十分に洗浄したのち、６０〜８０℃で−
・夜間乾燥する。To precipitate crystals of potassium hexachloroplatinate, it is added as an aqueous potassium chloride solution to cause the reaction to proceed quickly, and an excess amount of potassium chloride than the amount of potassium chloride required for the reaction is added as an aqueous solution, filtered, and a 2wt% potassium chloride aqueous solution is added. After washing thoroughly with
・Dry overnight.
前記塩化カリウム水溶液を加えるのは結晶を加えると該
結晶の表面でヘキサクロロ白金酸カリウムが析出するた
め純度の低下の原因となるからで、また過剰の塩化カリ
ウムを水溶液で加えるのは、析出したヘキサクロロ白金
酸カリウムが溶解するのを防ぐためで、２ｗｔ％塩化カ
リウム水溶液で十分に洗浄するのは不純物の除去とヘキ
サクロロ白金酸カリウムが溶解するのを防ぐためであり
、乾燥温度を６０〜８０℃で一夜間行うのは温度が高い
と分解しやすく、低いと乾燥時間が長くなるからである
。The reason why the potassium chloride aqueous solution is added is that when crystals are added, potassium hexachloroplatinate precipitates on the surface of the crystals, which causes a decrease in purity.Additionally, adding excess potassium chloride in the form of an aqueous solution prevents the precipitated hexachloroplatinate from being added. This is to prevent potassium platinate from dissolving.The reason for thorough washing with a 2wt% potassium chloride aqueous solution is to remove impurities and prevent potassium hexachloroplatinate from dissolving.The drying temperature is 60 to 80°C. The reason for doing this overnight is that if the temperature is high, it will easily decompose, and if the temperature is low, the drying time will be longer.
また、ヘキサクロロ白金酸カリウムをテトラクロロ白金
酸カリウムに還元させるのを、ヘキサクロロ白金酸カリ
ウムの結晶を計り取り、白金の量を白金含有率４０．１
４ｗｔ％として算出し、希塩酸で溶解して白金濃度を４
０〜６０ｇ／ｌに調製し、還元剤として二塩酸ヒドラジ
ンを用いるのは、還元反応において生成する物質が窒素
と塩酸でありテトラクロロ白金酸カリウムの結晶の純度
に影響しにくいからであり、加える量は白金量に対し化
学反応当量でその加える速さを１０ｇ／分〜２０ｇ／分
としたのは、２０ｇ／分以」二では二塩酸ヒドラジンが
分解して無駄を生じてしまい、１０ｇ／分以下では還元
時間が長くなり作業性に欠けるからである。In addition, when reducing potassium hexachloroplatinate to potassium tetrachloroplatinate, the amount of platinum was determined by measuring the crystals of potassium hexachloroplatinate and determining the amount of platinum at a platinum content of 40.1.
Calculated as 4wt%, and dissolved in dilute hydrochloric acid to reduce the platinum concentration to 4wt%.
The reason why hydrazine dihydrochloride is used as a reducing agent is because the substances produced in the reduction reaction are nitrogen and hydrochloric acid, which do not easily affect the purity of potassium tetrachloroplatinate crystals. The amount is a chemical reaction equivalent to the amount of platinum, and the adding rate is 10 g/min to 20 g/min. This is because the reduction time becomes longer and workability is lowered.
なお、上記の還元反応を行う条件として、ヘキサクロロ
白金酸カリウムの結晶を希塩酸（０，５〜１． ０規定
）に溶解して還元反応を安定した状態で速やかに行える
ようにし、攪拌下で湯浴上で７０〜９０℃で反応させ、
二塩酸ヒドラジンを加え終えてから、反応温度を維持し
攪拌を継続して２〜３時間熟成させる。The conditions for carrying out the above reduction reaction are to dissolve potassium hexachloroplatinate crystals in dilute hydrochloric acid (0.5 to 1.0 normal) so that the reduction reaction can be carried out quickly and in a stable state, and to boil the water under stirring. React on a bath at 70-90°C,
After adding hydrazine dihydrochloride, the reaction temperature is maintained and stirring is continued for 2 to 3 hours to age.
希塩酸を用いるのは還元反応を速やかに行わせるためで
、１．０規定以上の塩酸溶液では二塩酸ヒドラジンが分
解しやすく無駄となり、０．５規定以下では還元反応が
不安定となるためで、また、反応温度を７０〜９０℃と
したのは９０℃以上では白金ブラックが生成しやすくな
り、７０℃以下では反応時間が長（なるからである。The reason for using diluted hydrochloric acid is to quickly carry out the reduction reaction.If the hydrochloric acid solution is more than 1.0N, hydrazine dihydrochloride will be easily decomposed and wasted, and if it is less than 0.5N, the reduction reaction will be unstable. Further, the reaction temperature was set to 70 to 90°C because platinum black tends to be generated at temperatures above 90°C, and the reaction time becomes long at temperatures below 70°C.
次いで、濃塩酸を還元し熟成した溶液の体積の１／２の
量を加え攪拌して一夜間静置する。Next, 1/2 of the volume of the solution obtained by reducing and aging concentrated hydrochloric acid is added, stirred, and allowed to stand overnight.
その後、水を用いないで濾過し、濾波と等量のエタノー
ルを加えて攪拌しテトラクロロ白金酸カリウムの結晶を
析出させ、濾過し、エタノールで洗浄し、次いで、３０
℃で十分に乾燥したのち、１００℃以下で乾燥するとテ
トラクロロ白金酸カリウムの結晶が得られる。After that, it was filtered without using water, and the same amount of ethanol as the filter was added and stirred to precipitate crystals of potassium tetrachloroplatinate, filtered, washed with ethanol, and then
After sufficient drying at 100° C., crystals of potassium tetrachloroplatinate are obtained by drying at 100° C. or lower.
エタノールを加えるのはテトラクロロ白金酸カリウムの
溶解度を利用して結晶を析出させるためで、その量は前
記の如く等量で十分である。The reason for adding ethanol is to precipitate crystals by utilizing the solubility of potassium tetrachloroplatinate, and as mentioned above, the same amount is sufficient.
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）
ヘキサクロロ白金酸溶液（Ｐ ｔ ５０ ｇ／ｌ＞
１１に塩化カリウム水溶液（ＫＣＡ ２３０ ｇ／ｌ＞
２．３βを加え攪拌してヘキサクロロ白金酸カリウムの
結晶を析出させたのち静置し、３μ濾紙を用いて濾過し
、該結晶を７０℃空気乾燥機内で１２時間乾燥した。(Example 1) Hexachloroplatinic acid solution (P t 50 g/l>
11, potassium chloride aqueous solution (KCA 230 g/l>
After adding 2.3β and stirring to precipitate crystals of potassium hexachloroplatinate, the mixture was allowed to stand, filtered using 3 μ filter paper, and the crystals were dried in an air dryer at 70° C. for 12 hours.
次いで、結晶を５０ｇ計り取り０． ７規定の希塩酸溶
液に溶解して白金濃度として５０ｇ／ｆ！、に調製し、
湯浴中で７０℃に加熱し、攪拌下で白金量に当量の二塩
酸ヒドラジン６．０ｇを２０ｇ／分の速さで加え、その
後、加熱温度と攪拌を維持して３時間熟成して、テトラ
クロロ白金酸カリウム溶液とした。Next, 50g of crystals were weighed out and 0. Dissolved in 7N diluted hydrochloric acid solution to give a platinum concentration of 50g/f! , prepared in
Heated to 70°C in a water bath, added 6.0 g of hydrazine dihydrochloride equivalent to the amount of platinum at a rate of 20 g/min under stirring, and then aged for 3 hours while maintaining the heating temperature and stirring. A potassium tetrachloroplatinate solution was prepared.
次いで、該溶液に水を加えて白金濃度として４０ｇ／ｊ
７に調製し、その体積の１／２の濃塩酸を加え攪拌し、
一夜間静置した。Next, water was added to the solution to give a platinum concentration of 40 g/j.
7, add 1/2 of its volume of concentrated hydrochloric acid and stir.
It was left undisturbed overnight.
静置後、乾いた濾紙で濾過し、濾波と等量のエタノール
を加え攪拌してテトラクロロ白金酸カリウムの結晶を析
出させ、該結晶を乾いた濾紙を用いて濾過しエタノール
で４回洗浄したのち、３０℃に設定した空気乾燥機内で
５時間乾燥したのち、１００℃に温度を上げて１０時間
乾燥してテトラクロロ白金酸カリウムの結晶４２．５ｇ
を得た。After standing still, it was filtered through a dry filter paper, and an amount of ethanol equal to that of the filter was added and stirred to precipitate crystals of potassium tetrachloroplatinate.The crystals were filtered using a dry filter paper and washed four times with ethanol. After that, it was dried in an air dryer set at 30°C for 5 hours, and then the temperature was raised to 100°C and dried for 10 hours to obtain 42.5 g of potassium tetrachloroplatinate crystals.
I got it.
該結晶をＸ線回折により分析したところテトラクロロ白
金酸カリウム以外の化合物は検出されず、白金の投入量
から製造歩留りは６０％であった。When the crystals were analyzed by X-ray diffraction, no compounds other than potassium tetrachloroplatinate were detected, and the production yield was 60% based on the amount of platinum input.
（実施例２）
ヘキサクロロ白金酸溶液（Ｐｔ５０ｇ／１）１１に塩化
カリウム水溶液（ＫＣｌ ２３０ ｇ／ｌ）２．３１！
を加え攪拌してヘキサクロロ白金酸カリウムの結晶を析
出させたのち静置し、３μ濾紙を用いて濾過し、該結晶
を７０℃空気乾燥機内で１２時間乾燥した。(Example 2) Hexachloroplatinic acid solution (Pt50g/1) 11 to potassium chloride aqueous solution (KCl 230g/l) 2.31!
was added and stirred to precipitate crystals of potassium hexachloroplatinate, then allowed to stand, filtered using 3 μ filter paper, and the crystals were dried in an air dryer at 70° C. for 12 hours.
次いで、結晶を５０ｇ計り取り１． Ｏ規定の希塩酸
溶液に溶解して白金濃度として４５ ｇ／Ｉ！に調製し
、湯浴中で９０℃に加熱し、攪拌下で白金量と当量の二
塩酸ヒドラジン６、Ｏｇを１０ｇ／分の速さで加え、そ
の後、加熱温度と攪拌を保持して２時間熟成して、テト
ラクロロ白金酸カリウム溶液とした。Next, weigh out 50g of crystals and 1. Platinum concentration is 45 g/I when dissolved in dilute hydrochloric acid solution with O standard! was prepared and heated to 90°C in a hot water bath, and while stirring, hydrazine dihydrochloride 6,0g in an amount equivalent to the amount of platinum was added at a rate of 10 g/min, and then the heating temperature and stirring were maintained for 2 hours. It was aged to obtain a potassium tetrachloroplatinate solution.
次いで、該溶液に水を加えて白金濃度として４０ｇ／ｌ
に調製し、その体積の１／２の濃塩酸を加え攪拌し、一
夜間静置した。Next, water was added to the solution to give a platinum concentration of 40 g/l.
1/2 of the volume of concentrated hydrochloric acid was added thereto, stirred, and allowed to stand overnight.
静置後、乾いた濾紙で濾過し、濾波と等量のエタノール
を加え攪拌してテトラクロロ白金酸カリウムの結晶を析
出させ、該結晶を乾いた濾紙を用いて濾過しエタノール
で４回洗浄したのち、３０℃に設定した空気乾燥機内で
５時間乾燥したのち、１００℃に温度を上げて１０時間
乾燥してテトラクロロ白金酸カリウムの結晶４３．２ｇ
を得た。After standing still, it was filtered through a dry filter paper, and an amount of ethanol equal to that of the filter was added and stirred to precipitate crystals of potassium tetrachloroplatinate.The crystals were filtered using a dry filter paper and washed four times with ethanol. After that, it was dried in an air dryer set at 30°C for 5 hours, and then the temperature was raised to 100°C and dried for 10 hours to obtain 43.2 g of potassium tetrachloroplatinate crystals.
I got it.
該結晶をＸ線回折により分析したところテトラクロロ白
金酸カリウム以外の化合物は検出されず、白金の投入量
から製造歩留りは６１％であった。When the crystals were analyzed by X-ray diffraction, no compounds other than potassium tetrachloroplatinate were detected, and the production yield was 61% based on the amount of platinum input.
（従来例）
ヘキサクロロ白金酸の結晶を少量の水で溶解し、塩化カ
リウム結晶を過剰に加えて攪拌し水浴中で冷却してヘキ
サクロロ白金酸カリウムの結晶を析出させ、濾過し、６
０℃に加熱したエタノール中に濾過した結晶を溶解し、
手早く濾過して過剰の塩化カリウムを分離し、得られた
濾波にジオキサンを加えて水浴中で冷却して再びヘキサ
クロロ白金酸カリウムの結晶を析出させ、濾過し、少量
の水で再び結晶を溶解して、真空デシケータ（０，５Ｔ
ｏｒｒ以下）中、室温で一夜間放置して結晶を得た。(Conventional example) Hexachloroplatinic acid crystals are dissolved in a small amount of water, potassium chloride crystals are added in excess, stirred, cooled in a water bath to precipitate potassium hexachloroplatinate crystals, and filtered.
Dissolve the filtered crystals in ethanol heated to 0 °C,
Quickly filter to separate excess potassium chloride, add dioxane to the resulting filter, cool in a water bath to precipitate potassium hexachloroplatinate crystals again, filter, and dissolve the crystals again with a small amount of water. and a vacuum desiccator (0.5T
orr or less) at room temperature overnight to obtain crystals.
次いで、該結晶を少量の水中に懸濁させ、水蒸気浴上で
８５℃で攪拌しながら、亜硫酸水を１ｒｒＩ加え亜硫酸
ガス臭がなくなってから再び亜硫酸水を加えるという操
作を繰り返し行い還元反応を終えたのち、水蒸気浴」−
で８５℃で濃縮し、結晶が析出しはじめたら止めて、室
温まで冷却し、濾過した結晶を冷水に溶解し、未反応の
ヘキサクロロ白金酸カリウムを濾過し、濾波に体積の約
１０倍量のアセトン・エーテル等量混合溶液を加えて急
速に攪拌してテトラクロロ白金酸カリウムの結晶を析出
させ、静置したのち、デカンテーションして上澄液を除
き、結晶をアセトン・エーテル等量混合溶液を加えて攪
拌し静置しデカンテーションして上澄液を除（操作を３
回行い、次いで、エーテルで同様に３回行い、濾紙上に
結晶を移し、風乾してテトラクロロ白金酸カリウムの結
晶３５．１ｇを得た。Next, the crystals were suspended in a small amount of water, and while stirring on a steam bath at 85°C, 1rrl of sulfurous acid water was added, and after the sulfurous gas odor disappeared, sulfurous acid water was added again. This operation was repeated to complete the reduction reaction. Later, steam bath”
Concentrate at 85°C, stop when crystals start to precipitate, cool to room temperature, dissolve the filtered crystals in cold water, filter unreacted potassium hexachloroplatinate, and add about 10 times the volume to the filter. Add a mixed solution of equal amounts of acetone and ether and stir rapidly to precipitate crystals of potassium tetrachloroplatinate.After standing, decant the supernatant liquid and remove the crystals from a mixed solution of equal amounts of acetone and ether. Add to
The reaction was repeated three times, and then the same reaction was performed three times with ether, and the crystals were transferred onto a filter paper and air-dried to obtain 35.1 g of potassium tetrachloroplatinate crystals.
投入したヘキサクロロ白金酸の結晶から、得られたテト
ラクロロ白金酸カリウムの製造歩留りを白金について算
出すると３３％であった。The production yield of potassium tetrachloroplatinate obtained from the hexachloroplatinic acid crystals charged was calculated to be 33% with respect to platinum.
（発明の効果）
以上説明したように、本発明の製造方法によれば、従来
法とくらべ、簡便で約４時間の製造時間の短縮が可能で
あり、投入したヘキサクロロ白金酸からの製造歩留りが
約２倍向上し、生成させたテトラクロロ白金酸カリウム
の純度も高く、極めて効果大なるものと言える。(Effects of the Invention) As explained above, the production method of the present invention is simpler and can shorten the production time by about 4 hours compared to the conventional method, and the production yield from input hexachloroplatinic acid can be improved. The improvement is about twice as high, and the purity of the produced potassium tetrachloroplatinate is also high, so it can be said that it is extremely effective.
Claims (1)
、ヘキサクロロ白金酸溶液に塩化カリウム水溶液を加え
てヘキサクロロ白金酸カリウムの結晶を析出し、濾過洗
浄して６０〜８０℃で乾燥してヘキサクロロ白金酸カリ
ウムの結晶を得る工程（イ）と、前記ヘキサクロロ白金
酸カリウムの結晶を計り取り白金量を算出し、希塩酸に
懸濁して白金濃度を４０〜６０ｇ／ｌに調製し、該算出
した白金量から還元反応に必要とする二塩酸ヒドラジン
量を算出して計り取り、還元反応温度７０〜９０℃攪拌
下で二塩酸ヒドラジンを１０ｇ／分〜２０ｇ／分の速さ
で加えたのち、該還元反応温度を維持し、攪拌を継続し
て２〜３時間熟成させる工程（ロ）と、熟成した溶液を
白金濃度３５〜４５ｇ／ｌに調製して液量を計り、該液
量の体積の１／２に相当する量の濃塩酸を加えて攪拌し
、一夜間静置したのち濾過して濾波を得る工程（ハ）と
、該濾波の量に等量のエタノールを加えて攪拌しテトラ
クロロ白金酸カリウムの結晶を析出させ、濾過し、エタ
ノールで結晶を洗浄し、３０℃で乾燥したのち１００℃
に温度を上昇させて乾燥する工程（ニ）から成ることを
特徴とするテトラクロロ白金酸カリウムの製造方法。(1) In the method for producing potassium tetrachloroplatinate, a potassium chloride aqueous solution is added to a hexachloroplatinic acid solution to precipitate potassium hexachloroplatinate crystals, which are filtered and washed and dried at 60 to 80°C. Step (a) of obtaining crystals of potassium hexachloroplatinate, calculating the amount of platinum by measuring the crystals of potassium hexachloroplatinate, suspending in dilute hydrochloric acid to adjust the platinum concentration to 40 to 60 g/l, and reducing from the calculated amount of platinum. Calculate and measure the amount of hydrazine dihydrochloride required for the reaction, and add hydrazine dihydrochloride at a rate of 10 g/min to 20 g/min while stirring at a reduction reaction temperature of 70 to 90°C. Step (b) of aging the solution for 2 to 3 hours while maintaining the temperature and stirring for 2 to 3 hours, and adjusting the aged solution to a platinum concentration of 35 to 45 g/l, measuring the liquid volume, and adding 1/2 of the volume of the liquid. A step (c) of adding an equivalent amount of concentrated hydrochloric acid, stirring, leaving it to stand overnight, and then filtering to obtain a filter (c); Adding an equal amount of ethanol to the filter and stirring to obtain potassium tetrachloroplatinate. Crystals were precipitated, filtered, washed with ethanol, dried at 30°C, and then heated at 100°C.
A method for producing potassium tetrachloroplatinate, comprising the step (d) of drying by increasing the temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26759889A JP2820289B2 (en) | 1989-10-13 | 1989-10-13 | Method for producing potassium tetrachloroplatinate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26759889A JP2820289B2 (en) | 1989-10-13 | 1989-10-13 | Method for producing potassium tetrachloroplatinate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03131529A true JPH03131529A (en) | 1991-06-05 |
| JP2820289B2 JP2820289B2 (en) | 1998-11-05 |
Family
ID=17446961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26759889A Expired - Fee Related JP2820289B2 (en) | 1989-10-13 | 1989-10-13 | Method for producing potassium tetrachloroplatinate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2820289B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001022915A3 (en) * | 1999-09-29 | 2001-10-25 | Pliva Lachema As | Process for production of cis-dichloro-(trans-1-1,2-cyclohexanediamine)platinum(ii) |
| CN102390874A (en) * | 2011-08-01 | 2012-03-28 | 山东铂源化学有限公司 | Preparation method of potassium chloroplatinite |
| CN105441693A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for separating and extracting platinum group metals |
| CN112126789A (en) * | 2020-09-17 | 2020-12-25 | 朱俊 | Chloroplatinic acid solution concentration process and equipment |
| WO2021045709A1 (en) * | 2019-09-05 | 2021-03-11 | T.C. Marmara Üni̇versi̇tesi̇ | Platinum recovery method |
| CN114315912A (en) * | 2021-12-28 | 2022-04-12 | 江西贝特利新材料有限公司 | Preparation method of cis-dichlorobis (diethyl sulfide) platinum (II) |
-
1989
- 1989-10-13 JP JP26759889A patent/JP2820289B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001022915A3 (en) * | 1999-09-29 | 2001-10-25 | Pliva Lachema As | Process for production of cis-dichloro-(trans-1-1,2-cyclohexanediamine)platinum(ii) |
| CN102390874A (en) * | 2011-08-01 | 2012-03-28 | 山东铂源化学有限公司 | Preparation method of potassium chloroplatinite |
| CN105441693A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for separating and extracting platinum group metals |
| WO2021045709A1 (en) * | 2019-09-05 | 2021-03-11 | T.C. Marmara Üni̇versi̇tesi̇ | Platinum recovery method |
| CN112126789A (en) * | 2020-09-17 | 2020-12-25 | 朱俊 | Chloroplatinic acid solution concentration process and equipment |
| CN114315912A (en) * | 2021-12-28 | 2022-04-12 | 江西贝特利新材料有限公司 | Preparation method of cis-dichlorobis (diethyl sulfide) platinum (II) |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2820289B2 (en) | 1998-11-05 |
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