JPS6147440A - Preparation of palladium acetate - Google Patents
Preparation of palladium acetateInfo
- Publication number
- JPS6147440A JPS6147440A JP16976084A JP16976084A JPS6147440A JP S6147440 A JPS6147440 A JP S6147440A JP 16976084 A JP16976084 A JP 16976084A JP 16976084 A JP16976084 A JP 16976084A JP S6147440 A JPS6147440 A JP S6147440A
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- mixture
- heat
- palladium acetate
- acetic acid
- 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
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は酢酸パラジウムの調製に関するものであり、特
に高純度の酢酸パラジウムを調製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 the preparation of palladium acetate, and particularly to a method for preparing high purity palladium acetate.
（従来の技術）
酢酸パラジウムは種々の有機化学反応の触媒として有用
なものであシ、酢酸パラジウムの調製法としては、通常
、パラジウム金属を、硝酸を酸化剤として酢酸中で加熱
処理する方法が一般に知られている。(Prior Art) Palladium acetate is useful as a catalyst for various organic chemical reactions, and the usual method for preparing palladium acetate is to heat-treat palladium metal in acetic acid using nitric acid as an oxidizing agent. generally known.
（発明が解決しようとする問題点）
しかしながら、この方法で調製される酢酸パラジウムは
例えば、硝酸根などの窒素分を微量に含むことになり、
窒素分の含有量が多い酢酸パラジウムを触媒として用い
る場合には、適用する反応によっては、触媒の反応活性
が大幅に低下することがあるため、触媒として用いる酢
酸パラジウムとしては、できる限り高純度のものが望ま
れている。(Problems to be Solved by the Invention) However, palladium acetate prepared by this method contains a trace amount of nitrogen such as nitrate radicals,
When palladium acetate, which has a high nitrogen content, is used as a catalyst, the reaction activity of the catalyst may decrease significantly depending on the reaction to which it is applied. something is desired.
（発明の目的）
本発明は、窒素含有量の極めて少ない高純度の酢酸パラ
ジウムを調製する方法の提供を目的とする。(Objective of the Invention) The object of the present invention is to provide a method for preparing highly pure palladium acetate with extremely low nitrogen content.
（問題点を解決するための手段）
本発明は、パラジウム粉末を硝酸の存在下、酢酸中で加
熱処理することによシ酢酸パラジウムを調製するに当シ
、加熱処理後の混合物に７０℃以上の温度下で、不活性
ガスを流通させることを特徴とする酢酸パラジウムの調
製法を要旨とする。(Means for Solving the Problems) The present invention provides for preparing palladium cyanoacetate by heat-treating palladium powder in acetic acid in the presence of nitric acid. The gist of this invention is a method for preparing palladium acetate, which is characterized by passing an inert gas through the temperature.
本発明は、金属パラジウムを硝酸の存在下、酢酸中で加
熱処理することにより酢酸パラジウムを調製するもので
あるが、酢酸の使用量□と（ては、パラジウムに対して
３〜１００重量倍、好ましくは２０−！０重量倍の範囲
を挙げることができる。In the present invention, palladium acetate is prepared by heat-treating metallic palladium in acetic acid in the presence of nitric acid. Preferably, the range is 20-!0 times by weight.
一方、硝酸の存在量としては、酸化剤として必要な量が
あればよく、パラジウムに対して、０、ｇ ％ ／、！
ｒ ｍｏ’ｌｅ倍の範囲を挙げることができる。On the other hand, the amount of nitric acid present only needs to be the amount necessary as an oxidizing agent, which is 0, g % /,! with respect to palladium.
A range of r mo'le times may be mentioned.
硝酸の存在量があまり多いと加熱処理後においても、酸
化剤として使用され々かった硝酸が残存するので好まし
くない。If the amount of nitric acid present is too large, nitric acid that has not been used as an oxidizing agent will remain even after heat treatment, which is not preferable.
加熱処理の温度としては、り０℃以上、好ましくはｔθ
℃〜還流下全流下ることができる。The temperature of the heat treatment is 0°C or higher, preferably tθ
°C to reflux.
処理時間としては、ＩＯ分〜３時間、好ましくは３０分
〜コ時間の範囲を挙げることができ、あｔｂ短かいと十
分に酢酸パラジウムが生成せず、高純度のものが得られ
ない。この加熱処理によって、酢酸に分散していたパラ
ジウム金属が溶解し酢酸パラジウムとなる。The treatment time can be in the range of 10 minutes to 3 hours, preferably 30 minutes to 10 hours; if the atb is too short, palladium acetate will not be produced sufficiently and high purity will not be obtained. Through this heat treatment, palladium metal dispersed in acetic acid is dissolved to become palladium acetate.
不活性ガスとしては、窒素、アルゴン、ヘリウムなどが
挙げられ、なかでも窒素が望ましい。Examples of the inert gas include nitrogen, argon, helium, and the like, with nitrogen being particularly desirable.
不活性ガスの流通量としては、混合物／ｎ？に対して１
０〜３０−の範囲を挙げることができ、あまシ少ないと
、窒素含有量の少々い高純度の酢酸パラジウムが調製で
きず、逆に、多過ぎても効果に変シはない。また、流通
時間としては、温度及びガス量によシ異なるが、一般的
、には、１５分〜２時間程度を挙げることができる。The flow rate of inert gas is mixture/n? 1 for
A range of 0 to 30-30- is possible, and if the amount is too low, high-purity palladium acetate with a small nitrogen content cannot be prepared; on the other hand, if the amount is too high, the effect will not change. Further, although the flow time varies depending on the temperature and the amount of gas, it is generally about 15 minutes to 2 hours.
不活性ガスの流通方式としては、通常、混合物の下部よ
シネ活性ガスを供給し混合物をバブリングする方法が採
用されるが、さらにこの操作を攪拌下に行ってもよい。As for the inert gas distribution method, a method is usually adopted in which a cine active gas is supplied from the bottom of the mixture and the mixture is bubbled, but this operation may also be performed while stirring.
この不活性ガスの流通処理によシ加熱処理後の混合物中
に残存す（、る窒素含有物が大幅に減少する。This inert gas flow treatment significantly reduces the nitrogen-containing substances remaining in the mixture after the heat treatment.
上述の処理を終えた混合物は常法に従って蒸発乾固する
ことによシ酢酸パラジウムの結晶を回収することができ
る。また、場合により、混合物を例えば、３０℃Ｍ下ま
で冷却晶析することによシ酢酸バ２ジウムを結晶として
回収することができる。特に、冷却晶析による場合には
、極めて高純度の酢酸パラジウムが得られるので好まし
い。このようにして回収した結晶は必要に応じて、例え
ば、酢酸で洗浄し乾燥される。After the above-mentioned treatment, the mixture is evaporated to dryness according to a conventional method to recover palladium cyacetate crystals. Further, depending on the case, the mixture may be cooled and crystallized to, for example, 30° C.M, thereby recovering batidium cyanoacetate as crystals. In particular, cooling crystallization is preferable because palladium acetate of extremely high purity can be obtained. The crystals thus collected are washed with, for example, acetic acid and dried, if necessary.
、（効 果）
本発明によれば、硝酸根などの窒素分の含有量が少ない
高純度の酢酸パラジウムを簡単に得・ることかできる。(Effects) According to the present invention, high purity palladium acetate with a low content of nitrogen such as nitrate radicals can be easily obtained.
したがって本発明で調製される酢酸パラジウムを種々の
有機化学反応の触媒として適用した場合には、高い触媒
活性が得られるものである。Therefore, when palladium acetate prepared according to the present invention is applied as a catalyst for various organic chemical reactions, high catalytic activity can be obtained.
（実施例）
次に、本発明を実施例によシ更に詳細に説明するが、本
発明は以下の実施例に罎定されるものではない。(Examples) Next, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to the following Examples.
実施例／
温度調節器及び攪拌機を有する容器に、パラジウム粉末
＆、９と酢酸：ｔｋＯｗｔを仕込み、このスラリーに、
還流下（約１ｌｔｒｒ；）で、濃硝酸（！；、９．９
）、酢酸（３０ｙｄ）の混合液を３０分かけて滴下した
後、同温度で７時間加熱処理することによシ酢酸パラジ
ウムを調製した。次いでこの混合物を還流下（約ｌ／ざ
℃）の温度で第１表に示す量の窒素ガスを３０分かけて
系内に流通させた後混合物を、２０℃まで冷却し、次い
で、析出した酢酸パラジウムの結晶を濾過によシ回収し
た。得られた結晶を酢酸で懸濁洗浄した後、減圧下、７
００℃の温度で１０時間乾燥し酢酸パラジウムの結晶を
得た。Example / In a container equipped with a temperature controller and a stirrer, palladium powder & 9 and acetic acid: tkOwt were charged, and this slurry was
Under reflux (approximately 1 ltrr;), concentrate nitric acid (!;, 9.9
) and acetic acid (30 yd) was added dropwise over 30 minutes, followed by heat treatment at the same temperature for 7 hours to prepare palladium cyanoacetate. Next, nitrogen gas in the amount shown in Table 1 was passed through the system for 30 minutes at a temperature of reflux (approximately 1/°C), and the mixture was cooled to 20°C, followed by precipitation. Crystals of palladium acetate were collected by filtration. After suspending and washing the obtained crystals with acetic acid, the crystals were washed under reduced pressure for 7
It was dried at a temperature of 00°C for 10 hours to obtain crystals of palladium acetate.
この結晶につき結晶中に含有される窒素分を全窒素計〔
三菱化成工業■製、ＴＮ−０／型全窒素盆析装置〕によ
って測定したところ第１表に示す結果が得られた。For this crystal, measure the nitrogen content in the crystal using a total nitrogen meter [
The results shown in Table 1 were obtained using a TN-0/type total nitrogen basin analyzer manufactured by Mitsubishi Chemical Industries, Ltd.
Claims (1)
理することにより酢酸パラジウムを調製するに当り、加
熱処理後の混合物に７０℃以上の温度下で不活性ガスを
流通させることを特徴とする酢酸パラジウムの調製法。(1) In preparing palladium acetate by heat-treating palladium powder in acetic acid in the presence of nitric acid, an inert gas is passed through the heat-treated mixture at a temperature of 70°C or higher. Preparation method of palladium acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16976084A JPS6147440A (en) | 1984-08-14 | 1984-08-14 | Preparation of palladium acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16976084A JPS6147440A (en) | 1984-08-14 | 1984-08-14 | Preparation of palladium acetate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6147440A true JPS6147440A (en) | 1986-03-07 |
| JPH0522691B2 JPH0522691B2 (en) | 1993-03-30 |
Family
ID=15892341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16976084A Granted JPS6147440A (en) | 1984-08-14 | 1984-08-14 | Preparation of palladium acetate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6147440A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008031104A (en) * | 2006-07-28 | 2008-02-14 | Seiko Epson Corp | Method for producing copper formate, method for producing copper particle and method for producing wiring board |
| CN102320951A (en) * | 2011-06-13 | 2012-01-18 | 陕西瑞科新材料股份有限公司 | Method for preparing palladium acetate tripolymer |
| KR20170045202A (en) * | 2014-08-19 | 2017-04-26 | 헤레우스 도이칠란트 게엠베하 운트 코. 카게 | Method for preparing active palladium(0) powder |
-
1984
- 1984-08-14 JP JP16976084A patent/JPS6147440A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008031104A (en) * | 2006-07-28 | 2008-02-14 | Seiko Epson Corp | Method for producing copper formate, method for producing copper particle and method for producing wiring board |
| CN102320951A (en) * | 2011-06-13 | 2012-01-18 | 陕西瑞科新材料股份有限公司 | Method for preparing palladium acetate tripolymer |
| KR20170045202A (en) * | 2014-08-19 | 2017-04-26 | 헤레우스 도이칠란트 게엠베하 운트 코. 카게 | Method for preparing active palladium(0) powder |
| JP2017532435A (en) * | 2014-08-19 | 2017-11-02 | ヘレウス ドイチェラント ゲーエムベーハー ウント カンパニー カーゲー | Method for producing active palladium (0) powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0522691B2 (en) | 1993-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3584940B2 (en) | Ammoxidation catalyst composition | |
| CN108126723B (en) | Catalyst for preparing 3-cyanopyridine and preparation method thereof | |
| JPS63130144A (en) | Regeneration of oxidizing catalyst | |
| JPS63222011A (en) | Production of polycrystal silicon | |
| JPS6147440A (en) | Preparation of palladium acetate | |
| CA1162936A (en) | Oxydehydrogenation catalyst | |
| WO2019187840A1 (en) | Catalyst, method for manufacturing catalyst, method for manufacturing acrylonitrile | |
| JPH047037A (en) | Preparation of catalyst for manufacturing methacrylic acid | |
| CZ290055B6 (en) | Oxidation catalyst containing vanadium and phosphorus mixed oxides and process of its preparation | |
| JP3272689B2 (en) | Direct synthesis of methylchlorosilane | |
| JPH05177141A (en) | Preparation of methacrylic acid | |
| JPH03173840A (en) | Production of chlorotrifluoroethylene | |
| JP3410121B2 (en) | Ammonia purification method | |
| US4372934A (en) | Production of isocyanic acid | |
| JPH05221647A (en) | Method for oxidizing reduced polyoxoanionic compound | |
| JP2773920B2 (en) | Method for producing tetraammine palladium (II) chloride | |
| JPH05255190A (en) | Production of alpha-keto acid ester | |
| HU219197B (en) | Static condition process for the preparation of phosphorus/vanadium oxidation catalyst | |
| JPS5836910A (en) | Removal of organic impurities from phosphoric acid | |
| JPS5846444B2 (en) | Manufacturing method of hydroxylammonium salt | |
| JPH057216Y2 (en) | ||
| SU691396A1 (en) | Method of purifying phosphoric acid | |
| JP2000053611A (en) | Reduction of propionic acid in acrylic acid mixture gas | |
| JPS5936647A (en) | Preparation of oxamide | |
| JPH0214100B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |