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Preparation method of palladium (II) bis (oxalate) hydrate acid

A hydrated dioxalic acid and bisoxalic acid technology, which is applied in carboxylate preparation, organic chemistry, etc., can solve problems such as the preparation method of hydrated bisoxalate palladium, and achieve the effects of easy control, reduced production cost, and high product purity

Pending Publication Date: 2022-07-22
HOOTECH
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Problems solved by technology

At present, there are no bibliographical reports on the preparation method of hydrated bisoxalate palladium (II) acid

Method used

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Embodiment 1

[0020] A preparation method of hydrated bis-oxalate palladium (II) acid, comprising the following steps:

[0021] (1) Weigh 20.0g of pure palladium powder into a clean beaker, add 20mL of pure water, 80mL of analytically pure hydrochloric acid, then slowly drip analytically pure nitric acid until the palladium powder is completely dissolved, concentrate after dissolving and use hydrochloric acid to purify the nitric acid , then diluted, filtered, with pure water, the solution was adjusted to a 5% chloropalladous acid solution with a palladium content;

[0022] (2) The obtained chloropalladous acid solution was slowly added to 380 g of 10% analytically pure sodium hydroxide solution under stirring, and slowly heated to 80° C., stirred and refluxed for 6 h and left to stand, cooled and filtered to obtain a tetrahydroxyl group sodium palladium;

[0023] (3) add acetate buffer solution to sodium tetrahydroxypalladate, adjust the pH of the solution to be 6~8, then slowly add 68g o...

Embodiment 2

[0027] A preparation method of hydrated bis-oxalate palladium (II) acid, comprising the following steps:

[0028] (1) Weigh 20.0g of pure palladium powder into a clean beaker, add 20mL of pure water, 80mL of analytically pure hydrochloric acid, then slowly drip analytically pure nitric acid until the palladium powder is completely dissolved, concentrate after dissolving and use hydrochloric acid to purify the nitric acid , then diluted, filtered, and the solution was adjusted to a chloropalladous acid solution with a palladium content of 10% with pure water;

[0029] (2) The obtained chloropalladous acid solution was slowly added to 225g of 20% analytically pure sodium hydroxide solution under stirring, and slowly heated to 90°C, stirred and refluxed for 8h and then left to stand for 0.5h, and filtered to obtain tetrahydroxyl sodium palladium;

[0030] (3) add acetate buffer solution to sodium tetrahydroxypalladate, adjust the pH of the solution to be 6~8, then slowly add 102...

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Abstract

The preparation method comprises the following steps: dissolving palladium powder by using aqua regia, removing nitrate to obtain a chloropalladite solution, and converting the chloropalladite into tetrahydroxy sodium palladate by using sodium hydroxide; the method comprises the following steps: reacting sodium tetrahydroxy palladate with oxalic acid to obtain a hydrate bis (oxalate) palladic acid precipitate, and filtering, washing and drying to obtain hydrate bis (oxalate) palladic acid (II) with the purity of more than or equal to 99.95%. The initial raw materials are common and easy to obtain, other auxiliary materials are low in price, and the production cost can be reduced; in addition, the method not only avoids the residues of chloride ions and nitrate ions, but also reduces the inclusion residues of insoluble substances in the product. The method is carried out at normal pressure and low temperature, and is simple in process, easy to control and high in reaction yield (gt; the product purity is high (greater than or equal to 99.95%), and the method is suitable for batch and industrial production of the hydrated palladium bis (oxalate) (II) acid.

Description

[0001] technical field [0002] The invention belongs to the field of fine chemical industry, and in particular relates to a preparation method of hydrated bis-oxalate palladium (II) acid. Background technique [0003] Hydrated bis-oxalate palladium(II) acid compounds are an important class of palladium compounds, which are mainly used to prepare precursor compounds of supported catalysts. Due to its good water solubility, relatively stable solution chemical properties, and can directly obtain metal palladium when thermally decomposed, free of halogen, nitrate and ammonia, clean and environmentally friendly, it can be used as a starting material for the synthesis of other palladium compounds, and as a carrier for palladium The application of catalyst precursors has also received more and more attention. At present, there is no literature report on the preparation method of hydrated bis-oxalate palladium (II) acid. SUMMARY OF THE INVENTION [0004] The object of the present...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C55/07
CPCC07C51/418C07C55/07
Inventor 夏军李富荣刘芳奚红杰索永喜
Owner HOOTECH
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