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Preparation method for palladium acetylacetonate

A technology of palladium acetylacetonate and metal palladium, which is applied in the preparation of aldehyde/ketone chelates, organic chemistry, etc., can solve the problems of affecting the dissolution rate of palladium, increasing the preparation cost, and harsh reaction conditions, so as to shorten the preparation time and dissolve the speed Fast, gentle operating conditions

Active Publication Date: 2012-12-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN101033182A discloses a method for preparing palladium acetylacetonate with palladium salt as the starting material, dissolves soluble potassium salt or sodium salt and soluble palladium salt in deionized water, adjusts the pH value with a strong base, and then adds acetylacetone to obtain the product , although the method has mild preparation conditions and convenient operation, the added potassium salt or sodium salt increases the preparation cost
The yield of palladium acetylacetonate prepared by this method is low, only 95%, and the hydrogen peroxide of a large amount of heat needs to be used in the preparation process, and hydrogen peroxide is easy to decompose when heated, the higher the concentration, the faster the decomposition, and the hydrogen peroxide of low concentration has no effect on palladium. The dissolving ability is weak, which affects the dissolution rate of palladium, especially the metal palladium block, and the reaction conditions are relatively harsh

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 10 grams of sponge palladium powder with a purity >99.95wt%, put it into a 1-liter beaker, slowly add 30 grams of concentrated nitric acid with a weight concentration of 65% and 25 grams of hydrogen peroxide with a weight concentration of 30%, and put the solution on the electric heater Heat to 45°C, after complete dissolution, cool to room temperature, place in a 1000ml three-necked flask reaction device with reflux condenser to stir the reaction, then slowly add sodium hydroxide solution with a concentration of 3mol / L until the pH of the solution is 9 Stop adding, get brown precipitate, continue stirring for 1 hour, add 37.61g of acetylacetone, reflux and stir at 60°C for 8 hours, collect the yellow precipitate by filtration, wash with deionized water until neutral, and dry at 70°C for 9 hours, Product A was obtained, and determined by elemental analysis and mass spectrometry (MS), the compound was the target product palladium acetylacetonate.

Embodiment 2

[0022] Take 15 grams of sponge palladium powder with a purity >99.95wt%, put it into a 1-liter beaker, slowly add 60 grams of concentrated nitric acid with a weight concentration of 65% and 30 grams of hydrogen peroxide with a weight concentration of 30%, and put the solution on the electric heater Heat to 50°C, after complete dissolution, cool to room temperature, place in a 1000ml three-neck flask reaction device with reflux condenser to stir the reaction, then slowly add potassium hydroxide solution with a concentration of 4mol / L until the pH of the solution is 8 Stop adding, get a brown precipitate, continue to stir the reaction for 1.5 hours, add 42.31g of acetylacetone, reflux and stir at 65°C for 8 hours, collect the yellow precipitate by filtration, wash with deionized water until neutral, and dry at 80°C for 8 hours, Product B was obtained, and determined by elemental analysis and mass spectrometry (MS), the compound was the target product palladium acetylacetonate.

Embodiment 3

[0024] Take 10 grams of metal palladium blocks with a purity of >99.95wt%, put them into a 1-liter beaker, slowly add 70 grams of concentrated nitric acid with a weight concentration of 65% and 60 grams of hydrogen peroxide with a weight concentration of 30%, and heat the solution on an electric heater After completely dissolving at 55°C, cool to room temperature, place in a 1000ml three-neck flask reaction device with a reflux condenser and stir the reaction, then slowly add potassium hydroxide solution with a concentration of 5mol / L until the pH value of the solution is 9 and stop Added to obtain a brown precipitate, continue to stir the reaction for 2 hours, add 47.02g of acetylacetone, reflux and stir at 70°C for 8 hours, filter and collect the yellow precipitate, wash with deionized water until neutral, and dry at 80°C for 12 hours to obtain Product C, as determined by elemental analysis and mass spectrometry (MS), is the target product palladium acetylacetonate.

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Abstract

The present invention discloses a preparation method for palladium acetylacetonate. The preparation method comprises: adding high purity metal palladium or sponge palladium to a container; adding concentrated nitric acid and hydrogen peroxide; heating and dissolving; cooling to a room temperature; adding a strong alkali solution to adjust the pH value to 8-11; and adding excess acetylacetone to obtain the product palladium acetylacetonate. Compared with the preparation method in the prior art, the preparation method of the present invention has the following characteristics that: a palladium salt compound is not required to be adopted as a starting material so as to substantially reduce cost; when the high purity metal palladium or the sponge palladium is adopted as a starting material, concentrated nitric acid and hydrogen peroxide are added during the dissolution process to generate pernitric acid so as to enhance dissolution on palladium, accelerate reaction speed, reduce a use amount of hydrogen peroxide, and improve product yield and purity. In addition, the method of the present invention has characteristics of mild process conditions, simple steps and the like.

Description

technical field [0001] The invention relates to a preparation method of palladium acetylacetonate. Background technique [0002] Palladium acetylacetonate [Pd (acac) 2 ] is a yellow crystalline powder, which is a noble metal organic coordination compound, soluble in organic solvents such as benzene, chloroform, absolute ethanol, etc. , easy to decompose, easy to dissolve in a variety of organic solvents and other characteristics, it has become an ideal precursor. The palladium catalyst prepared by impregnating porous supports in palladium acetylacetonate dissolved in organic solvents has a much better metal dispersion than inorganic compounds made of palladium. The prepared palladium catalyst can be used to prepare palladium metal coatings, carrier catalysts, membrane catalysts, nanometer palladium and palladium alloys by CVD. It is also an important catalyst for homogeneous catalytic reactions and photocatalytic reactions. It has extensive applications in the fields of new...

Claims

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Application Information

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IPC IPC(8): C07C49/92C07C49/14C07C45/77
Inventor 宋丽芝乔凯王海波勾连科薛冬
Owner CHINA PETROLEUM & CHEM CORP
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