Method of preparing palladium acetylacetonate

A technology of palladium acetylacetonate and acetylacetone, which is applied in the field of preparation of palladium acetylacetonate, can solve the problems of harsh reaction conditions and low yield of palladium acetylacetonate, and achieve the effect of mild reaction conditions and simple process

Inactive Publication Date: 2007-09-12
BEIJING UNIV OF CHEM TECH
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  • Abstract
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AI Technical Summary

Problems solved by technology

The yield of palladium acetylacetonate prepared by this method is low, only 95%, and the prep...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Step A: 5.84g (0.1mole) NaCl, 26.64g (0.1mole) Pd(NO 3 ) 2 2H 2 O and 180g (10mole) of deionized water were added into a 2000ml three-necked flask, stirred and dissolved at a temperature of 80°C, and the brown transparent solution was obtained and allowed to cool down to room temperature.

[0014] Step B: Weigh 16.83g (0.3 mole) KOH and dissolve it in 108g (6 mole) deionized water to prepare an alkaline solution.

[0015] Step C: Slowly add the solution obtained in step B to the solution obtained in step A under stirring at room temperature, and stop the dropwise addition when the pH of the solution is 8. At this time, a brown precipitate is formed in the three-neck flask. After continuing to stir and react for 1 hour, 40.02 g of acetylacetone (0.4 mole) was added into the three-necked flask, and the temperature was raised to 70° C. and stirred for 8 hours. Wash with deionized water 8 times after the reaction, and the consumption of each deionized water is 300g. The...

Embodiment 2

[0018] Step A: 14.85g (0.2mole) KCl, 26.64g (0.1mole) Pd (NO 3 ) 2 2H 2 O and 270g (15mole) of deionized water were added into a 2000ml three-neck flask, stirred and dissolved at a temperature of 70°C, and a brown transparent solution was obtained and allowed to cool down to room temperature.

[0019] Step B: Dissolve 8.00 g (0.2 mole) of NaOH in 90 g (5 mole) of deionized water to form an alkaline solution.

[0020] Step C: Slowly add the solution obtained in step B to the solution obtained in step A under stirring at room temperature, and stop the dropwise addition when the pH of the solution is 9. At this time, a brown precipitate is formed in the three-neck flask. After continuing to stir and react for 1 hour, 30.01 g of acetylacetone (0.3 mole) was added into the three-necked flask, and the temperature was raised to 70° C. and stirred for 12 hours. Wash with deionized water 8 times after the reaction, and the consumption of each deionized water is 300g. The washed pre...

Embodiment 3

[0023] Step A: 17.52g (0.3mole) NaCl, 17.74g (0.1mole) PdCl 2 and 360g (20mole) of deionized water were added into a 2000ml three-neck flask, stirred and dissolved at a temperature of 70°C, and the brown transparent solution was obtained, and allowed to cool down to room temperature.

[0024] Step B: Dissolve 11.22g (0.2 mole) of KOH in 108g (6 mole) of deionized water to form an alkaline solution.

[0025] Step C: Slowly add the solution obtained in step B to the solution obtained in step A under stirring at room temperature. After the addition, the pH of the solution is 7, and a brown precipitate is formed in the three-neck flask. After continuing to stir and react for 1 hour, 30.02 g (0.3 mole) of acetylacetone was added into the three-necked flask, and the temperature was raised to 40° C. and stirred for 12 hours. Wash with deionized water 8 times after the reaction, and the consumption of each deionized water is 400g. The washed precipitate was dried at 80°C for 24 hour...

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Abstract

This invention provides a method for preparing Pd acetylacetone, which solves dissoluble K-salt or Na-salt and Pd salt in deionized water under warm temperature then converts the Pd salt into Pd(OH)2 under the action of alkali then to add acetylacetone in a reaction mixture with Pd(OH)2, in which, since neutralization reaction occurs to the alpha active H atoms in the molecules and Pd(OH)2, Pd acetylacetone products are got.

Description

Technical field: [0001] The invention relates to a preparation method of palladium acetylacetonate. technical background: [0002] Palladium acetylacetonate is a precious metal organic compound obtained by synthesis, in addition to metal palladium, palladium oxide, palladium hydroxide and palladium inorganic salts. Palladium acetylacetonate is easily soluble in a variety of organic solvents and has high-temperature sublimation properties. It is an ideal precursor for the preparation of low-dimensional palladium metal materials by chemical vapor deposition (CVD) technology. Metal palladium has very high activity to hydrogenation and dehydrogenation chemical reactions. Studies have shown that dissolving palladium acetylacetonate in an appropriate organic solvent to prepare a solution impregnated with a porous carrier can prepare a supported catalyst in which Pd is uniformly dispersed in the carrier. Compared with the catalyst prepared by the inorganic compound precursor of pa...

Claims

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Application Information

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IPC IPC(8): C07C49/14C07C49/92C07C45/77C07F15/00
Inventor 李殿卿林彦军徐向宇刘鹏程
Owner BEIJING UNIV OF CHEM TECH
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