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One-step synthetic method of palladium tetraammine acetate dihydrate (II)

A technology of acetic acid dihydrate and palladium acetate, applied in the field of chemistry and chemical industry, can solve problems such as difficulty in mass production, difficult control of reaction end points, application limitations, etc., and achieves the effects of high reaction yield, simple operation, and high product purity.

Active Publication Date: 2013-12-18
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Similarly, this method has the problem that the reaction end point is difficult to control
In view of the problem that the above two conventional preparation methods are difficult to produce in batches, the application of tetraamminepalladium(II) acetate as a catalytic precursor is greatly limited, so the development of new efficient synthesis methods will be of great significance

Method used

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  • One-step synthetic method of palladium tetraammine acetate dihydrate (II)
  • One-step synthetic method of palladium tetraammine acetate dihydrate (II)
  • One-step synthetic method of palladium tetraammine acetate dihydrate (II)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1 Measure 500 mL of concentrated ammonia water, add 100.00 g (446.4 mmol) of palladium acetate solid in batches under stirring, after the addition is complete, stir at 40-50°C until the palladium acetate is completely dissolved to obtain a light yellow solution, filter to remove a small amount of insoluble The filtrate was concentrated under reduced pressure to 80-100mL, and then 5mL of concentrated ammonia water was added and stirred to obtain a light yellow tetraamminepalladium(II) acetate solution; the concentrated solution was added to 2000 mL of acetone under vigorous stirring, and the After stirring for 30 minutes, filter, wash the filter cake once with 50 mL of acetone, concentrate the filtrate again, reverse analysis with acetone, combine the obtained light yellow solids, and dry at 40-50°C for 3 hours to obtain 144.2 g of tetraamminepalladium(II) acetate Pale yellow solid, yield 98%.

[0013] Feature structure parameters:

[0014] Elemental analy...

Embodiment 2

[0018] Example 2 Measure 1500 mL of concentrated ammonia water, add 500.00 g (2.232 mol) of palladium acetate solid in batches under stirring, after the addition is complete, stir at 40-50°C until the palladium acetate is completely dissolved to obtain a light yellow solution, filter to remove a small amount of insoluble The filtrate was concentrated under reduced pressure to 150-200mL, then 5mL of concentrated ammonia water was added and stirred to obtain a light yellow tetraamminepalladium(II) acetate solution; the concentrated solution was added to 5L of acetone under vigorous stirring, and stirred at room temperature Filter after 30 minutes, wash the filter cake once with 100 mL of acetone, concentrate the filtrate again, reverse analysis with acetone, combine the obtained pale yellow solids, and dry at 40-50°C for 3 hours to obtain 721.21 grams of tetraammine palladium (II) acetate Yellow [Pd(NH 3 ) 4 ](CH 3 COO) 2 2H 2 O, yield 98%.

Embodiment 3

[0019] Example 3 The thermal decomposition behavior of tetraammine palladium acetate dihydrate in air was determined by thermogravimetric analysis (DTA / TG), and the gas phase products of thermal decomposition were determined by gas chromatography-mass spectrometry.

[0020] Table 1. The main products of pyrolysis of tetraamminepalladium acetate dihydrate at 270℃

[0021]

[0022] The thermal cracking reaction formula of tetraammine palladium acetate dihydrate is as follows:

[0023]

[0024] Such as figure 1 , it can be known from the DTA / TG diagram in air that [Pd(NH 3 ) 4 ](CH 3 COO) 2 2H 2 O starts endothermic weight loss at 85°C, and an endothermic peak appears at 111°C, and the weight loss is 5.6% at 85-128°C; for the removal of two crystal waters, and then intense endothermic weight loss, the endothermic peak appears at 205°C, The peak and valley of the weight loss curve is 275 ° C, and the weight loss is 58.8%, which is equivalent to losing four ammonia...

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Abstract

The invention relates to a new method of synthesizing palladium tetraammine acetate dihydrate (II). The synthetic method comprises the steps of: carrying out a one-step reaction between palladium acetate [Pd3(CH3COO)6] and ammonia water to generate palladium tetraammine acetate dihydrate, and then counter-precipitating by using acetone to obtain the product. The synthetic method is simple in reaction operation and high in reaction yield (greater than 98.0%); the purity of the product is high (greater than 99.0%); the synthetic method is suitable for industrial production.

Description

technical field [0001] The invention relates to a new method for synthesizing a water-soluble complex of divalent palladium, i.e. tetraammine palladium (II) acetate dihydrate, belonging to the field of chemistry and chemical engineering. Background technique [0002] The largest industrial use of metal palladium is as a catalyst, especially supported palladium catalysts such as Pd / C, Pd-Rh / Al 2 o 3 It has been widely used in the purification fields of fine chemicals and automobile exhaust[Blaser H.-U., Indolese A., Schnyder A. Supported palladium catalysts for fine chemicals synthesis. Journal of Molecular Catalysis A: Chemical, 2001, v. 173, p . 3 – 181]. At present, the main method of industrially producing supported palladium catalysts is the chemical impregnation method [Brunelle J.P. Preparation of catalysts by adsorption of metal complexes on mineral oxides. Pure Applied Chemistry, 1978, v. 50, p. 1211 – 1229]. It involves the use of palladium compounds (such as pal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
Inventor 余娟叶青松刘伟平陈家林常桥稳姜婧晏彩先
Owner KUNMING INST OF PRECIOUS METALS
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