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Synthesis method of trans-dichlorodiammine palladium (II)

A technology of dichlorodiamine palladium and a synthesis method, applied in the field of inorganic compound synthesis, can solve the problems of low product purity, cumbersome process, environmental pollution and the like, and achieve the effects of improving reaction efficiency, simple preparation process and improving product purity

Active Publication Date: 2015-09-09
陕西煤业化工技术开发中心有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For this reason, the present invention provides a simple and easy-to-operate, one-step synthesis method in order to solve the problems of cumbersome process, long time consumption, low product purity and serious environmental pollution in the prior art. Synthetic method of trans-dichlorodiammine palladium (II) with high synthesis, high yield, high product purity, and environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve 1g of sodium tetrachloropalladate in 100ml of absolute ethanol, place it in an ultrasonic reactor and apply ultrasonic action, the ultrasonic frequency is 40KHz, the power is 800W, the ultrasonic time is 60min, and the temperature is 5°C. , high-purity ammonia gas enters the reaction system uniformly through the gas distributor at a flow rate of 2.5mL / min. The amount of ammonia gas introduced is 150.7mL. Then the reaction system is left to age for 5h, and then the precipitate is filtered out. Repeated washing with absolute ethanol and deionized water at a temperature of 5°C, and finally drying at a vacuum of 0.07MPa and 90°C for 6 hours to obtain a high-purity trans-dichlorodiammine palladium(II) product. The product yield measured by experiment is 99.80%, wherein the palladium content is 50.35%.

Embodiment 2

[0028] Dissolve 1g of sodium tetrachloropalladate in 100ml of absolute ethanol, place it in an ultrasonic reactor and apply ultrasonic action, the ultrasonic frequency is 25KHz, the power is 500W, the ultrasonic time is 150min, and the temperature is 10°C. , high-purity ammonia gas enters the reaction system uniformly through the gas distributor at a flow rate of 1mL / min. The amount of ammonia gas introduced is 150.7ml. Then the reaction system is left to age for 2h, and then the precipitate is filtered out. Repeated washing with absolute ethanol and deionized water at 10°C, and finally drying at 60°C for 5 hours at a vacuum of 0.1MPa to obtain a high-purity trans-dichlorodiammine palladium (II) product. The product yield measured by experiment is 99.64%, wherein the palladium content is 50.34%.

Embodiment 3

[0030] Dissolve 1g of sodium tetrachloropalladate in 100ml of absolute ethanol, place it in an ultrasonic reactor and apply ultrasonic action, the ultrasonic frequency is 60KHz, the power is 1200W, the ultrasonic time is 120min, and the temperature is 15°C. , high-purity ammonia gas enters the reaction system uniformly through the gas distributor at a flow rate of 1.25mL / min. The amount of ammonia gas introduced is 150.7ml, and then the reaction system is left to age for 8 hours, then the precipitate is filtered out, and the temperature Repeated washing with absolute ethanol and deionized water at 15°C, and finally drying at 120°C for 4 hours at a vacuum of 0.08MPa to obtain high-purity trans-dichlorodiammine palladium(II) product. The product yield measured by experiment is 99.45%, wherein the palladium content is 50.26%.

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PUM

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Abstract

The invention relates to the field of synthesis of inorganic compounds, in particular to a synthesis method of trans-Dichlorodiammine palladium (II). The method includes the following steps: dissolving a disodium tetrachloropalladate solution in anhydrous ethanol, and then introducing high-purity ammonia gas for reaction to generate trans-Dichlorodiammine palladium (II) through one step; leaving the solution system to stand after the reaction for aging, and then filtering; washing and drying the precipitate to obtain trans-Dichlorodiammine palladium (II). The synthesis method provided by the invention uses disodium tetrachloropalladate as a starting material and adopts a one-step synthesis method, so that the process is simple; high-purity ammonia gas is adopted, and precise control of the reaction system is achieved, so that the product purity is improved; an ultrasonic reactor is adopted, and the reaction efficiency is improved, so that the product yield reaches 99.5% or above; the product obtained through the reaction is uniform in particle size distribution, fine and loose in particles, and easy to wash and filter, so that the product purity is as high as 99.9% or above.

Description

technical field [0001] The invention relates to the field of inorganic compound synthesis, in particular to a synthesis method of trans-dichlorodiammine palladium (II). Background technique [0002] Trans-dichlorodiammine palladium(Ⅱ) (trans-Pd(NH 3 ) 2 Cl 2 ), is a yellow crystalline powder, stable in the air, insoluble in water; palladium content is about 50.40%. Trans-dichlorodiammine palladium (II) has very important uses in industry, and is mainly used in palladium plating in the electronics industry. It is used as a palladium source in electroplating solutions, and can also be used as a precursor compound for supported palladium catalysts. [0003] The conventional synthesis method of trans-dichlorodiammine palladium (II) is: dissolving palladium powder in aqua regia to generate tetrachloropalladium acid, and then generating trans-dichlorodiammine palladium (II) by dropwise adding ammonia water and hydrochloric acid. SD.Kirik (Structures and Isomerization in Diammi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 张蕾宋双田王振宇栗庆明祁敏吴玉秀赵国静
Owner 陕西煤业化工技术开发中心有限责任公司
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