Method for preparing palladium acetate compound

A technology of palladium acetate and compounds, which is applied in the field of preparation of palladium acetate compounds, can solve the problems of long time required and affecting the purity of palladium acetate crystals, etc., and achieve the effect of high yield

Active Publication Date: 2010-12-15
CHENZHOU GAOXIN MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A method for preparing trimeric palladium acetate reported by Jinchuan Group Co., Ltd. (publication number CN10127-9907), however, the addition of nitric acid will directly affect the purity of palladium ac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Accurately weigh 100g of palladium sponge, add aqua regia to dissolve it, and make it into 50g / L chloropalladium acid solution, add 1%-10% of , , One or two mixtures of aqueous solution and 5%–15% sodium hydroxide solution to adjust the pH value to 9, add an appropriate amount of 4:1 formaldehyde and hydrazine hydrate, and raise the temperature to 50 Restore the floating active palladium black sponge, filter and wash until there is no chloride ion; add the active palladium black sponge, glass beads and glacial acetic acid into the distillation flask, set up the reflux tube, and heat the reflux reaction in an infrared electric furnace, batch by batch Add 2–3 liters of glacial acetic acid, and the reaction is complete in about 30–120 minutes; filter while hot, transfer the filtrate to a rotary evaporator, control the negative pressure to 0.08MPa, and the evaporation temperature to 30–60 , evaporated to the precipitation of palladium acetate crystals, then cooling a...

Embodiment 2

[0021] Accurately weigh 100g of palladium sponge, add aqua regia to dissolve it, and make it into 50g / L chloropalladium acid solution, add 1%-10% of , , One or two mixtures of aqueous solution and 5%–15% sodium hydroxide solution to adjust the pH to 10, add an appropriate amount of 4:1 formaldehyde and hydrazine hydrate, and raise the temperature to 50 Restore the floating active palladium black sponge, filter and wash until there is no chloride ion; add the active palladium black sponge, glass beads and glacial acetic acid into the distillation flask, set up the reflux tube, and heat the reflux reaction in an infrared electric furnace, batch by batch Add 2–3 liters of glacial acetic acid, and the reaction is complete in about 30–120 minutes; filter while hot, transfer the filtrate to a rotary evaporator, control the negative pressure to 0.08MPa, and the evaporation temperature to 30–60 , evaporated to the precipitation of palladium acetate crystals, then cooled and cry...

Embodiment 3

[0023] Accurately weigh 100g of palladium sponge, add aqua regia to dissolve it, and make it into 50g / L chloropalladium acid solution, add 1%-10% of , , One or two mixtures of aqueous solution and 5%–15% sodium hydroxide solution to adjust the pH value to 9, add an appropriate amount of 5:1 formaldehyde and hydrazine hydrate, and raise the temperature to 50 Restore the floating active palladium black sponge, filter and wash until there is no chloride ion; add the active palladium black sponge, glass beads and glacial acetic acid into the distillation flask, set up the reflux tube, and heat the reflux reaction in an infrared electric furnace, batch by batch Add 2-3 liters of glacial acetic acid at a time, and the reaction is complete in about 30-120 minutes; filter the solution while it is hot and transfer it to a rotary evaporator, control the negative pressure to 0.08MPa, and the evaporation temperature to 30-60 , evaporated to the precipitation of palladium acetate cr...

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PUM

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Abstract

The invention discloses a method for preparing a palladium acetate compound, which comprises the following steps of: dissolving and reducing palladium sponge into floating active sponge palladium black; refluxing and completely reacting the active sponge palladium black with glacial acetic acid on the premise of not adding any aid; and concentrating, crystallizing and drying to prepare red-brown palladium acetate crystals. The key technology of the method is that: a foaming agent is added into a chloropalladite reduction system for reducing palladium ions into the floating active sponge palladium black, and the problem that the reaction between the active sponge palladium black and the glacial acetic acid is slow and incomplete is effectively solved on the premise of not adding any aid into a reaction system of the active sponge palladium black and the glacial acetic acid. The method for preparing the palladium acetate compound has the advantages of short reaction time, easy control, high stability, repeated use of glacial acetic acid, high product purity, yield of over 99 percent, and capacity of overcoming the defect of using nitric acid as an aid in the prior art.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to a preparation method of palladium acetate compound. Background technique [0002] Palladium acetate is a yellow-brown or red-brown uniform powder with a palladium content of 47.0%. It is stored in a sealed and dry environment at room temperature and is stable in the air. It is soluble in acetic acid, toluene, palladium acetate, chloroform, dichloromethane, acetone, acetonitrile and ether, and insoluble in water. Palladium acetate has a wide range of uses. It is a raw material for the synthesis of other palladium compounds, especially the precursor of metal palladium organic compounds; it is usually used as a catalyst precursor, and it is also an oxidation addition, cross-coupling, Suzuki coupling, cycloisomerization Catalysts for reactions such as oxidation and olefin aromatization; it can also be used in large quantities to prepare palladium plating bath solution. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41
Inventor 雷涤尘冯志杰杨拥军杨静
Owner CHENZHOU GAOXIN MATERIAL
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