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A kind of preparation method of palladium acetate

A technology of palladium acetate and hydrochloric acid, which is applied in the field of organic catalysis and the preparation of precious metal catalysts for pharmaceutical synthesis, can solve the problems of unstable product quality, difficulty in complete reaction of palladium, and generation of nitrogen oxides, etc., to facilitate large-scale production and reduce environmental pollution , easy-to-control effects

Active Publication Date: 2019-08-13
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current preparation method is roughly that palladium metal is activated, or newly reduced activated palladium black, with nitric acid (or nitrogen oxides) as an auxiliary agent, reacts with glacial acetic acid to prepare palladium acetate, and the problem of this method is that palladium and acetic acid and nitric acid It is difficult to react completely, and the performance is more prominent in mass production. It needs repeated activation and dissolution, and the operation is complicated, and the introduction of nitric acid will cause nitrogen oxides in the process, which is not environmentally friendly and the product quality is unstable.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation process of present embodiment palladium acetate comprises the following steps:

[0019] Step 1. Dissolve 200g of metal palladium with hydrochloric acid and hydrogen peroxide, then adjust the pH of the solution to 8 with 2mol / L sodium hydroxide solution to obtain a suspension, and continue stirring for 1h to obtain a reaction solution; the mass concentration of the hydrochloric acid is 32%. , the consumption of the hydrochloric acid is 2 times of the mass of the metal palladium, the mass concentration of the hydrogen peroxide is 27.5%, the consumption of the hydrogen peroxide is 2 times of the mass of the metal palladium, and the temperature when dissolving the metal palladium is 80°C;

[0020] Step 2: Add 1720 mL of glacial acetic acid to the reaction solution in Step 1, heat to 65°C, stir for 5 hours, cool and filter, wash the filtered solid with water and dry to obtain 408.4 g of solid palladium acetate. After testing, this example The yield of prepare...

Embodiment 2

[0023] The preparation process of present embodiment palladium acetate comprises the following steps:

[0024] Step 1. Dissolve 200g of metal palladium with hydrochloric acid and hydrogen peroxide, then adjust the pH of the solution to 9.5 with 2mol / L sodium hydroxide solution to obtain a suspension, and continue stirring for 1h to obtain a reaction solution; the mass concentration of the hydrochloric acid is 32%. , the consumption of the hydrochloric acid is 2 times of the mass of the metal palladium, the mass concentration of the hydrogen peroxide is 27.5%, the consumption of the hydrogen peroxide is 2 times of the mass of the metal palladium, and the temperature when dissolving the metal palladium is 80°C;

[0025] Step 2: Add 1300 mL of glacial acetic acid to the reaction solution in Step 1, heat to 80°C, stir for 3 hours, cool and filter, wash the filtered solid with water and dry to obtain 413.7 g of solid palladium acetate. After testing, this example The yield of prepa...

Embodiment 3

[0028] The preparation process of present embodiment palladium acetate comprises the following steps:

[0029] Step 1. Dissolve 200g of palladium with hydrochloric acid and hydrogen peroxide, then adjust the pH of the solution to 10 with 3mol / L potassium hydroxide solution to obtain a suspension, and continue stirring for 1h to obtain a reaction solution; the mass concentration of the hydrochloric acid is 32%. The consumption of described hydrochloric acid is 2 times of the quality of metal palladium, the mass concentration of described hydrogen peroxide is 27.5%, the consumption of hydrogen peroxide is 2 times of the quality of metal palladium, and the temperature when dissolving metal palladium is 80 ℃;

[0030] Step 2: Add 640 mL of glacial acetic acid to the reaction solution in Step 1, heat to 50°C, stir for 6 hours, cool and filter, wash the filtered solid with water and dry to obtain 409.8 g of solid palladium acetate. After testing, this example The yield of prepared p...

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Abstract

The invention discloses a preparation method of palladium acetate. The method comprises the following steps: 1. Using metal palladium as a raw material, hydrochloric acid and hydrogen peroxide are used to dissolve metal palladium to obtain a solution, and then an alkali solution is used to adjust the pH of the solution to obtain a suspension After continuing to stir for 1 h, a reaction solution was obtained; 2. Add glacial acetic acid to the reaction solution, heat and stir for reaction, after the reaction was completed, cool and filter, wash the filtered solid with water and dry to obtain palladium acetate. The present invention breaks through the method in which nitric acid or nitrogen oxide compound must be used as an auxiliary agent to produce palladium acetate in the existing method, avoids pollution to the environment, has little environmental pollution, and the preparation method adopted is simple, easy to control and operate, and is convenient for large-scale production Production.

Description

technical field [0001] The invention belongs to the technical field of preparation of precious metal catalysts for organic catalysis and medical synthesis, and in particular relates to a preparation method of palladium acetate. Background technique [0002] Palladium acetate is a widely used catalyst, mainly used in reactions such as molecular rearrangement, cross-coupling, Suzuki coupling, addition, substitution and isomerization of unsaturated hydrocarbons, in cyclohexanone. Adipic acid and caprolactam are widely used in industry, and palladium acetate is a halogen-free catalyst, and is an important raw material for palladium aqueduct liquid and gas sensitive materials. The current preparation method is roughly that palladium metal is activated, or newly reduced activated palladium black, with nitric acid (or nitrogen oxides) as an auxiliary agent, reacts with glacial acetic acid to prepare palladium acetate, and the problem of this method is that palladium and acetic acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C53/10
CPCC07C51/412C07C51/41C07C53/10
Inventor 王昭文崔静潘丽娟曾利辉曾永康
Owner XIAN CATALYST NEW MATERIALS CO LTD
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