Preparation method of palladium nitrate solution

A palladium nitrate solution technology, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problem of low chloride ion content in palladium nitrate solution, incomplete palladium dissolution, and technical problems The process is difficult to control and other problems, to achieve the effect of shortening the time for nitration, good product consistency, and easy operation

Inactive Publication Date: 2017-02-22
CHONGQING MATERIALS RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention overcomes the shortcomings of incomplete palladium dissolution and difficult control of the process in the prior art, and provides a method for preparing palladium nitrate solution with simple operation, short process flow, high

Method used

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Examples

Experimental program
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Effect test

Example Embodiment

[0018] Example 1:

[0019] Take 100 ml of concentrated nitric acid and 400 ml of concentrated hydrochloric acid, and mix them evenly to prepare solvent A.

[0020] 100g of metal palladium powder was weighed and placed in the reactor. The solvent A was added in batches to the reactor equipped with the metal palladium powder. The volume of the solvent A added for the first time was 200ml, and the volume of the solvent A added each time was 100ml. The timing of the addition was after a large amount of yellow gas was not emitted. After heating and dissolving, concentrate the dissolving solution, and when concentrating to 300ml, add concentrated hydrochloric acid to catch the nitrile until no yellow smoke emerges, that is, the nitrification is completed. The reactor was supplemented with deionized water and diluted to 1 L, so that the palladium concentration in the solution was 100 g / L. Add 200ml of reducing agent hydrazine hydrate under stirring state, and the reduction reaction...

Example Embodiment

[0021] Embodiment 2

[0022] Take 300 ml of concentrated nitric acid and 1200 ml of concentrated hydrochloric acid and mix them evenly to prepare solvent A.

[0023] 180 g of metal palladium powder was weighed and placed in the reactor. The solvent A was added in batches to the reactor equipped with the metal palladium powder. The volume of the solvent A added for the first time was 450ml, and the volume of the solvent A added each time was 350ml. The timing of the addition was after a large amount of yellow gas was not emitted. After heating and dissolving, concentrate the dissolving solution, and when concentrating to 600ml, add concentrated hydrochloric acid to catch the nitrile until no yellow smoke emerges, that is, the nitrification is completed. The reactor was supplemented with deionized water and diluted to 1 L, so that the palladium concentration in the solution was 180 g / L. Add 550 ml of reducing agent hydrazine hydrate under stirring, and the reduction reaction e...

Example Embodiment

[0024] Embodiment 3

[0025] Take 500 ml of concentrated nitric acid and 2000 ml of concentrated hydrochloric acid and mix them evenly to prepare solvent A.

[0026] 250 g of metal palladium powder was weighed and placed in the reactor. The solvent A was added in batches to the reactor equipped with the metal palladium powder. The volume of the solvent A added for the first time was 500ml, and the volume of the solvent A added each time was 500ml. The timing of the addition was after a large amount of yellow gas was not emitted. After heating and dissolving, concentrate the dissolving solution, and when concentrating to 750ml, add concentrated hydrochloric acid to catch the nitrile until no yellow smoke emerges, that is, the nitrification is completed. The reactor was supplemented with deionized water and diluted to 1 L, so that the palladium concentration in the solution was 250 g / L. Add 750ml of reducing agent hydrazine hydrate under stirring, and the reduction reaction em...

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Abstract

Provided is a preparation method of a palladium nitrate solution. The method comprises the steps that 1 part by volume of concentrated nitric acid and 4 parts by volume of concentrated hydrochloric acid are taken and mixed to prepare a solvent A which is used for dissolving metal palladium powder, after the metal palladium powder is completely dissolved, denitration is conducted, hydrazine hydrate is added for reduction, palladium black is obtained, the palladium black is put into a reactor, deionized water and concentrated nitric acid are added for dissolving, cooling is conducted to reach the room temperature, filtration is conducted, and the palladium nitrate solution is obtained. The preparation method is easy to implement, short in technological process, high in production efficiency and good in product consistency, the dissolving rate of metal palladium is high and exceeds 99.5%, the chlorine ion content of the obtained palladium nitrate solution is extremely low, and palladium nitrate catalyst poisoning can be effectively avoided.

Description

technical field [0001] The invention relates to the field of palladium nitrate fine chemical industry, in particular to a preparation method of a palladium nitrate solution. Background technique [0002] Since chloride ions can cause poisoning of the palladium nitrate catalyst and affect the catalytic effect, the chloride ion content in the palladium nitrate solution is required to be extremely low. [0003] In theory, high-purity palladium powder can be directly dissolved in nitric acid to prepare a palladium nitrate solution, and the chloride ion content in the prepared palladium nitrate solution is extremely low. However, due to differences in the control of process conditions when preparing palladium powder by different manufacturers, the particle size and dissolution activity of palladium powder are quite different, resulting in that these palladium powders are often slightly soluble in nitric acid. Therefore, nitric acid is directly dissolved in palladium powder with n...

Claims

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Application Information

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IPC IPC(8): C01G55/00B01J27/25
CPCC01G55/00B01J27/25
Inventor 罗凤兰万伟建罗维凡刘庆宾吴保安唐会毅陈小军翟步英
Owner CHONGQING MATERIALS RES INST
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