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Production method of tetraamminepalladium sulfate

A kind of technology of tetrahydropalladium sulfate, production method, applied in chemical instrument and method, preparation of ruthenium/rhodium/palladium/osmium/iridium/platinum compound, ruthenium/rhodium/palladium/osmium/iridium/platinum compound etc. direction, can Solve the problems of difficult control of product yield and quality, long process flow, excessive sulfuric acid, etc., to achieve the effect of high conversion rate, simple process and high product purity

Pending Publication Date: 2017-09-19
LESHAN DONGCHEN ADVANCED MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process, a large amount of sulfuric acid needs to be used to drive away nitric acid. The excess of sulfuric acid is large, and the by-products increase. In addition, during the complexation process, a large amount of ammonium sulfate is produced, which is mixed with tetraammonia palladium sulfate. An additional product separation process is required, and the process flow is long. Product yield and quality are more difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A kind of production method of palladium tetraammine sulfate, the steps are as follows:

[0017] (1) Complexation of ammonia water: Stir and heat 25kg ammonia water to 45°C, then add 8kg palladium dichloride, stir to dissolve, then filter out undissolved particles to obtain a clear solution; then continue to heat up to 80°C, stir and concentrate to crystal Precipitate, then stop heating, cool to room temperature, and precipitate a large amount of solid crystals; dry the solid crystals to remove ammonia, the drying temperature is 100 ° C, and the drying time is 5 hours;

[0018] (2) Ion exchange: Dissolve the crystalline solid obtained in step (1) in 500kg of water, then use D371 anion exchange resin to carry out ion exchange, check whether Cl-ions remain in the exchange tail liquid with silver nitrate solution, and exchange repeatedly until detection Does not produce Cl- ions;

[0019] (3) Sulfuric acid neutralization: in step (2) through ion-exchanged solution, adding...

Embodiment 2

[0022] A kind of production method of palladium tetraammine sulfate, the steps are as follows:

[0023] (1) Complexation of ammonia water: Stir and heat 35kg ammonia water to 50°C, then add 12kg palladium dichloride, stir to dissolve, then filter out undissolved particles to obtain a clear solution; then continue to heat up to 80-90°C, stir and concentrate Until the crystals are precipitated, then stop heating, cool to room temperature, and precipitate a large amount of solid crystals; dry the solid crystals to remove ammonia, and the drying temperature is 105°C;

[0024] (2) Ion exchange: Dissolve the crystalline solid obtained in step (1) in 800kg of water, then carry out ion exchange with D382 anion exchange resin, check whether Cl-ions remain in the exchange tail liquid with silver nitrate solution, exchange repeatedly until detection Does not produce Cl- ions;

[0025] (3) Sulfuric acid neutralization: in step (2) through ion-exchanged solution, adding volume concentrati...

Embodiment 3

[0028] A kind of production method of palladium tetraammine sulfate, the steps are as follows:

[0029] (1) Complexation of ammonia water: Stir and heat 30kg ammonia water to 47.5°C, then add 10kg palladium dichloride, stir to dissolve, then filter out undissolved particles to obtain a clear solution; then continue to heat up to 85°C, stir and concentrate to crystal Precipitate, then stop heating, cool to room temperature, and precipitate a large amount of solid crystals; dry the solid crystals to remove ammonia, and the drying temperature is 102.5°C;

[0030] (2) Ion exchange: the crystalline solid that step (1) obtains is dissolved in 650kg water, carries out ion exchange with anion exchange resin then, checks whether remaining Cl-ion remains in the exchange tail liquid with silver nitrate solution, exchanges repeatedly, until detecting no Out of Cl- ions;

[0031] (3) Sulfuric acid neutralization: in step (2) through ion-exchanged solution, adding volume concentration is 5...

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Abstract

The invention discloses a production method of tetraammonia palladium sulfate, which comprises the steps of ammonia water complexation, ion exchange, sulfuric acid neutralization, recrystallization and purification. The synthesis method of the invention has simple process, few by-products, The product has high purity and high conversion rate, and the present invention adds a drying step in the complexation of ammonia water, so that the residual ammonia water on the solid surface is avoided from participating in the next reaction step, which affects the purity of tetraammonia palladium sulfate, so that tetraammine palladium sulfate The purity has been further improved.

Description

technical field [0001] The present invention relates to chemical industry field, relate to a kind of production method of palladium tetraammine sulfate more specifically. Background technique [0002] Tetraammonia palladium sulfate is a new type of electroplating product, which is used for palladium plating in the electronics industry. It is mainly used for coating computer motherboards and network plugs, and manufacturing automotive catalytic crackers. Due to its high electroplating efficiency, halogen-free, clean and environmentally friendly, it can replace traditional halogen-containing electroplating solutions. At present, there is no tetraammine palladium sulfate synthesis process introduction in domestic public information, and U.S. Patent [US 6346222B1] reports using sulfuric acid to drive away the nitric acid in the palladium nitrate solution, obtains palladium sulfate solution, and then obtains tetraammine palladium sulfate with ammonia water complexation. In the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00C25D3/50
CPCC01G55/002C01G55/001C01P2004/10C01P2006/60C01P2006/80C25D3/50
Inventor 肖兴才车兴玉
Owner LESHAN DONGCHEN ADVANCED MATERIAL
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