Refining method capable of realizing mass production of palladium tetramine sulfate

A technology of tetraammonium palladium sulfate and a refining method, which is applied in the refining field that can mass-produce tetraammonium palladium sulfate, can solve problems such as affecting the quality of tetraammonium palladium sulfate, poor water solubility of silver sulfate, complicated exchange process, etc., and achieves low cost , The effect of high product yield and high product purity

Active Publication Date: 2019-11-22
SINO PLATINUM METALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the resin activation and exchange process is cumbersome, and there is inevitably residual palladium on the resin, the cost of the whole process is high and the yield is low
CN108946829A adopts the electrodialysis method, and needs to build an electrodialysis device, which is costly and requires precision, which is not conducive to industrialized production operations
CN102616869B adopts tetraammine palladium dichloride and silver sulfate quantitative reaction to generate tetraammine palladium sulfate, and the reaction principle is to generate tetraammine palladium sulfate by producing volatile gas HCl, but silver sulfate water solubility is bad and cost is high, and operation is difficult to realize, silver Ions affect the mass of tetraammine palladium sulfate
CN105836814A adopts the same principle as CN102616869B, replacing silver sulfate with sulfuric acid, and the process of making strong acid from strong acid is more difficult to realize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 20L glass reactor, add 17.5L of ammonia water, under stirring, add 3700.00g of palladium sulfate solid, heat to 60°C, keep for 2h, filter, concentrate to a volume of 10L, drop to room temperature, then add 1L of ethanol, continuously A white solid was precipitated, filtered, baked at 50°C for 5 hours, and then baked at 90°C for 3 hours to obtain 4091.81g of tetraammine palladium sulfate with a yield of 98.68%.

[0014] Structural characterization: (1) Elemental analysis: measured values ​​H 4.41%, N 20.62%, Pd 39.32% (theoretical values ​​H 4.44%, N 20.69%, Pd 39.35%).

[0015] (2)IR(cm -1 , KBr): 3240, 3150 [s, v(NH 3 )],1621[m,δ as (HNH)], 1299 [s, δ s (HNH)], 1112, 617 [vs, v(SO 4 )], 488 [w, v(Pd-N)].

Embodiment 2

[0017] In a 50L glass reactor, add 35L of ammonia water, under stirring, add 7400.00g of palladium sulfate solid, heat to 60°C, keep for 2h, filter, concentrate to a volume of 20L, drop to room temperature, then add 2L of ethanol, and continue to precipitate The white solid was filtered, baked at 50°C for 5 hours, and then baked at 90°C for 3 hours to obtain 8189.23g of tetraammine palladium sulfate with a yield of 98.75%.

[0018] Structural characterization: (1) Elemental analysis: measured values ​​H 4.42%, N 20.65%, Pd 39.33% (theoretical values ​​H 4.44%, N 20.69%, Pd 39.35%).

[0019] (2)IR(cm -1 , KBr): 3241, 3150 [s, v(NH 3 )],1622[m,δ as (HNH)], 1298 [s, δ s (HNH)], 1112, 618 [vs, v(SO 4 )], 487 [w, v(Pd-N)].

Embodiment 3

[0021] In a 100L glass reactor, add 70L of ammonia water, under stirring, add 14.80kg of palladium sulfate solid, heat to 60°C, keep for 2h, filter, concentrate to a volume of 40L, drop to room temperature, then add 4L of ethanol, and continue to precipitate The white solid was filtered, baked at 50°C for 5 hours, and then baked at 90°C for 3 hours to obtain 16.39kg of tetraammine palladium sulfate with a yield of 98.79%.

[0022] Structural characterization: (1) Elemental analysis: measured values ​​H 4.40%, N 20.63%, Pd 39.31% (theoretical values ​​H 4.44%, N 20.69%, Pd 39.35%).

[0023] (2)IR(cm -1 , KBr): 3242, 3151 [s, v(NH 3 )],1621[m,δ as (HNH)], 1300[s, δ s (HNH)], 1118, 617 [vs, v(SO 4 )], 489 [w, v(Pd-N)].

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PUM

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Abstract

The invention discloses a refining method capable of realizing mass production of palladium tetramine sulfate. The method comprises the following specific steps: adding palladium sulfate solid into acertain amount of ammonia water, filtering after reaction, concentrating mother liquor to 1 / 2 of the original volume, cooling to room temperature, adding a certain amount of alcohol or ketone reagent,separating out a large amount of white solid, filtering, drying the solid for 5 hours at 50 DEG C and then drying for 3 hours at 90 DEG C by using a blast drying oven to obtain apalladium tetramine sulfate refined product. The method has the advantages of simple operation conditions, low equipment requirements, high product yield (more than 98%), high product purity (more than 99.5%), and obviouseconomic and environmental protection benefits.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to a refining method capable of mass producing tetraammonia palladium sulfate. Background technique [0002] Tetraammonia palladium sulfate is a chlorine-free ammonia electroplating salt. It has high electroplating efficiency, is clean and environmentally friendly, and is free of chlorine and nitrate. It is widely used in the electroplating industry, especially for palladium plating in the electronics industry. The market demand is increasing. It replaces the traditional electroplating salt containing nitric acid and chlorine. [0003] US6346222B1 and CN103395847A only introduce the synthesis method of palladium tetraammonium sulfate, but do not report the refining method, and cannot produce high-yield and high-purity products on a large scale. Both CN107176625A and CN102786100B adopt anion exchange resin to synthesize palladium tetraammine sulfate. Du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
CPCC01G55/002C01P2002/82C01P2002/85
Inventor 张雄波侯文亮沈峰肖云左川侯文明罗媛刘益溪韩媛
Owner SINO PLATINUM METALS CO LTD
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