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
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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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