CN105621500B - A kind of method prepared by ammino palladium (II) of high activity dichloro four - Google Patents
A kind of method prepared by ammino palladium (II) of high activity dichloro four Download PDFInfo
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- CN105621500B CN105621500B CN201410615438.0A CN201410615438A CN105621500B CN 105621500 B CN105621500 B CN 105621500B CN 201410615438 A CN201410615438 A CN 201410615438A CN 105621500 B CN105621500 B CN 105621500B
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Abstract
A kind of preparation method of the ammino palladium (II) of high activity dichloro four, is characterized in：(1) prepared by the ammino palladium (II) of dichloro four, when using ammonia volume in Rotary Evaporators for 40.5ml-45.5ml/, 130-150r/min of speed of agitator, 80-110 DEG C of reaction temperature, 60-85min of reaction time, the ammino palladium (II) of preliminary product dichloro four is drawn, in case follow-up recrystallization processing；(2) dichloro four ammino palladium (II) product is recrystallized:The faint yellow thick ammino palladium (II) of dichloro four recrystallization that step (1) is obtained, to effectively improve product palladium content, its process conditions is：Using 60 DEG C-75 DEG C recrystallized to it, 15-30min of crystallization time.Present invention, avoiding conventional process flow length, the low drawback of product purity, it is low to solve product palladium content, the problems such as storage is difficult, and cost will be reduced a lot.
Description
Technical field
The present invention relates to a kind of preparation method of precious metal palladium compound, more particularly to a kind of ammino of high activity dichloro four
The preparation method of palladium (II), belongs to precious metals metallurgy field.
Background technology
The ammino palladium (II) of dichloro four is important palladium compound, is widely used in chemical catalysis and electroplating industry.It is a kind of
The main salt of novel electroplating, its electroplating efficiency is high, clean environment firendly, has been widely used in electronics industry plating palladium.In addition the ammonia of dichloro four
Close palladium (II) due to good water solubility, solution chemistry relatively stablize, can also as load type palladium catalyst presoma
Compound.There are proportioning Parameter uncertainties in existing ammino palladium (II) preparation flow of dichloro four, consersion unit is simple, obtained by primary crystallization
Containing largely free ammoniacal liquor in product, and there are Pd (NH in washing crystal repeatedly3)4Cl2A large amount of dissolvings, palladium recovery rate is not high.
The content of the invention
The problem of present invention aims at existing for existing ammino palladium (II) preparation method of dichloro four, exploitation is simple, high
The new method that effect, safety and ammino palladium (II) the product palladium content of dichloro four are high, activity is high.
The technical solution that the present invention is provided is：The preparation method of this ammino palladium (II) of high activity dichloro four, uses ammonia
Water and tetrachloro close palladium and are is prepared by the ammino palladium (II) of dichloro four, and recrystallization essence is carried out to dichloro four ammino palladium (II) product
System, is characterized in being made up of following steps.
(1) prepared by the ammino palladium (II) of dichloro four.
It is 40.5ml -45.5ml/ that ammonia volume is used in Rotary Evaporators（20ml H2PdCl4）When, speed of agitator
130-150r/min, reaction temperature is at 80-110 DEG C, and 60-85min of reaction time draws the ammino palladium of preliminary product dichloro four
(II), in case follow-up recrystallization processing.
(2) dichloro four ammino palladium (II) product is recrystallized.
The faint yellow thick ammino palladium (II) of dichloro four recrystallization that step (1) is obtained, to effectively improve product palladium content, its
Process conditions are：Using 60 DEG C-75 DEG C recrystallized to it, 15-30min of crystallization time.
When prepared by step (1), optimum process condition is：The 20 mL H in Rotary Evaporators2PdCl4Correspondence ammonia volume
42.5 mL, under 130 r/min stirrings, react 80 min in 85 DEG C, draw the ammino palladium (II) of preliminary product dichloro four, in case
Follow-up recrystallization processing.Following react occurs in system.
2H2PdCl4+4NH3H2O→Pd(NH3)4·PdCl4↓+4HCl+4H2O。
Pd(NH3)4·PdCl4+4 NH3H2O→2Pd(NH3)4Cl2+4H2O。
During step (2) processing, experiment shows that recrystallization processing dichloro four ammino palladium (II) product can effectively improve product palladium
Content, optimum process condition is：The ammino palladium (II) of product dichloro four is crystallized into 25 min at 70 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows.
1. proposing brand-new preparation system, ammoniacal liquor batch addition is realized, reaction stirring evenly, accurately, and makes reaction institute
Byproduct hydrochloric acid is obtained to be recycled.Whole production procedure is simple, cleanliness without any pollution.
Technological gap is filled up 2. providing and accurately preparing proportioning parameter.
3. recrystallizing the determination of product condition, palladium recovery rate is substantially increased, contains product dichloro four ammino palladium (II) palladium
Amount reaches 43.3%.
Specific embodiment
Embodiment 1.
Take 20 mL H2PdCl4, add 42.5ml ammoniacal liquor（28%）, in 85 DEG C of temperature in reaction system, the reaction time
80min, system speed of agitator 130r/min.Material is taken out, the ammino palladium (II) of product dichloro four is crystallized 25 at 70 DEG C
min.Weight is weighed, and is chemically examined.
As a result：
Dichloro four ammino palladium (II) quality：12.21g
Dichloro four ammino palladium (II) purity：99.35%
Dichloro four ammino palladium (II) palladium content：43.3 %.
Embodiment 2.
Take 20 mL H2PdCl4, add 40.5ml ammoniacal liquor（28%）, in 90 DEG C of temperature in reaction system, the reaction time
60min, system speed of agitator 150r/min.Material is taken out, the ammino palladium (II) of product dichloro four is crystallized 15 at 60 DEG C
min.Weight is weighed, and is chemically examined.
As a result：
Dichloro four ammino palladium (II) quality：11.98g
Dichloro four ammino palladium (II) purity：99.23%
Dichloro four ammino palladium (II) palladium content：43.1%.
Embodiment 3.
Take 20 mL H2PdCl4, add 43.5ml ammoniacal liquor（28%）, in 95 DEG C of temperature in reaction system, the reaction time
70min, system speed of agitator 140r/min.Material is taken out, the ammino palladium (II) of product dichloro four is crystallized 30 at 75 DEG C
min.Weight is weighed, and is chemically examined.
As a result：
Dichloro four ammino palladium (II) quality：12.09g
Dichloro four ammino palladium (II) purity：99.31%
Dichloro four ammino palladium (II) palladium content：42.9%.
The present invention prepares ammino palladium (II) product of high activity dichloro four, it is to avoid conventional process flow length, product purity are low
The problems such as；Solve product palladium content low, store the drawbacks such as difficulty, and cost will be reduced a lot.
Claims (1)
1. a kind of method prepared by ammino palladium (II) of high activity dichloro four, it is characterised in that including the ammino palladium (II) of dichloro four system
Standby, dichloro four ammino palladium (II) product recrystallizes two steps, wherein：
(1) prepared by the ammino palladium (II) of dichloro four:
The 20 mL H in Rotary Evaporators2PdCl4The correspondence mL of ammonia volume 42.5 is anti-in 85 DEG C under 130 r/min stirrings
80 min are answered, the ammino palladium (II) of preliminary product dichloro four is drawn, in case follow-up recrystallization processing;
(2) dichloro four ammino palladium (II) product is recrystallized:
The ammino palladium (II) of faint yellow preliminary product dichloro four recrystallization that step (1) is obtained, to effectively improve product palladium content,
Its process conditions is：It is recrystallized using 75 DEG C of temperature, crystallization time 25min.
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| CN102616869A (en) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | Tetrammine palladium sulphate synthesis method |
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Address after: 110141 No. 7, No. 6, No. seven road, Shenyang economic and Technological Development Zone, Shenyang, Liaoning. Patentee after: Shenyang Nonferrous Metal Research Institute Co., Ltd. Address before: 110141 No. 7, No. 6, No. seven road, Shenyang economic and Technological Development Zone, Shenyang, Liaoning. Patentee before: Shenyang Research Institute of Nonferrous Metals |
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