CN105621500A - Method for preparing high-activity palladium(II) tetrammine chloride - Google Patents
Method for preparing high-activity palladium(II) tetrammine chloride Download PDFInfo
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- CN105621500A CN105621500A CN201410615438.0A CN201410615438A CN105621500A CN 105621500 A CN105621500 A CN 105621500A CN 201410615438 A CN201410615438 A CN 201410615438A CN 105621500 A CN105621500 A CN 105621500A
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Abstract
The invention relates to a method for preparing high-activity palladium (II) tetrammine chloride. The method is characterized in that 1) preparation of palladium(II) tetrammine chloride, when ammoniacal liquor amount used in a rotary evaporation instrument is 40.5 ml-45.5 ml, an agitation speed is 130-150 r/min, a reaction temperature is 80-110 DEG C, a reaction time is 60-85 min, and primary product palladium(II) tetrammine chloride can be obtained for subsequent recrystallization; and 2) recrystallization of palladium(II) tetrammine chloride: recrystallization of light yellow palladium(II) tetrammine chloride in the step 1) can be obtained, product palladium content can be effectively increased, the technical condition is characterized in that recrystallization is carried out at temperature of 60-75 DEG C, and a crystallization time is 15-30 min. The method can avoid disadvantages of long traditional process flow and low product purity, solves the problems of low product palladium content and difficult storage, and has advantage of cost reduction.
Description
Technical field
The preparation method that the present invention relates to a kind of precious metal palladium compound, the preparation method particularly relating to a kind of high activity dichloro four ammino palladium (II), belong to precious metals metallurgy field.
Background technology
Dichloro four ammino palladium (II) is important palladium compound, is widely used in chemical catalysis and electroplating industry. Being a kind of main salt of Novel electroplating, its electroplating efficiency is high, clean environment firendly, has been widely used in electron trade plating palladium. In addition dichloro four ammino palladium (II) due to good water solubility, solution chemistry relatively stable, it is also possible to as the precursor compound of load type palladium catalyst. There is proportioning Parameter uncertainties in existing dichloro four ammino palladium (II) preparation flow, consersion unit is simple, and containing a large amount of free ammonia in primary crystallization products obtained therefrom, and Pd (NH occurs in washing crystal repeatedly3)4Cl2A large amount of dissolvings, palladium recovery rate is not high.
Summary of the invention
Present invention aim at for existing dichloro four ammino palladium (II) preparation method Problems existing, develop simple, efficient, safety and dichloro four ammino palladium (II) product palladium content high new method high, active.
The technical solution that the present invention provides is: the preparation method of this high activity dichloro four ammino palladium (II), with ammonia and four chloro palladiums, dichloro four ammino palladium (II) is prepared, and dichloro four ammino palladium (II) product is carried out recrystallizing and refining, it is characterized in being made up of following steps.
(1) prepared by dichloro four ammino palladium (II).
Using ammonia volume in Rotary Evaporators is 40.5ml 45.5ml/(20mlH2PdCl4) time, speed of agitator 130 150r/min, reaction temperature at 80 110 DEG C, response time 60 85min, draw preliminary product dichloro four ammino palladium (II), process in order to follow-up recrystallization.
(2) dichloro four ammino palladium (II) product recrystallization.
Faint yellow thick dichloro four ammino palladium (II) recrystallization that step (1) is obtained, to be effectively improved product palladium content, its process conditions are: adopt 60 DEG C 75 DEG C it is carried out recrystallization, crystallization time 15 30min.
Time prepared by step (1), optimum process condition is: 20mLH in Rotary Evaporators2PdCl4Corresponding ammonia volume 42.5mL, under 130r/min stirs, reacts 80min in 85 DEG C, draws preliminary product dichloro four ammino palladium (II), process in order to follow-up recrystallization. Following reaction is there is in system.
2H2PdCl4+4NH3H2O��Pd(NH3)4��PdCl4��+4HCl+4H2O��
Pd(NH3)4��PdCl4+4NH3H2O��2Pd(NH3)4Cl2+4H2O��
When step (2) processes, experiments show that recrystallization processes dichloro four ammino palladium (II) product and can be effectively improved product palladium content, optimum process condition is: by product dichloro four ammino palladium (II) crystallization 25min at 70 DEG C.
Compared with prior art, the invention has the beneficial effects as follows.
1. proposing brand-new preparation system, it is achieved ammonia batch adds, reaction stirring evenly, accurately, and makes reaction gained byproduct hydrochloric acid be recycled. Whole production procedure is simple, cleanliness without any pollution.
2. provide and prepare proportioning parameter accurately and fill up technological gap.
3. the determination of recrystallization product condition, substantially increases palladium recovery rate, makes product dichloro four ammino palladium (II) palladium content reach 43.3%.
Specific embodiments
Embodiment 1.
Take 20mLH2PdCl4, add 42.5ml ammonia (28%), in temperature 85 DEG C in reaction system, response time 80min, system speed of agitator 130r/min. Material is taken out, by product dichloro four ammino palladium (II) crystallization 25min at 70 DEG C. Weigh weight, and chemically examine.
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 20mLH2PdCl4, add 40.5ml ammonia (28%), in temperature 90 DEG C in reaction system, response time 60min, system speed of agitator 150r/min. Material is taken out, by product dichloro four ammino palladium (II) crystallization 15min at 60 DEG C. Weigh weight, and chemically examine.
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 20mLH2PdCl4, add 43.5ml ammonia (28%), in temperature 95 DEG C in reaction system, response time 70min, system speed of agitator 140r/min. Material is taken out, by product dichloro four ammino palladium (II) crystallization 30min at 75 DEG C. Weigh weight, and chemically examine.
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 high activity dichloro four ammino palladium (II) product, it is to avoid the problem such as conventional process flow length, product purity are low; Solve product palladium content low, store the drawbacks such as difficulty, and cost to reduce a lot.
Claims (3)
1. the method that prepared by a high activity dichloro four ammino palladium (II), it is characterised in that include dichloro four ammino palladium (II) prepare, dichloro four two steps of ammino palladium (II) product recrystallization, wherein:
(1) prepared by dichloro four ammino palladium (II):
Using ammonia volume in Rotary Evaporators is 40.5ml 45.5ml/(20mlH2PdCl4) time, speed of agitator 130 150r/min, reaction temperature at 80 110 DEG C, response time 60 85min, draw preliminary product dichloro four ammino palladium (II), process in order to follow-up recrystallization;
(2) dichloro four ammino palladium (II) product recrystallization:
Faint yellow thick dichloro four ammino palladium (II) recrystallization that step (1) is obtained, to be effectively improved product palladium content, its process conditions are: adopt 60 DEG C 75 DEG C it is carried out recrystallization, crystallization time 15 30min.
2. the method that prepared by high activity dichloro four ammino palladium (II) according to claim 1, it is characterised in that optimum process condition time prepared by step (1) is: 20mLH in Rotary Evaporators2PdCl4Corresponding ammonia volume 42.5mL, under 130r/min stirs, reacts 80min in 85 DEG C, draws preliminary product dichloro four ammino palladium (II), process in order to follow-up recrystallization.
3. the method that prepared by high activity dichloro four ammino palladium (II) according to claim 1, it is characterised in that optimum process condition time prepared by step (2) is: by product dichloro four ammino palladium (II) crystallization 25min at 70 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410615438.0A CN105621500B (en) | 2014-11-05 | 2014-11-05 | A kind of method prepared by ammino palladium (II) of high activity dichloro four |
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| CN201410615438.0A CN105621500B (en) | 2014-11-05 | 2014-11-05 | A kind of method prepared by ammino palladium (II) of high activity dichloro four |
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| CN105621500A true CN105621500A (en) | 2016-06-01 |
| CN105621500B CN105621500B (en) | 2017-09-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939100A (en) * | 2021-03-15 | 2021-06-11 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraammine palladium (II) bicarbonate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04108616A (en) * | 1990-08-29 | 1992-04-09 | Tanaka Kikinzoku Kogyo Kk | Production of tetraammine palladium dihydroxide |
| 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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2014
- 2014-11-05 CN CN201410615438.0A patent/CN105621500B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04108616A (en) * | 1990-08-29 | 1992-04-09 | Tanaka Kikinzoku Kogyo Kk | Production of tetraammine palladium dihydroxide |
| CN102616869A (en) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | Tetrammine palladium sulphate synthesis method |
Non-Patent Citations (1)
| Title |
|---|
| 余建民: "《贵金属化合物及配合物合成手册》", 28 February 2009, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939100A (en) * | 2021-03-15 | 2021-06-11 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraammine palladium (II) bicarbonate |
| CN112939100B (en) * | 2021-03-15 | 2021-11-09 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraammine palladium (II) bicarbonate |
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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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