CN104891582A - Synthesis method of trans-dichlorodiammine palladium (II) - Google Patents
Synthesis method of trans-dichlorodiammine palladium (II) Download PDFInfo
- Publication number
- CN104891582A CN104891582A CN201510315777.1A CN201510315777A CN104891582A CN 104891582 A CN104891582 A CN 104891582A CN 201510315777 A CN201510315777 A CN 201510315777A CN 104891582 A CN104891582 A CN 104891582A
- Authority
- CN
- China
- Prior art keywords
- palladium
- trans
- synthetic method
- ammino
- trans dichloro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the field of synthesis of inorganic compounds, in particular to a synthesis method of trans-Dichlorodiammine palladium (II). The method includes the following steps: dissolving a disodium tetrachloropalladate solution in anhydrous ethanol, and then introducing high-purity ammonia gas for reaction to generate trans-Dichlorodiammine palladium (II) through one step; leaving the solution system to stand after the reaction for aging, and then filtering; washing and drying the precipitate to obtain trans-Dichlorodiammine palladium (II). The synthesis method provided by the invention uses disodium tetrachloropalladate as a starting material and adopts a one-step synthesis method, so that the process is simple; high-purity ammonia gas is adopted, and precise control of the reaction system is achieved, so that the product purity is improved; an ultrasonic reactor is adopted, and the reaction efficiency is improved, so that the product yield reaches 99.5% or above; the product obtained through the reaction is uniform in particle size distribution, fine and loose in particles, and easy to wash and filter, so that the product purity is as high as 99.9% or above.
Description
Technical field
The present invention relates to mineral compound synthesis field, particularly relate to a kind of synthetic method of trans dichloro two ammino palladium (II).
Background technology
Trans dichloro two ammino palladium (II) (trans-Pd (NH
3)
2cl
2), be a kind of yellow crystalline powder, stable, water insoluble in air; Palladium content is about 50.40%.Trans dichloro two ammino palladium (II) industrially has very important purposes, is mainly used in electron trade plating palladium, uses, also can be used as the precursor compound of load type palladium catalyst as palladium source in electroplate liquid.
The synthetic method that trans dichloro two ammino palladium (II) is conventional is: be dissolved in chloroazotic acid by palladium powder and generate tetrachloro-palladium acid, then generates trans dichloro two ammino palladium (II) by dropping ammoniacal liquor and hydrochloric acid.SD.Kirik (Structures and Isomerization in Diamminedichloropalladium (II) [J] .Acta Cryst.1996, B52, palladous oxide and hydrochloric acid reaction 909-916) is adopted to obtain tetrachloro-palladium acid, then add excessive ammonia and generate dichloro four ammino palladium, finally add hydrochloric acid again and generate trans dichloro two ammino palladium (II).
Above-mentioned two kinds of preparation methods are first prepare generation tetrachloro-palladium acid, and then by adding ammoniacal liquor and hydrochloric acid, finally generate trans dichloro two ammino palladium (II).Although the raw material of initial action is different, add ammoniacal liquor different with the process of hydrochloric acid, but above-mentioned two kinds of preparation methods at least generate end product by two-step reaction, and generate in the process of tetrachloro-palladium acid, palladium powder need be dissolved in the chloroazotic acid of severe corrosive and generate tetrachloro-palladium acid, or palladous oxide and hydrochloric acid reaction are obtained tetrachloro-palladium acid, capital is carried out under the environment of strong acid, equipment and operating process require strict, cause preparation process loaded down with trivial details, consuming time longer.In the tetrachloro-palladium acid of preparation, add excessive ammonia, too much consume raw material, and cause purification difficult in follow-up process, and also will introduce hydrochloric acid in reaction process, add the difficulty of subsequent wash, make product purity not high, cause serious environmental pollution.
Summary of the invention
For this reason, the present invention in order to solve dichloro two ammino palladium (II) synthetic method process in prior art loaded down with trivial details, consuming time longer, product purity is not high, the problem that causes environmental pollution serious, provide a kind of simple to operation, one-step synthesis, productive rate are high, product purity is high, the synthetic method of trans dichloro two ammino palladium (II) of environmental protection.
For achieving the above object, the present invention is by the following technical solutions:
A kind of synthetic method of trans dichloro two ammino palladium (II), comprises the following steps:
(1) by tetrachloro-palladium acid sodium (Na
2pdCl
4) be dissolved in dehydrated alcohol, then pass into ammonia and react, a step generates trans dichloro two ammino palladium (II);
(2) filtered after standing aging by step (1) reacted solution system, gained precipitation is trans dichloro two ammino palladium (II) after washing, drying.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), the purity of described ammonia is more than 99.99%.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), ammonia evenly passes into reaction system, and flow velocity is 0.5 ~ 5mL/min.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), the amount of substance passing into ammonia is 2-2.005 times of palladium amount of substance in tetrachloro-palladium acid sodium.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), the mass concentration that tetrachloro-palladium acid sodium is dissolved in tetrachloro-palladium acid sodium in the solution that dehydrated alcohol obtains is 0.5-5%.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), a step formation reaction is reacted under ultrasonication.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), carry out in ultrasonic reactor, ultrasonic frequency is 15 ~ 60KHz, and power is 200 ~ 1200W, and ultrasonic time is 30 ~ 300min, and temperature is 0 ~ 25 DEG C.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), the described standing aging time is 2 ~ 8h, is dehydrated alcohol and the deionized water wash of 0 ~ 25 DEG C repeatedly by temperature.
In the synthetic method of above-mentioned trans dichloro two ammino palladium (II), the condition of described drying is: vacuum tightness is 0.07 ~ 0.1MPa, and temperature is 40 ~ 120 DEG C, and the time is 4 ~ 8h.
Concrete reaction scheme is: Na
2pdCl
4+ 2NH
3→ trans-Pd (NH
3)
2cl
2+ 2NaCl.
Compared with prior art, the present invention has the following advantages:
1, the synthetic method of trans dichloro two ammino palladium (II) of the present invention, with tetrachloro-palladium acid sodium for starting raw material, obtains product with high-purity ammonia one-step synthesis, and preparation process is simple, consuming time short.
2, the synthetic method of trans dichloro two ammino palladium (II) of the present invention, tetrachloro-palladium acid salt and ammonia is adopted to react, ammonia can react with tetrachloro-palladium acid sodium fast, equably on the one hand, and accurately can control intake by coutroi velocity and the time that passes into; The usage quantity of ammonia is made to be no more than in tetrachloro-palladium acid salt and ammonia gas react process 0.5% of required stoichiometric number, need not excessive use ammonia, while conservation, reduce the content of ammonia impurity in product, be also convenient to subsequent purification, improve product purity.Use ammonia not use ammoniacal liquor on the other hand, be because local ammoniacal liquor in reaction system likely can be made in ammoniacal liquor adition process excessive, generate dichloro four ammino palladium (II) impurity.
3, the synthetic method of trans dichloro two ammino palladium (II) of the present invention, use tetrachloro-palladium acid sodium and dehydrated alcohol system, because this reaction need be carried out at a lower temperature, avoid causing the spilling of ammonia because temperature is too high and cause the impact on reaction, tetrachloro-palladium acid sodium is insoluble to cold water, but can be dissolved in dehydrated alcohol.
4, the synthetic method of trans dichloro two ammino palladium (II) of the present invention, utilize ultrasonic reactor, provide uniform reaction system, and with highly purified, even inflow, flow velocity is that the ammonia that 0.5 ~ 5mL/min passes into matches, improve reaction efficiency on the one hand, on the other hand the product of ammonia and the preparation passed into is uniformly dispersed fast, improve product yield, product yield can reach more than 99.5%, and the product cut size obtained is evenly distributed, particle is tiny and loose, easy washing and filtering, further increase the purity of product, make product purity up to more than 99.9%.
Embodiment
Illustrate in greater detail with specific embodiment below, but protection scope of the present invention is not limited to this.Wherein highly purified ammonia described in the present invention or high-purity ammonia to be purity be more than 99.99% ammonia.
Embodiment 1
1g tetrachloro-palladium acid sodium is dissolved in 100ml dehydrated alcohol, be placed in ultrasonic reactor and impose ultrasonication, ultrasonic frequency is 40KHz, power is 800W, ultrasonic time is 60min, temperature is 5 DEG C, while ultrasonication, highly purified ammonia is with the flow velocity of 2.5mL/min, reaction system is entered equably by gas distributor, the intake of ammonia is 150.7mL, subsequently reaction system is left standstill aging 5h, then precipitation is leached, be that the dehydrated alcohol of 5 DEG C and deionized water carry out repetitive scrubbing by temperature respectively, last is 0.07MPa in vacuum tightness, at 90 DEG C, dry 6h can obtain highly purified trans dichloro two ammino palladium (II) product.It is 99.80% that experiment records product yield, and wherein palladium content is 50.35%.
Embodiment 2
1g tetrachloro-palladium acid sodium is dissolved in 100ml dehydrated alcohol, be placed in ultrasonic reactor and impose ultrasonication, ultrasonic frequency is 25KHz, power is 500W, ultrasonic time is 150min, temperature is 10 DEG C, while ultrasonication, highly purified ammonia is with 1mL/min flow velocity, reaction system is entered equably by gas distributor, the intake of ammonia is 150.7ml, subsequently reaction system is left standstill aging 2h, then precipitation is leached, be that the dehydrated alcohol of 10 DEG C and deionized water carry out repetitive scrubbing by temperature respectively, last is 0.1MPa in vacuum tightness, at 60 DEG C, dry 5h can obtain highly purified trans dichloro two ammino palladium (II) product.It is 99.64% that experiment records product yield, and wherein palladium content is 50.34%.
Embodiment 3
1g tetrachloro-palladium acid sodium is dissolved in 100ml dehydrated alcohol, be placed in ultrasonic reactor and impose ultrasonication, ultrasonic frequency is 60KHz, power is 1200W, ultrasonic time is 120min, temperature is 15 DEG C, while ultrasonication, highly purified ammonia is with 1.25mL/min flow velocity, reaction system is entered equably by gas distributor, the intake of ammonia is 150.7ml, subsequently reaction system is left standstill aging 8h, then precipitation is leached, be that the dehydrated alcohol of 15 DEG C and deionized water carry out repetitive scrubbing by temperature respectively, last is 0.08MPa in vacuum tightness, at 120 DEG C, dry 4h can obtain highly purified trans dichloro two ammino palladium (II) product.It is 99.45% that experiment records product yield, and wherein palladium content is 50.26%.
Embodiment 4
1g tetrachloro-palladium acid sodium is dissolved in 24mL dehydrated alcohol, be placed in ultrasonic reactor and impose ultrasonication, ultrasonic frequency is 60KHz, power is 1200W, ultrasonic time is 100min, temperature is 5 DEG C, while ultrasonication, highly purified ammonia is with 1.5mL/min flow velocity, reaction system is entered equably by gas distributor, the intake of ammonia is 150.7ml, subsequently reaction system is left standstill aging 3h, then precipitation is leached, be that the dehydrated alcohol of 0 DEG C and deionized water carry out repetitive scrubbing by temperature respectively, last is 0.09MPa in vacuum tightness, at 40 DEG C, dry 8h can obtain highly purified trans dichloro two ammino palladium (II) product.It is 99.67% that experiment records product yield, and wherein palladium content is 50.35%.
Embodiment 5
1g tetrachloro-palladium acid sodium is dissolved in 252mL dehydrated alcohol, be placed in ultrasonic reactor and impose ultrasonication, ultrasonic frequency is 15KHz, power is 200W, ultrasonic time is 30min, temperature is 0 DEG C, while ultrasonication, highly purified ammonia is with 5mL/min flow velocity, reaction system is entered equably by gas distributor, the intake of ammonia is 150.7ml, subsequently reaction system is left standstill aging 3h, then precipitation is leached, be that the dehydrated alcohol of 0 DEG C and deionized water carry out repetitive scrubbing by temperature respectively, last is 0.09MPa in vacuum tightness, at 40 DEG C, dry 8h can obtain highly purified trans dichloro two ammino palladium (II) product.It is 99.56% that experiment records product yield, and wherein palladium content is 50.3%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a synthetic method for trans dichloro two ammino palladium (II), is characterized in that, comprise the following steps:
(1) be dissolved in dehydrated alcohol by tetrachloro-palladium acid sodium, then pass into ammonia and react, a step generates trans dichloro two ammino palladium (II);
(2) filtered after standing aging by step (1) reacted solution system, gained precipitation is trans dichloro two ammino palladium (II) after washing, drying.
2. the synthetic method of trans dichloro two ammino palladium (II) according to claim 1, is characterized in that, the purity of described ammonia is more than 99.99%.
3. the synthetic method of trans dichloro two ammino palladium (II) according to claim 2, it is characterized in that, ammonia evenly passes into reaction system, and flow velocity is 0.5 ~ 5mL/min.
4. the synthetic method of trans dichloro two ammino palladium (II) according to claim 3, is characterized in that, the amount of substance passing into ammonia is 2-2.005 times of palladium amount of substance in tetrachloro-palladium acid sodium.
5. the synthetic method of trans dichloro two ammino palladium (II) according to claim 1-4, is characterized in that, the mass concentration that tetrachloro-palladium acid sodium is dissolved in tetrachloro-palladium acid sodium in the solution that dehydrated alcohol obtains is 0.5-5%.
6. the synthetic method of trans dichloro two ammino palladium (II) according to claim 1-5, is characterized in that, a step formation reaction is reacted under ultrasonication.
7. the synthetic method of trans dichloro two ammino palladium (II) according to claim 6, is characterized in that, carry out in ultrasonic reactor, ultrasonic frequency is 15 ~ 60KHz, power is 200 ~ 1200W, and ultrasonic time is 30 ~ 300min, and temperature is 0 ~ 25 DEG C.
8. the synthetic method of trans dichloro two ammino palladium (II) according to claim 1-7, is characterized in that, the described standing aging time is 2 ~ 8h, is dehydrated alcohol and the deionized water wash of 0 ~ 25 DEG C repeatedly by temperature.
9. the synthetic method of trans dichloro two ammino palladium (II) according to claim 1-8, is characterized in that, the condition of described drying is: vacuum tightness is 0.07 ~ 0.1MPa, and temperature is 40 ~ 120 DEG C, and the time is 4 ~ 8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510315777.1A CN104891582B (en) | 2015-06-10 | 2015-06-10 | A kind of synthetic method of trans dichloro two ammino palladium (II) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510315777.1A CN104891582B (en) | 2015-06-10 | 2015-06-10 | A kind of synthetic method of trans dichloro two ammino palladium (II) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104891582A true CN104891582A (en) | 2015-09-09 |
| CN104891582B CN104891582B (en) | 2017-03-01 |
Family
ID=54024621
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510315777.1A Active CN104891582B (en) | 2015-06-10 | 2015-06-10 | A kind of synthetic method of trans dichloro two ammino palladium (II) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104891582B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776022A (en) * | 2019-09-23 | 2020-02-11 | 励福(江门)环保科技股份有限公司 | Preparation method of palladium tetraammine dichloride solid crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4335087A (en) * | 1979-08-16 | 1982-06-15 | Mpd Technology Corporation | Process for preparing cis-Pt(NH3)2 Cl2 |
| DD290546A7 (en) * | 1989-09-29 | 1991-06-06 | Saxonia Ag,De | PROCESS FOR PREPARING DIAMOND INDITROPALLADIUM (II) |
-
2015
- 2015-06-10 CN CN201510315777.1A patent/CN104891582B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4335087A (en) * | 1979-08-16 | 1982-06-15 | Mpd Technology Corporation | Process for preparing cis-Pt(NH3)2 Cl2 |
| DD290546A7 (en) * | 1989-09-29 | 1991-06-06 | Saxonia Ag,De | PROCESS FOR PREPARING DIAMOND INDITROPALLADIUM (II) |
Non-Patent Citations (4)
| Title |
|---|
| R. LE PENVEN等: "Studies of the electrodeposition of palladium from baths based on [Pd(NH3)2X2] salts. I. [Pd(NH3)2Cl2] baths", 《JOURNAL OF APPLIED ELECTROCHEMISTRY》 * |
| SUGIURA, CHIKARA等: "Palladium Liii x-ray absorption-edge structures of K2PdCl6, K2PdCl4, (NH4)2PdCl4, and trans-[Pd(NH3)2Cl2]", 《THE JOURNAL OF CHEMICAL PHYSICS》 * |
| V. ALETRAS等: "TERNARY COMPLEXES OF TRANS-Pt(NH3)2Cl2 WITH AMINO ACIDS AND NUCLEOBASES", 《POLYHEDRON》 * |
| 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776022A (en) * | 2019-09-23 | 2020-02-11 | 励福(江门)环保科技股份有限公司 | Preparation method of palladium tetraammine dichloride solid crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104891582B (en) | 2017-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103395847B (en) | The synthetic method of sulphuric acid four ammino palladium | |
| CN103183330A (en) | Controllable synthesis method for nitrogen and phosphorus co-doped graphitized carbon ball with hollow structure | |
| CN103241754B (en) | Production method of high-purity aluminum oxide | |
| CN110639475A (en) | UTSA-280 adsorbent material large-batch synthesis and forming method | |
| CN104163449A (en) | Preparation method of gamma-copper iodide | |
| CN102500315A (en) | LiX molecular sieve adsorbent and preparation method thereof | |
| CN104478699A (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN102584660A (en) | Method for purifying thiocarbamide | |
| CN103318976B (en) | A kind of technique being prepared tricobalt tetroxide by cobalt-carrying solution | |
| CN104891582A (en) | Synthesis method of trans-dichlorodiammine palladium (II) | |
| CN105152231A (en) | Method for preparing lithium battery anode material cobaltous hydroxide | |
| CN101224901B (en) | Continuous preparation method of high-purity magnesium hydroxide | |
| CN105984882A (en) | High-adsorption-capacity oxygen generation molecular sieve and preparation method thereof | |
| CN103803622B (en) | A kind of by the method for Aluminum Chloride Hexahydrate Dehydration for Aluminum chloride anhydrous | |
| CN110170311B (en) | Adsorption material based on modified sodium alginate microspheres and preparation method and application thereof | |
| CN102092766B (en) | Preparation method of ultrafine lanthanum oxide powder | |
| CN103524450A (en) | Synthetic method for accelerator DZ by using methanol as solvent | |
| CN111017979A (en) | Preparation method of low-calcium lutetium oxide | |
| CN110894066A (en) | Method for preparing sheet iron phosphate from titanium dioxide slag | |
| CN103482662A (en) | Method for intensifying Bayer method seeded precipitation process to produce sandy alumina | |
| WO2022242424A1 (en) | Purification method, system and detection method for n-methylmorpholine n-oxide and obtained n-methylmorpholine-n-oxide | |
| CN106220494B (en) | A kind of palladium acetate trimer preparation method | |
| CN105692667B (en) | A kind of preparation technology of aluminium hydroxide and alumina powder | |
| CN106905138A (en) | Microwave method synthesizes the method for rhodium caprylate | |
| CN203128193U (en) | Purifying and recovering equipment system of sulfur tetrafluoride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |