CN109592722A - A kind of preparation method of palladium nitrate - Google Patents
A kind of preparation method of palladium nitrate Download PDFInfo
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- CN109592722A CN109592722A CN201710925133.3A CN201710925133A CN109592722A CN 109592722 A CN109592722 A CN 109592722A CN 201710925133 A CN201710925133 A CN 201710925133A CN 109592722 A CN109592722 A CN 109592722A
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- palladium
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- palladium nitrate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A kind of preparation method of palladium nitrate, it is characterized in that, the Metal Palladium powder of high-purity is taken to be added in reactor, then the pure concentrated nitric acid solution of analysis that the mass percentage concentration for adding 4~9 times of metal palladium powder body weight is 65%~68%, maintain 10~70 DEG C of reactor temperature, side uniform stirring reaction solution takes 37% hydrochloric acid of mass concentration to 1~2%, and dilute hydrochloric acid is added in reaction solution until HCl mass is the 0.005%~0.25% of palladium powder quality in reactor；React 0.5~4h under constant stirring to get the palladium nitrate solution being completely dissolved to palladium powder；Beneficial effects of the present invention: operation of the present invention is simple, and process conditions temperature can make Metal Palladium be completely dissolved into palladium nitrate, remains without undissolved palladium-containing solid, the operation cycle is short, high yield rate.Chlorine is lower than 0.3% relative to mass percent (Cl/Pd, the wt%) content of palladium in the palladium nitrate solution of preparation, it might even be possible to be lower than 0.05%.
Description
Technical field
The present invention relates to a kind of methods for preparing fine chemical product palladium nitrate, the especially palladium nitrate solution of low chlorine content
Preparation method, belong to technical field of fine.
Background technique
Palladium nitrate solution is mainly for the preparation of catalyst, material surface coating etc..In palladium nitrate for much containing palladium chtalyst
When the preparation of agent, since chlorine element will cause the poisoning of catalyst, the chlorinity pole in palladium nitrate is generally required
It is low.Traditional method with aqua regia dissolution's palladium contains a large amount of chlorine in obtained solution, and is difficult to remove, this method one
As be used to prepare palladium chloride.And palladium is dissolved by heating with pure concentrated nitric acid, the extremely low palladium nitrate solution of available chlorinity, but
Be that this process can not be such that palladium is completely dissolved, thus be typically necessary after dissolution reaction filter out it is undissolved solid containing palladium
It is carried out dissolving this part palladium-containing solid again with a small amount of chloroazotic acid after body, or filtering.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies in the prior art, a kind of easy to operate, process conditions temperature is provided
The method of the palladium nitrate solution for preparing ultralow chlorinity of sum.Method provided by the invention can be such that Metal Palladium is completely dissolved into
Palladium nitrate is remained without undissolved palladium-containing solid, and the operation cycle is short, high yield rate.The nitre of method preparation provided by the invention
Sour palladium Chlorine in Solution is lower than 0.3%, especially matter of the chlorine relative to palladium relative to mass percent (Cl/Pd, the wt%) content of palladium
0.05% can be lower than by measuring degree.
A kind of preparation method of palladium nitrate, which is characterized in that take the Metal Palladium powder of high-purity to be added in reactor, then
The pure concentrated nitric acid solution of analysis that the mass percentage concentration for adding 4~9 times of metal palladium powder body weight is 65%~68%, maintains
10~70 DEG C of reactor temperature, side uniform stirring reaction solution takes 37% hydrochloric acid of mass concentration to 1~2%, is reacting
Dilute hydrochloric acid is added in liquid until HCl mass is the 0.005%~0.25% of palladium powder quality in reactor；Under constant stirring
0.5~4h is reacted to get the palladium nitrate solution being completely dissolved to palladium powder；
Chlorine is lower than 0.3% relative to the mass percentage content of palladium in obtained palladium nitrate solution.
Hydrochloric acid solution is added dropwise into reactor, until reactor in HCl mass be palladium powder quality 0.01%~
0.045%.Reaction process is to react 1~2h under constant stirring.Quality of the chlorine relative to palladium in obtained palladium nitrate solution
Degree is lower than 0.05%.
Beneficial effects of the present invention: operation of the present invention is simple, and process conditions temperature can make Metal Palladium be completely dissolved into nitric acid
Palladium is remained without undissolved palladium-containing solid, and the operation cycle is short, high yield rate.Chlorine is relative to palladium in the palladium nitrate solution of preparation
Mass percent (Cl/Pd, wt%) content be lower than 0.3%, it might even be possible to be lower than 0.05%.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
The Metal Palladium powder used in following embodiment is purchased from Shanghai Jiu Yue Chemical Co., Ltd., analyzes pure concentrated nitric acid and salt
Acid is purchased from Wuxi City prospect chemical reagent Co., Ltd.
Embodiment 1
100g Metal Palladium powder is added in reactor, the pure concentrated nitric acid solution of analysis of 8 times of palladium powder weight is then added,
Then stirred under the conditions of 35 DEG C, at the same add diluted aqueous hydrochloric acid solution (the HCl mass contained is palladium powder quality
0.02%) it, reacts 1 hour under constant stirring, palladium powder is completely dissolved as palladium nitrate solution, and Chlorine in Solution is relative to palladium
Mass percentage content is 0.027%.
Embodiment 2
100g Metal Palladium powder is added in reactor, the pure concentrated nitric acid solution of analysis of 9 times of palladium powder weight is then added,
Then stir at room temperature, at the same add diluted aqueous hydrochloric acid solution (the HCl mass contained is palladium powder quality
0.20%) it, reacts 3 hours under constant stirring, palladium powder is completely dissolved as palladium nitrate solution, and Chlorine in Solution is relative to palladium
Mass percentage content is 0.21%.
Embodiment 3
100g Metal Palladium powder is added in reactor, the pure concentrated nitric acid solution of analysis of 4 times of palladium powder weight is then added,
Then stirred under the conditions of 70 DEG C, at the same add diluted aqueous hydrochloric acid solution (the HCl mass contained is palladium powder quality
0.005%) it, reacts 2 hours under constant stirring, palladium powder is completely dissolved as palladium nitrate solution, and Chlorine in Solution is relative to palladium
Mass percentage content is 0.011%.
Claims (5)
1. a kind of preparation method of palladium nitrate, which is characterized in that take the Metal Palladium powder of high-purity to be added in reactor, then
The pure concentrated nitric acid solution of analysis that the mass percentage concentration for adding 4~9 times of metal palladium powder body weight is 65%~68%, maintains
10~70 DEG C of reactor temperature, side uniform stirring reaction solution takes 37% hydrochloric acid of mass concentration to 1~2%, is reacting
Dilute hydrochloric acid is added in liquid until HCl mass is the 0.005%~0.25% of palladium powder quality in reactor；Under constant stirring
0.5~4h is reacted to get the palladium nitrate solution being completely dissolved to palladium powder.
2. a kind of preparation method of palladium nitrate according to claim 1, which is characterized in that in obtained palladium nitrate solution
Chlorine is lower than 0.3% relative to the mass percentage content of palladium.
3. a kind of preparation method of palladium nitrate according to claim 1, which is characterized in that it is molten that hydrochloric acid is added dropwise into reactor
Liquid, until HCl mass is the 0.01%~0.045% of palladium powder quality in reactor.
4. a kind of preparation method of palladium nitrate according to claim 1, which is characterized in that reaction process is to be stirred continuously
1~2h of lower reaction.
5. a kind of preparation method of palladium nitrate according to claim 1, which is characterized in that in obtained palladium nitrate solution
Chlorine is lower than 0.05% relative to the mass percentage content of palladium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710925133.3A CN109592722A (en) | 2017-10-03 | 2017-10-03 | A kind of preparation method of palladium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710925133.3A CN109592722A (en) | 2017-10-03 | 2017-10-03 | A kind of preparation method of palladium nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109592722A true CN109592722A (en) | 2019-04-09 |
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ID=65956696
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710925133.3A Pending CN109592722A (en) | 2017-10-03 | 2017-10-03 | A kind of preparation method of palladium nitrate |
Country Status (1)
| Country | Link |
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| CN (1) | CN109592722A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4265757A1 (en) | 2022-04-22 | 2023-10-25 | Institute of Process Engineering, Chinese Academy of Sciences | Method for clean recovery of palladium |
-
2017
- 2017-10-03 CN CN201710925133.3A patent/CN109592722A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4265757A1 (en) | 2022-04-22 | 2023-10-25 | Institute of Process Engineering, Chinese Academy of Sciences | Method for clean recovery of palladium |
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| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190409 |
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| WD01 | Invention patent application deemed withdrawn after publication |