CN105836814A - Synthesis method of tetraamminepalladium sulfate (II) - Google Patents
Synthesis method of tetraamminepalladium sulfate (II) Download PDFInfo
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- CN105836814A CN105836814A CN201610165127.8A CN201610165127A CN105836814A CN 105836814 A CN105836814 A CN 105836814A CN 201610165127 A CN201610165127 A CN 201610165127A CN 105836814 A CN105836814 A CN 105836814A
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- ammino palladium
- dichloro
- palladium
- sulphuric acid
- ammino
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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
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
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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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Abstract
The invention discloses a synthesis method of tetraamminepalladium sulfate (II). The method is composed of the following steps: dissolving potassium tetrachloroplatinate and ammonium acetate in water, then carrying out reflux reaction to synthesize cis-diamminedichloropalladium (II); reacting the cis-diamminedichloropalladium (II) with ammonia water to generate a tetraamminepalladium sulfate (II) compound. The method provided by the invention is easy to operate, can effectively remove chlorine ions, and has yield up to more than 90%.
Description
Technical field
The present invention relates to chemical field, the method for specifically a kind of synthesis sulphuric acid four ammino palladium (II).
Background technology
For manufacturing the part of high stable high-wearing feature, it usually needs deposit one layer of noble metal on coating, due to product requirement
Constantly increasing, require more and more lower to the residual of halogen element, the consumption of Halogen electroplate liquid is increasing.
Four ammino palladium (II) compounds are the palladium compounds that a class is important, are widely used in chemical catalysis and electroplating industry.
Wherein sulphuric acid four ammino palladium (II) ([Pd (NH3)4](SO4)) it is a kind of main salt of Novel electroplating, owing to its electroplating efficiency is high,
Clean environment firendly, has been widely used for electron trade plating palladium.The most often can be as the presoma of load type palladium catalyst
Compound.United States Patent (USP) [US6346222B] report uses sulphuric acid to drive the nitric acid in palladium nitrate solution, obtains palladium sulfate solution,
Sulphuric acid four ammonia palladium is obtained again with ammonia complexation.During need sulphuric acid to drive the nitric acid in palladium nitrate solution, obtain palladium sulfate,
Excess sulfuric acid is more, and by-product increases, and can produce substantial amounts of ammonium sulfate, affect the quality of product.Chinese patent
(201210315379.6) use Palladous chloride. and ammonia to react generation dichloro four ammino palladium solution, handed over by repeatedly anion
Swap out chloride ion, then generates sulphuric acid four ammino palladium with sulfuric acid reaction, and the method can effectively remove chloride ion, it is to avoid sulphuric acid
The generation of ammonium by-product, however it is necessary that and repeatedly exchange through ion, add workload, and part noble metal can adsorb
On ion exchange resin, the workload reclaimed after adding.Chinese patent (201210099564.6) uses Palladous chloride. and ammonia
Water reaction generates dichloro four ammino palladium (II), then reacts generation sulphuric acid four ammino palladium (II) with silver sulfate, and the method operates
Simply, generate without byproduct of ammonium sulfate, but silver sulfate to be used adds cost, and the silver chloride generated
By-product has a certain amount of palladium residual, adds difficulty for later noble metal recovery operation.Chinese patent
(201310312422.8) using Palladous chloride. is raw material, first generates palladium dydroxide with sodium hydroxide, is generating with sulfuric acid reaction
Palladium sulfate, palladium sulfate and ammonia react generation sulphuric acid four ammino palladium (II), the method can reduce the residual of inorganic salt, but
Reaction process is longer, and to use substantial amounts of ammonia with ammonia when palladium sulfate reacts, and has greater environmental impacts.
Summary of the invention
It is an object of the invention to provide a kind of simple to operate, can effectively remove the synthesis more than 90% of chloride ion, productivity
The method of sulphuric acid four ammino palladium (II), with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of method of synthesis sulphuric acid four ammino palladium (II), comprises the steps of:
(1) by back flow reaction synthesizing cis-dichloro two ammino palladium (II) after potassium chloropalladite and ammonium acetate water dissolution；
(2) cis-dichloro two ammino palladium (II) and ammonia react generation dichloro four ammino palladium (II)；
(3) after dichloro four ammino palladium (II) and sulphuric acid water dissolution, back flow reaction generates sulphuric acid four ammino palladium (II).
As the further scheme of the present invention: in step (1), potassium chloropalladite is 1:0.5～0.6 with the mass ratio of ammonium acetate,
Potassium chloropalladite is 1:50～100g/mL with the mass volume ratio of water, and with vinegar acid for adjusting pH value 5～6, during back flow reaction
Between be 3～5h.
As the further scheme of the present invention: in step (3), dichloro four ammino palladium (II) and H2SO4Mol ratio is
1:1.05～1.1, the molal volume of dichloro four ammino palladium (II) and water is than for 1:1.5～2mol/L, and reflux time is 4～6h.
Compared with prior art, the invention has the beneficial effects as follows:
The invention provides the synthetic method of a kind of sulphuric acid four ammino palladium (II), utilize potassium chloropalladite and ammonium acetate to react conjunction
Become cis-dichloro two ammino palladium (II)；The most cis-dichloro two ammino palladium (II) and ammonia react generation dichloro four ammino
Palladium (II)；Again dichloro four ammino palladium (II) is generated sulphuric acid four ammino palladium (II) compound with sulphuric acid back flow reaction.This
Inventing simple to operate, can effectively remove chloride ion, productivity is more than 90%.
Accompanying drawing explanation
Fig. 1 is the synthesis technique figure of the present invention.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, aobvious
So, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all
Belong to the scope of protection of the invention.
Potassium chloropalladite used in following example is self-control, and other reagent are domestic analytical pure, and water used is purification
Water.
Embodiment 1
Referring to Fig. 1, in the embodiment of the present invention, weigh potassium chloropalladite 100g respectively, ammonium acetate 55g, after water dissolution
Mixing, mends and adds water to 6L, with the 4h that refluxes after vinegar acid for adjusting pH value to 5, is filtered by the solid obtained, obtain after cooling
62g is cis-dichloro two ammino palladium (II), and productivity 96%.
Weigh 60g cis-dichloro two ammino palladium (II), with after the transparent clarification of appropriate ammonia solvent to solution by solution decompression
68g dichloro four ammino palladium (II) solid, productivity 98% is obtained after being concentrated near doing.
Weigh 61.2g dichloro four ammino palladium (II) with after water dissolution, add the sulfuric acid solution of 26.3mL 10mol/L, add
Water to the 5h that refluxes after 0.45L, solution is concentrated near dry after be concentrated under reduced pressure to give 65.5g sulphuric acid four ammino palladium (II), produce
Rate 97%, comprehensive yied (in terms of potassium chloropalladite) 91.2%, Chloride residue ＜ 5ppm.
Embodiment 2
Referring to Fig. 1, in the embodiment of the present invention, weigh potassium chloropalladite 750g respectively, ammonium acetate 450g, after water dissolution
Mixing, mends and adds water to 38L, with the 4h that refluxes after vinegar acid for adjusting pH value to 5, is filtered by the solid obtained, obtain after cooling
461g is cis-dichloro two ammino palladium (II), and productivity 95%.
Weigh 460g cis-dichloro two ammino palladium (II), after the transparent clarification of appropriate ammonia solvent to solution, solution is subtracted
Pressure is concentrated into after closely doing and obtains 523g dichloro four ammino palladium (II) solid, productivity 98%.
Weigh 490g dichloro four ammino palladium (II) with after water dissolution, add the sulfuric acid solution of 220mL 10mol/L, add
Water to the 5h that refluxes after 4L, solution is concentrated near dry after be concentrated under reduced pressure to give 518.4g sulphuric acid four ammino palladium (II), productivity
97%, comprehensive yied (in terms of potassium chloropalladite) 90.1%, Chloride residue ＜ 5ppm.
Embodiment 3
Refer to Fig. 1, in the embodiment of the present invention, weigh potassium chloropalladite 1000g, ammonium acetate 600g respectively, use water dissolution
Rear mixing, mends and adds water to 55L, with the 4h that refluxes after vinegar acid for adjusting pH value to 5, is filtered by the solid obtained after cooling,
To 621g cis-dichloro two ammino palladium (II), productivity 96%.
Weigh 620g cis-dichloro two ammino palladium (II), after the transparent clarification of appropriate ammonia solvent to solution, solution is subtracted
Pressure is concentrated into after closely doing and obtains 705g dichloro four ammino palladium (II) solid, productivity 98%.
Weigh 612.5g dichloro four ammino palladium (II) with after water dissolution, add the sulfuric acid solution of 263mL 10mol/L, add
Water to the 5h that refluxes after 5L, solution is concentrated near dry after be concentrated under reduced pressure to give 648g sulphuric acid four ammino palladium (II), productivity
96%, comprehensive yied (in terms of potassium chloropalladite) 90.3%, Chloride residue ＜ 5ppm.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only comprises
One independent technical scheme, this narrating mode of description is only the most for clarity sake, and those skilled in the art should be by
Description is as an entirety, and the technical scheme in each embodiment can also be through appropriately combined, and forming those skilled in the art can
With other embodiments understood.
Claims (3)
1. the method for synthesis sulphuric acid four ammino palladium (II), it is characterised in that comprise the steps of:
(1) by back flow reaction synthesizing cis-dichloro two ammino palladium (II) after potassium chloropalladite and ammonium acetate water dissolution；
(2) cis-dichloro two ammino palladium (II) and ammonia react generation dichloro four ammino palladium (II)；
(3) after dichloro four ammino palladium (II) and sulphuric acid water dissolution, back flow reaction generates sulphuric acid four ammino palladium (II).
The method of synthesis sulphuric acid four ammino palladium (II) the most according to claim 1, it is characterised in that step (1)
In, potassium chloropalladite is 1:0.5～0.6 with the mass ratio of ammonium acetate, and potassium chloropalladite with the mass volume ratio of water is
1:50～100g/mL, and with vinegar acid for adjusting pH value 5～6, reflux time is 3～5h.
The method of synthesis sulphuric acid four ammino palladium (II) the most according to claim 1, it is characterised in that step (3)
In, dichloro four ammino palladium (II) and H2SO4Mol ratio is 1:1.05～1.1, dichloro four ammino palladium (II) and water mole
Volume ratio is 1:1.5～2mol/L, and reflux time is 4～6h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610165127.8A CN105836814B (en) | 2016-03-22 | 2016-03-22 | The method of one kind synthesis ammino palladium (II) of sulfuric acid four |
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| CN201610165127.8A CN105836814B (en) | 2016-03-22 | 2016-03-22 | The method of one kind synthesis ammino palladium (II) of sulfuric acid four |
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| CN105836814B CN105836814B (en) | 2017-12-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946829A (en) * | 2018-08-06 | 2018-12-07 | 金川集团股份有限公司 | A kind of electrodialysis preparation method of four ammonia palladium of sulfuric acid |
| CN112897600A (en) * | 2021-03-15 | 2021-06-04 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraamminepalladium sulfate (II) |
| CN113185450A (en) * | 2021-03-15 | 2021-07-30 | 江苏海洋大学 | Palladium removal method for irinotecan hydrochloride intermediate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616869A (en) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | Tetrammine palladium sulphate synthesis method |
| CN102786100A (en) * | 2012-08-30 | 2012-11-21 | 贵研资源（易门）有限公司 | Synthetic method of palladium tetra-ammino sulfate |
-
2016
- 2016-03-22 CN CN201610165127.8A patent/CN105836814B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616869A (en) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | Tetrammine palladium sulphate synthesis method |
| CN102786100A (en) * | 2012-08-30 | 2012-11-21 | 贵研资源（易门）有限公司 | Synthetic method of palladium tetra-ammino sulfate |
Non-Patent Citations (1)
| Title |
|---|
| 杨天足等: ""贵金属冶金及产品深加工"", 《贵金属冶金及产品深加工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946829A (en) * | 2018-08-06 | 2018-12-07 | 金川集团股份有限公司 | A kind of electrodialysis preparation method of four ammonia palladium of sulfuric acid |
| CN112897600A (en) * | 2021-03-15 | 2021-06-04 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraamminepalladium sulfate (II) |
| CN113185450A (en) * | 2021-03-15 | 2021-07-30 | 江苏海洋大学 | Palladium removal method for irinotecan hydrochloride intermediate |
| CN112897600B (en) * | 2021-03-15 | 2021-11-19 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraamminepalladium sulfate (II) |
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| CN105836814B (en) | 2017-12-12 |
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