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Author: Subject: Making Lead(IV) acetate
guy
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[*] posted on 2-3-2005 at 18:58
Making Lead(IV) acetate


Lead(IV) acetate is described in my chemical dictionary as Pb(II) acetate plus Cl2 gas. It is a powerful oxidizer.
I'm confused on the details. Would this reaction be taken place in solution or dry and under what conditions? I don''t think it could be solution because the Cl- ion would react to precipitate PbCl2.

Does anyone know anything about this?

thx
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[*] posted on 3-3-2005 at 03:53


This synthesis was already detailed elsewhere. Please search. It's in the PbO2 thread, created by axehandle. The method was given by chemoleo.



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Eclectic
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[*] posted on 3-3-2005 at 11:12


I searched and couldn't find it. He's asking about lead TETRAacetate. Usually prepared from Pb3O4 and acetic anhydride.
However, if you bubbled Cl2 through a lead(II) acetate solution, I suspect you would get more PbO2 than lead tetraacetate. The ony way I can see it working is if the chlorine oxidizes half of the lead(II) acetate to lead tetraacetate and half of the lead is precipitated as PbCl2.
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[*] posted on 3-3-2005 at 11:23


Man I must be going blind, lately I'm making so many mistakes. Lead tetraacetate is made by reacting Pb3O4 (red lead - possibly obtainable from old ironmongers) with glacial acetic acid (glacial is usually used, I don't recall the use of dilute. A conc. solution >55% will probably be enough). A mixture of lead (II) and lead (IV) acetates results. For the method of seperation I'll must check it out. Thank you Eclectic for correcting me and sorry for correcting.

Edit: I've checked out for the seperation. It turned out that my old chem book has only a short reference to it, and only said to leave the mixture to crystallize. Lead (II) acetate must be formed due to the reaction with a mixed oxide (2PbO.PbO2), but it was not mentioned. The use of PbO2 with glacial acetic acid should be tested, maybe it will work. I've never heard about such a preparation though, sorry.

Edit2: Ecletic, I checked out your procedure. A mixture of glacial acetic and acetic anhydride can also be used. They do not mention the formation of lead (II) acetate. Maybe none is formed this way. Nice to know.

[Edited on 3-3-2005 by Esplosivo]

[Edited on 3-3-2005 by Esplosivo]




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[*] posted on 3-3-2005 at 11:57


Preparation without acetic anhydride (AA): Pb3O4 is slowly added to GAA, the temperature is kept below 60°C or the formed acetate is hydrolysed.
Purification by recrystalsation from GAA.

Another method using GAA and AA is described whereby a second crop of the acetate is yielded by venting dry Cl2 through the soup after the first batch has precipitated. This second batch is contaminated but can be cleaned by recrystallisation from GAA.

From the Brauer.




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[*] posted on 3-3-2005 at 14:41


Quote:
Originally posted by Esplosivo
Edit2: Ecletic, I checked out your procedure. A mixture of glacial acetic and acetic anhydride can also be used.

I've done this preparation long ago. It's really extremely easy when an excess of Ac2O and AcOH is used. The Pb(OAc)4 crystallizes out as white needles.
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[*] posted on 8-12-2005 at 19:40


Although out of the correct section (should be in technochemistry I guess), does anyone know any information on the electrochemical prepratory methods for lead tetraacetate?

The inorganic synthesis collection had this to say on lead tetracetate (BTW, is it tetraacetate or tetracetate? I get a fair number of either spellings in references).
Quote:
As is the case with most salts of higher valence metals, lead tetracetate may be obtained by electrolytic oxidation. This may be done by direct oxidation of the lower actate<sup>(1)</sup> or indirectly through the sulfate.<sup>(2)</sup>

(1)Elbs and Rixon: Zeit. Elektrochem., 9, 267 (1903)
(2)Elbs and Fisher: Zeit. Elektrochem., 7, 345 (1900)

Also in a synthesis for lead tetraacetate I found online by Cherrie Baby there were more references to the electrochemical preparation of this compound:
Quote:
[5] CA 51, 16146 (1957)
[6] CA 74, 49005x (1971)
[7] Oxidations in Org. Chem. part A, Wiberg, 1965, p277-366 - Academic Press.
I imagine the electrochemical methods might be just as taxing on my chemical supplies as the chemical methods of preparation but out of curiosity I was wondering if anyone had something else to go on.



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[*] posted on 21-3-2012 at 16:41


The attached paper, from IUPAC, goes into quite a description of the difficulties surrounding preparing & keeping Lead Tetraacetate. Based upon the discussion in the first part of the paper, of the problems caused by Acetic Anhydride (which apparently reacts with & presumably alters the product), the author describes the preparation using glacial acetic acid. Interesting read really.

Quote:
Preparation

Lead tetraacetate may be prepared (i) by the action of red lead (Pb3O4) with anhydrous acetic acid - a substantial amount of lead diacetate is also formed - the lead(II) salt may be separated by making use of its lower solubility in glacial acetic acid; (ii) by oxidation of lead diacetate with gaseous chlorine, again in a medium of glacial acetic acid; the PbCl2 formed is removed by filtration; (iii) for volumetric purposes we recommend the reagent to be prepared by dissolving red lead (Pb3O4) in glacial acetic acid at elevated temperatures; the lead tetraacetate crystals formed are isolated, recrystallized and the required amount is dissolved in a known volume of glacial acetic acid; solutions thus prepared contain no lead(II) salts, and if kept in dark-coloured stock bottles will remain stable for periods of several months. Their stability is decreased substantially by the presence of acetic anhydride or alkaline metal acetates. Due to the great volume changes of glacial acetic acid with temperature variations, conditions used must be such that the temperature does not vary within a range of more than +/- 1C during the analysis.


Attachment: Zyka.Analytical.Study.of.the.Basic.Properties.of.Lead.Tetraacetate.as.Oxidizing.Agent.pdf (1004kB)
This file has been downloaded 3518 times





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[*] posted on 31-12-2012 at 17:19


I guess, not sure about it, but lead ii, iv acetate can be prepared by dissolving lead with H2O2 Ac acid mix.
Pure lead IV acetate can be separated by Cl- as i didn't

ps.: a sort PbO2.H2O seems to exist aswell PbO.H2O, and it is white, calcining at mild heat reveals red lead oxide as product, first mistaken as Cd contamination

[Edited on 1-1-2013 by platedish29]
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[*] posted on 17-6-2020 at 01:46


If Pb3O4 is reacted with vinegar(10%), will it form tetra or only diacetate?
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