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Bedlasky
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Very impressive work Monoamine! I really enjoyed reading this report. Have you some plans for your thionyl chloride? I have some papers about
reactions of some transition metal oxides with SOCl2 or PCl5 if you are interested. You can also make VOCl3 from V2O5 and SOCl2.
Quote: Originally posted by teodor  |
It is different when SO2 is used because it looks like in this case SOCl2 is formed in a pure form. I mean the reaction of SO2 (usually in liquid
form) with PCl5, NbCl5, WCl6, and similar higher chlorides. |
Hi, Teodor. May I ask you where did you read this? Usually this goes in opposite way (metal oxide + SOCl2 --> metal chloride (or oxychloride,
depending on metal) + SO2).
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teodor
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| Quote: Originally posted by Bedlasky |
Hi, Teodor. May I ask you where did you read this? Usually this goes in opposite way (metal oxide + SOCl2 --> metal chloride (or oxychloride,
depending on metal) + SO2). |
Hi Bedlasky. Yes, this is interesting because is not mentioned very often. The first historical mention which I found is in the German book "Die
Chemie in Wasserahnlichen Losungsmitteln", Berlin, 1949. It's available from z-lib. If you will not find please U2U me, I will send it to you.
But I read first about this type of reaction in the book "Synthetic Inorganic Chemistry", William J.Lolly which I have in the paper form only. Here is
the scan of relevant pages:
Attachment: img-211222214652.pdf (2MB)
This file has been downloaded 197 times
But probably after evaporating SO2 the reaction goes as you said, so may be SOCl2 exists here only as dissolved molecules in SO2.
But your remark is very interesting. Probably all reaction which you have mentioned can go in opposite direction in such conditions.
[Edited on 22-12-2021 by teodor]
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Bedlasky
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Thanks, Teodor!
Maybe there is some sort of equilibrium. For example:
NbCl5 + SO2 <--> NbOCl3 + SOCl2
So when you dissolve NbCl5 in few times excess of liquid SO2, you obtain good yield of SOCl2. But when you rise temperature, SO2 become gas and
equilibrium shift to the left. I wonder how they separate SOCl2 from NbOCl3 and NbCl5 without evaporation of SO2.
This sort of equilibrium would exist even at room temperature. Wiki says this:
In the laboratory, niobium pentachloride is often prepared from Nb2O5, the main challenge being incomplete reaction to give NbOCl3. The conversion can
be effected with thionyl chloride.
So even at RT, conversion of Nb2O5 to NbCl5 isn't complete. These dehydratation reactions using SOCl2 or PCl5 are often quite complicated, involving
various chlorides/oxychlorides at different oxidation states or some addcuts with SOCl2/PCl5/POCl3.
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teodor
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Maybe adducts like Al2Cl6 * SOCl2 could be used to shift an equilibrium during the synthesis. This is also the way to purify the result. The question
is, how to break this adduct to make SOCl2 free.
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Alucard
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| Quote: Originally posted by Monoamine |
The heating mantle was turned to maximum.
At first, at around 100C, a lot of bubbling was observed in the H2SO4 bath. This is from evolving O2 via the
reaction:
2Na2S2O8 -> 2Na2S2O7 + O2
As the temperature in the still head rises to 300C the contents of flask A melts and is converted to SO3 and Na2SO4
via the reaction:
Na2S2O7 -> Na2SO4 + SO3
At this point vapours filled the apparatus and small clear drops of SO3 began to come over. Some vapour even came out of the upturned
funnel in the H2SO4 bath. There was also some brown discolouration in the SO3 that comes over which is due to the
SO3 oxidizing residual organic matter in the glassware.
[Edited on 14-12-2021 by Monoamine]
[Edited on 15-12-2021 by Monoamine] |
It's very strange cause Na2S2O7 melts about 400C, and it was not able to be molten by using gas camp stove (LPG), due to a reason camp stove gives
about 350C-380C heat range. I used Na2S2O7 made from NaHSO4 though...
Maybe it's possible to add some 95% H2SO4 to the molten chunk of Na2S2O7 in the flask I have, it is just a one damn piece of salt, but not sure if
this will help to melt it at about 300C, but I think I could try to do it.
Not sure it will help anyway, probably doing this will only cause H2SO4 azeotrope will be distilled over solid Na2S2O7 instead.
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Monoamine
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| Quote: Originally posted by Alucard |
It's very strange cause Na2S2O7 melts about 400C, and it was not able to be molten by using gas camp stove (LPG), due to a reason camp stove gives
about 350C-380C heat range. I used Na2S2O7 made from NaHSO4 though...
Maybe it's possible to add some 95% H2SO4 to the molten chunk of Na2S2O7 in the flask I have, it is just a one damn piece of salt, but not sure if
this will help to melt it at about 300C, but I think I could try to do it.
Not sure it will help anyway, probably doing this will only cause H2SO4 azeotrope will be distilled over solid Na2S2O7 instead.
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Hi Alucard,
I would give it a try. Adding sulfuric acid to catalyze the decomposition is what's done here and a camp stove should be plenty hot. You'll know when
it starts to work when the apparatus fils with dense white vapours. Let us know how it goes 
Also, cleaning out the remaining Na2SO4 (and probably some sodium pyrosulfate) is a bit tedious. Yes, it will fuse into a solid
chunk when it's cooled, so adding some water, heating it until a lot of solid dissolves in the water and pouring it into a bucket a few times will
eventually get the flask clean again.
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Monoamine
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| Quote: Originally posted by Bedlasky | Very impressive work Monoamine! I really enjoyed reading this report. Have you some plans for your thionyl chloride? I have some papers about
reactions of some transition metal oxides with SOCl2 or PCl5 if you are interested. You can also make VOCl3 from V2O5 and SOCl2.
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Hello Bedlasky, I was mostly hoping to use it to make acid chlorides and chlorinate alcohols. In terms of inorganic chemistry, trying to make thionyl
bromide (by reacting SOCl2 with dry HBr) might be something too. I don't know much about transition metals, but I'm curious to find out.
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Monoamine
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| Quote: Originally posted by teodor | Monoamine,
I have enough quantity of SOCl2 and that is the only reason I don't try to repeat your experiment which is very interesting indeed.
I think you can try to remove chlorosulfonic acid with NaCl or follow a procedure of SOCl2 purification with quinoline or dimethylaniline which I also
want to try because for some applications it is better to use a purified compound.
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Re distilling at a lower temperature could shed some light on whether there is chlorosulfonic acid in the product. Since their boiling points differ
by around 77C this should work fine.
Excess SO3 in the mixture can be dealt with by adding more SCl2 and then fractionally distilling off the unreacted
SCl2.
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Alucard
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| Quote: Originally posted by Monoamine |
Hi Alucard,
I would give it a try. Adding sulfuric acid to catalyze the decomposition is what's done here and a camp stove should be plenty hot. You'll know when
it starts to work when the apparatus fils with dense white vapours. Let us know how it goes
Also, cleaning out the remaining Na2SO4 (and probably some sodium pyrosulfate) is a bit tedious. Yes, it will fuse into a solid
chunk when it's cooled, so adding some water, heating it until a lot of solid dissolves in the water and pouring it into a bucket a few times will
eventually get the flask clean again. |
To add sulphuric acid as a catalyst I will need to prepare Na2S2O7 as a single step and mill it to powder before continuing. I see no reason to add
H2SO4 to a single chunk of Na2S2O7 in the flask, I think it will only cause H2SO4 to be distilled off, especially if H2SO4 will not be able to reach
bottom of the flask and will stay over surface of the Na2S2O7.
I only followed garage chemist's post
http://www.sciencemadness.org/talk/viewthread.php?tid=5495&goto=search&pid=121391
but reached about 550C or maybe 600C only, so Na2S2O7 melted and gave bubbling but very rarely aside with a small quantity of white mist, and nothing
was distilled off, because there was no enough of heat, as 650C or 700C needed, not 600C...
So I don't know if adding H2SO4 will even work when starting from sodium bisulfate but not from sodium persulfate, I think there might be a big
difference, and persulfate is better than bisulfate.
To say the truth it's probably not necessary to deal with oleum to obtain thionyl chloride, because there might be a possibility to prepare thionyl
chloride starting from sulfuryl chloride without using SO3, but using exactly SO2Cl2 and S2Cl2.
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teodor
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I am dreaming of getting SOBr2 from the reaction of SOCl2 with BBr3 which is described as good both in purity and yield. Also, I wish one day I will
be able to study the group of BX3 compounds including BF3.
But what is interesting, you can accidentally fall to sleep working with SOBr2. It is exceptionally good in delivering Br2 directly to the brain when
you have it in the air. And this causes this effect. At least, it is what the literature says.
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Monoamine
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| Quote: Originally posted by teodor | I am dreaming of getting SOBr2 from the reaction of SOCl2 with BBr3 which is described as good both in purity and yield. Also, I wish one day I will
be able to study the group of BX3 compounds including BF3.
But what is interesting, you can accidentally fall to sleep working with SOBr2. It is exceptionally good in delivering Br2 directly to the brain when
you have it in the air. And this causes this effect. At least, it is what the literature says. |
And by "asleep" you mean forever. Right? 
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teodor
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No, probably until the excess of Br2 will be metabolized by the body. But the danger is probably about those processes you will have going in the
laboratory while you are unconscious.
[Edited on 24-12-2021 by teodor]
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S.C. Wack
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Refluxing with S will convert the SCl2 to S2Cl2.
SCl2 + HSO3Cl -> SOCl2 + SO2 + HCl
| Quote: Originally posted by Monoamine | | Excess SO3 in the mixture can be dealt with by adding more SCl2 and then fractionally distilling off the unreacted
SCl2. |
SCl2 + 3SO3 -> S2O5Cl2 + SO2.
If one is going through this much trouble, I suspect that SO3 is better made from SO2, O2, a quartz tube, fire, and part of a catalytic heater from
ebay (it's a shame Coleman got out of the business...used models sell for at least twice as much as they did new 15 years ago) or equivalent...would
you believe that it might be easier to substitute SCl2 for SO2, soda-lime glass for quartz, and C for Pt?
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Monoamine
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Hi bibliomaster. Thank you for the insights. I'm starting to suspect that pyrosulfurylchloride may actually be a significant constituent of the final
product I got.
I'm reading this publication about it atm. (Sorry, I couldn't find a translation). One reason is also that the temperature at which distillate started coming
over at a fast rate is right around the boiling point of pyrosulfurylchloride.
Theoretically I would have had about 4x (molar) more SO3 than SCl2, I just thought I'd be very inefficient in producing it,
hence the excess. Now I wonder if the pyrosulfurylchloride could be induced to decompose to SOCl2...
But maybe it would be easier to just use 1kg of Na2S2O8 to make SO3 and distill it into 200ml of
SCl2, rather than 50ml. Then there would not be expected to be an excess of SO3 and it would be approximately stoichiometrically
equivalent.
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Monoamine
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| Quote: Originally posted by teodor |
No, probably until the excess of Br2 will be metabolized by the body. But the danger is probably about those processes you will have going in the
laboratory while you are unconscious.
[Edited on 24-12-2021 by teodor] |
Yes, that's a real truth. Don't do chemistry while unconcious. Also, turn off all flames before becoming unconscious.
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Bedlasky
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Sorry, but this reaction really doesn't work. You have 9 oxygen on the left and 7 on the right. Don't forget that this is redox reaction.
If your idea is dehydration of SOCl2, S2O3Cl2 is product. However I didn't find mention about this compound anywhere. Which isn't surprising,because
tetravelent sulfur doesn't form series of condensed compounds with S-O-S bridge like hexavalent sulfur.
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S.C. Wack
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Add another SO2.
Also, 2SO3 + SOCl2 -> S2O5Cl2 + SO2, and 5SO3 +S2Cl2 -> S2O5Cl2 + 5SO2
(do not bother counting)
This difficulty can however be overcome. DE139455 may interest you:
...Es wurde nun gefunden, daß man viel bequemer und billiger zum Thionylchlorid gelangen kann, wenn man Schwefeltrioxyd auf Einfachchlorschwefel
S2Cl2 bei einer Temperatur von etwa 75 bis 80C einwirken läßt.
Der Vorgang verläuft nach folgender Gleichung:
SO3 + S2Cl2 = SOCl2 + SO2 + S.
Sorgt man nun dafür, daß der bei der Reaktion gebildete Schwefel sofort wieder durch einen passend gewählten Chlorstrom zu Einfachchlorschwefel
chloriert wird, so erreicht man nahezu die theoretische Ausbeute an Thionylchlorid. Durch das vorliegende Verfahren wird also das lästige Arbeiten
mit dem leicht dissoziierbaren Doppeltchlorschwefel und das kostspielige Kühlen durch die Einhaltung der erforderlichen niederen Temperaturen, sowie
endlich die Bildung von Nebenproducten, wie Pyrosulfurylchlorid, vermieden. Das Verfahren wird durch das folgende Beispiel erläutert.
Beispiel:
In 1000 kg Einfachchlorschwefel, die sich in einem mit Rührwerk und Rückflußkühler versehenen Kessel befinden, läßt man ebenfalls 1000 kg
Schwefeltrioxyd in langsamem Tempo zutreten, indem man die Temperatur auf 75 bis 80C hält und gleichzeitig Chlor einleitet, um den bei der Reaktion
gebildeten Schwefel sofort wieder zu Einfachchlorschwefel zu chlorieren und somit der Umsetzung mit SO3 zu entziehen. Nach Beendigung der Reaktion
wird rektifiziert...
[Edited on 26-12-2021 by S.C. Wack]
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AJKOER
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My recent thoughts based on a source providing a guide on reaction rates relating to SO3 formation. Please review Page 209, here https://www.google.com/books/edition/Sulfur_in_the_Atmospher... by clicking on the 'Preview' key.
Based on this reference, I no longer, for example, recommend a Singlet oxygen path, but a path based on nitrogen oxide radicals that appears strong.
As to revised ideas, I once noted a seemingly strange path to SO3 cited in an old text that passing SO2 over HNO2 that can reputedly create SO3 (see
citation here http://www.sciencemadness.org/talk/viewthread.php?tid=85001#...). However, more recently, I found a reference consistent with such a path. Some
ideas as to how to implement follow, starting first with the proposed action of UV light on HNO2:
HNO2 + UV -> •OH + •NO
Or, perhaps better, •NO as a generated product from the decomposition on heating of HNO2, per Wikipedia https://en.wikipedia.org/wiki/Nitrous_acid , to quote:
"Gaseous nitrous acid, which is rarely encountered, decomposes into nitrogen dioxide, nitric oxide, and water:
2 HNO2 → •NO2 + •NO + H2O"
where HNO2 can be created, for example, by the careful step wise addition of H2O2 to NH3 (see https://www.researchgate.net/publication/317692348_Effects_o...) with an approximate reaction (use as a working estimate) given by:
NH3 + 3 H2O2 -> HNO2 + 4 H2O
where even dilute HNO2 here may be acceptable as it can be dehydrated (with CaCl2) or warmed to induce primarily nitrogen oxide product formation.
Note: a better (less water) perhaps choice on thermal decomposition at 330 C is Mg(NO3)2 with products, per Wikipedia https://en.wikipedia.org/wiki/Magnesium_nitrate:
2 Mg(NO3)2 → 2 MgO + 4 NO2 + O2
where MgO is a photocatalyst and note the added benefit of oxygen.
Continuing with the presumed action of minor water vapor on SO2:
SO2 + H2O = H2SO3 = H+ + HSO3-
My suggested path to the apparent required radical •HSO3 (per the source link provided below) is:
HSO3- + •NO -> •HSO3 + NO-
the last ion being a precursor to unstable H2N2O2. Note, the reaction rate between HSO3- and •NO2 (from the oxidation •NO) is provided previously
on Page 209, Eq 27 in the opening reference.
And finally, per Equation 10 at https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7558052/ , the final reaction with air/oxygen is claimed to be:
•HSO3 + O2 -> SO3 + H+ + •O2-
A confirming source on this path, per Page 43 at https://mymission.lamission.edu/userdata%5Cpaziras%5CChem102... , •NO being apparently a known catalyst for the action of O2 and SO2 leading to
SO3.
However, not sure if one can obtain a good amount of SO3 here, but the chemistry is suggestive of any path that conveniently radicalize humid SO2
creating •HSO3 which is further exposed to oxygen. For example, humid SO2 in strong light and air which actually is mentioned in Atomistry on SO3 at
http://sulphur.atomistry.com/sulphur_trioxide.html , to quote:
"Sulphur dioxide, when exposed to strong illumination, undergoes partial and reversible conversion into sulphur and sulphur trioxide."
which also suggests adding a strong photocatalyst (like ZnO, as conveniently sourced from zinc acetate at https://nanoscalereslett.springeropen.com/articles/10.1186/s...) where the electron hole (h+) may promote the •HSO3 radical formation:
HSO3- + h+ -> •HSO3
Another, less friendly path, but well known:
"Sulphur trioxide is formed to a small extent together with sulphur dioxide when sulphur or compounds of sulphur are burned in oxygen or air. In an
oxygen tomb, in the presence of a compound which on combustion yields water vapour and oxides of nitrogen, for example ammonium nitrate, the
combustion goes completely to sulphur trioxide."
Albeit, note: "Ammonium nitrate mixed with sulfur or with metal powders can be exploded by shock. " per https://webwiser.nlm.nih.gov/substance?substanceId=453&i... .
===========================
An interestingly idea on a more speculated path (which I surmised from the opening reference) is to employ the •HO2 radical, albeit, only half as
effective as •NO2, but this idea may still provide a workable and safer path.
In the current context, •HO2 could perhaps be conveniently formed from say a solid peroxide like zinc peroxide mixed with riboflavin subject to
water vapor and strong fluorescent light (see Reactions (6) to (9) here https://www.tandfonline.com/doi/pdf/10.1080/10473289.1996.10... and also this source: https://www.researchgate.net/publication/6323324_Formation_o... ).
Expected reactions leading to •HO2 are:
ZnO2 + H2O (vapor) = ZnO + H2O2
H2O2 + UV = •OH + •OH
H2O2 + •OH -> H2O + •HO2
and thereby theoretically also some SO3 in the gas stream per cited Reaction (31), which per the cited text may also be photochemical based again with
riboflavin as the photocatalyst under strong fluorescent light:
•HO2 + SO2 -> •HO + SO3 (31)
which all occurs apparently at around a reaction rate of 1/2 of the cited reaction rate with •NO2, namely:
•NO2 + SO2 -> •NO + SO3 (27)
where the SO3 would hopefully appear as a fine white deposit with cooling.
Kind of an interesting idea as one would be working without exposure to a very toxic acidic gas or high temperatures used to induce radicalization,
albeit all likely slower with a reduced yield.
Note: This approach can be viewed as cited above "Sulphur dioxide, when exposed to strong illumination, undergoes partial and reversible conversion
into sulphur and sulphur trioxide" with the added benefit of a peroxide (ZnO2) and also the photocatalyst ZnO created from the ZnO2, all in a very
amenable path.
[Edited on 27-12-2021 by AJKOER]
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Monoamine
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| Quote: Originally posted by S.C. Wack | Add another SO2.
Also, 2SO3 + SOCl2 -> S2O5Cl2 + SO2, and 5SO3 +S2Cl2 -> S2O5Cl2 + 5SO2
(do not bother counting)
This difficulty can however be overcome. DE139455 may interest you:
...Es wurde nun gefunden, daß man viel bequemer und billiger zum Thionylchlorid gelangen kann, wenn man Schwefeltrioxyd auf Einfachchlorschwefel
S2Cl2 bei einer Temperatur von etwa 75 bis 80C einwirken läßt.
Der Vorgang verläuft nach folgender Gleichung:
SO3 + S2Cl2 = SOCl2 + SO2 + S.
Sorgt man nun dafür, daß der bei der Reaktion gebildete Schwefel sofort wieder durch einen passend gewählten Chlorstrom zu Einfachchlorschwefel
chloriert wird, so erreicht man nahezu die theoretische Ausbeute an Thionylchlorid. Durch das vorliegende Verfahren wird also das lästige Arbeiten
mit dem leicht dissoziierbaren Doppeltchlorschwefel und das kostspielige Kühlen durch die Einhaltung der erforderlichen niederen Temperaturen, sowie
endlich die Bildung von Nebenproducten, wie Pyrosulfurylchlorid, vermieden. Das Verfahren wird durch das folgende Beispiel erläutert.
Beispiel:
In 1000 kg Einfachchlorschwefel, die sich in einem mit Rührwerk und Rückflußkühler versehenen Kessel befinden, läßt man ebenfalls 1000 kg
Schwefeltrioxyd in langsamem Tempo zutreten, indem man die Temperatur auf 75 bis 80C hält und gleichzeitig Chlor einleitet, um den bei der Reaktion
gebildeten Schwefel sofort wieder zu Einfachchlorschwefel zu chlorieren und somit der Umsetzung mit SO3 zu entziehen. Nach Beendigung der Reaktion
wird rektifiziert...
[Edited on 26-12-2021 by S.C. Wack] |
Oh wow! This is interesting info. Especially since S2Cl2 is somewhat easier to make (and more stable to store) than
SCl2! Thank you for sharing!
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Alucard
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| Quote: Originally posted by AJKOER |
•NO2 + SO2 -> •NO + SO3 (27)
where the SO3 would hopefully appear as a fine white deposit with cooling.
Kind of an interesting idea as one would be working without exposure to a very toxic acidic gas or high temperatures used to induce radicalization,
albeit all likely slower with a reduced yield.
[Edited on 27-12-2021 by AJKOER] |
I think you can probably burn sulfur in NO2 atmosphere with no O2 or air present, so :
2S + 3NO2 = 2SO3 + N2
If you really like NO2 to be involved...
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S.C. Wack
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BTW len1 was aware of the patent and made SCl2 anyways.
https://www.sciencemadness.org/whisper/viewthread.php?tid=10...
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Colleen Ortiz
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Hello,
This is such an insightful post. I have always found thionyl chloride fascinating myself. SOCl 2 is the chemical formula for thionyl chloride, an
inorganic compound. It's a colorless, fairly volatile liquid with a terrible acrid odor. The reaction between sulfur trioxide with sulfur dichloride
is the most important commercial synthesis. By heating oleum and gently distilling sulfur trioxide into a cooled flask of sulfur dichloride, this
synthesis may be adapted to the laboratory.
SO3 + SCl2 → SOCl2 + SO2
Syntheses from phosphorus pentachloride (The chemical compound PCl5 stands for phosphorus pentachloride. One of the most significant phosphorus
chlorides, along with PCl3 and POCl3, is POCl3. As a chlorinating reagent, PCl5 is used. Although commercial samples can be yellowish and polluted
with hydrogen chloride, it is a colorless, water-sensitive, and moisture-sensitive solid), chlorine and sulfur dichloride, or phosgene (The organic
chemical compound phosphogene has the formula COCl2. It's a colorless gas with an odor similar to freshly cut hay or grass in low quantities. Phosgene
is a valuable industrial component, notably for the manufacturing of polyurethane and polycarbonate plastic precursors.) are some of the other ways.
SO2 + PCl5 → SOCl2 + POCl3
SO2 + Cl2 + SCl2 → 2 SOCl2
SO3 + Cl2 + 2 SCl2 → 3 SOCl2
SO2 + COCl2 → SOCl2 + CO2
You should also try new reactions with thionyl chloride further. Thionyl chloride is primarily utilized in the manufacture of organochlorine
compounds, which are often employed as intermediates in medicines and agrichemicals. It is frequently favored over other reagents like phosphorus
pentachloride because its by-products (HCl and SO2) are gaseous, making product purification easier.
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basement
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I was just pointed to this thread.
Your method of producing SO3 was really neat. I was expecting this whole synthesis project to be based on Leonid Lerner's book and I'm surprised this
wasn't mentioned at all.
A very valuable source which also describes this process very similar in detail
I thought it has to be mentioned!
SMALL-SCALE SYNTHESIS of LABORATORY REAGENTS with Reaction Modeling
Leonid Lerner
2011
https://www.routledge.com/Small-Scale-Synthesis-of-Laborator...
[Edited on 25-1-2022 by basement]
[Edited on 25-1-2022 by basement]
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Monoamine
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Leonid Learner's Book
Hi Basement,
Props for mentioning Leonid Lerners book: "Small scale synthesis of laboratory reagents". I have a copy, but I was out of country at the time so I
couldn't use it. But I also highly recommend it. It's a really fun book and even goes into some of the mathematics behind reaction modelling.
Now that you mention it. I just saw a very relevant reaction in Lerner's book: It's how to make sodium pyrosulfate from the much easier to obtain
sodium hydrogen sulfate (NaHSO4). THis is from page 180:
2NaHSO4 -> Na2S2O7 + H2O, at T = 310oC.
So you can make sodium pyrosulfate at the same temperatures as the SO3 from pH down swimming pool additive. This is kind of neat, it means
that thionyl chloride can entirely be made from swimming pool supplies. (The things people put in their pools... yikes)
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