| Pages:
1
2
3 |
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
MAP PRO as a starting buildblock in home chemistry
MAP PRO gas is made out of propylene. It can be baugth for 10$ per pound without the taxes. This is quite cheap if compared to other hobby chemicals.
Because propylene contain a double bound, it is fairly reactive. If it was of me, I would start wit ethylene, but due to its low availability for the
home chemist, it would be hard to start with, considering its preparation from ethanol need quite a bit of apparatus.
Here will be started my journey to complex organic chemical, from industrial precursor. Some precursor can be considered as rare, but in later post,
there preparation will be disclosed.
Propylene oxide and 1-2 dichloropropane are the first tier of industrial propylene chemistry.
As a test run, I made 1-2 dibromopropane, however, soon I will make the dichloro variant.
The setup was made as in the picture 1 and 3ml of bromine added. Then the minimal flow of propylene was passed in the bromine with a glass tube. In
the original 0.3 ml of bromine try, PVC was used, but it dissolved in the product. After 10 minutes, a clear liquid with a smell which I already
smelled, but was not able to put my finger on it. I would say it smell isopropyl alcohol-alkanes. Yield was 4 ml with bad cooling
Next preparation: 1-2 dichloropropane and 1-chloro-2-propanol/2-chloro-1-propanol
Pictures:
[Edited on 29-5-2013 by plante1999]
[Edited on 29-5-2013 by plante1999]
I never asked for this.
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
1,2 dichloropropane
I would have weight the map pro bottle if I had a large enough scale, but it was not the case.
Chlorine was generated using hydrochloric acid and TCCA. The map gas was regulated to compensate for chlorine flow fluxuation.
The glass set up was very rudimentary, due to lack of liebig condenser 14/20, a water pump, and 14/18 thermometer. And ice bath was made arround the
flask and filled with propylene gas, then TCCA was added to diluted (15%) hydrochloric acid, a fog and some condensation imediatly appeared. The glass
adapter where the two gas mixed was extremly hot but the cooling bath did a good job. hydrochloric acid refill were made in the flask time to time,
and after 1 hour the experiment was stopped.
During the experiment, when the propylene gas flow was too fast, some fumes could get out of the flask, and indicated me to slow the flow of
propylene.
The yield was 53 g of 1,2 dichloropropane with some water condensation in it.
Costs:
HCl: 0.35 CAD
TCCA: 1 CAD
Propylene: Unknow, but approximatly 0.65 CAD
Total: 2.00 CAD for 53g (about 50ml)
Which bring the cost to 20$ per 500 ml (approx)
Hopefully, someone find this interesting... Next preparations should be propylene oxide and 1,2 diaminopropane (maybe propylene glycol)
Pictures:
I never asked for this.
|
|
|
Justin Blaise
Hazard to Self
Posts: 82
Registered: 5-10-2011
Location: Parts Unknown
Member Is Offline
Mood: No Mood
|
|
Very interesting. Do you plan on purifying the product by distillation? The MSDS for map pro gas says it only contains propene and propane, so perhaps
just drying the liquid is sufficient for good purity.
What is your plan for making propylene oxide? Do you plan on starting with propene, a chloropropanol, or something else?
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
Not distillation, due to lack of material, but it will be washed from possible HCl and drying it with K2CO3. MAPP gas used to contain methylacetylene,
but it is not the case anymore, the main impurity is propane, which is fairly unreactive in these conditions.
For the propylene oxide, chlorine will be passed in water with propylene to make chloropropanol, minimal amount of water will be added, and the
mixture distilled with Calcium oxide or sodium hydroxide.
The is possibility of dropping the price of 1,2 chloropropane greatly by using different mean of generating chlorine, it could easily drop to 6.50 $ /
500 ml.
I will see if I can put my paper diagram to something of interest on the computer.
That was easier than I tough, however I was using a trial, does anyone know a good free program to make diagrams?
PS: There is a small mistake, it should be both diaphragm. And not one membrane.
[Edited on 31-5-2013 by plante1999]
[Edited on 31-5-2013 by plante1999]
[Edited on 31-5-2013 by plante1999]
[Edited on 31-5-2013 by plante1999]
I never asked for this.
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
Very interesting that you have propylene readily available from the hardware store. I was under the impression that the MAPP gas cartridges contained
either methylacetylene-propadiene mixture (the original MAPP gas) or some kind of mixture which may or may not contain propylene. How can you be sure
that you're using pure propylene?
On the MAPP gas cartridges in my country it says "Propylene-Mixture". No further information is available on the manufacturer's website.
I think I should condense a portion of our MAPP gas product in a cold trap and then take a boiling curve with a thermometer while it boils off again.
If this is actually pure propylene, which would boil at a constant temperature of -48°C it would be great.
Propylene makes an excellent refrigerant for a single stage compressor cooling system, with both higher volumetric refrigeration capacity and lower
attainable temperatures than propane.
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
The purity is similar to laboratory grade chem:
http://www.worthingtoncylinders.com/Libraries/MSDS_Sheets/WC...
You may want to check for MAP-PRO(tm).
I never asked for this.
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
I'd really like to get a cylinder of this propylene. We don't have the gas from this manufacturer here (Germany), we only have Rothenberger cartridges
which are made from aluminium:
http://www.rothenberger.com/produkte/rothenberger/verbinden-...
I should ask the manufacturer for the safety data sheet on this.
In Austria, they have the steel MAPP gas cylinders which are similar to yours.
If you lived in Europe then I could fill some of my ethylene into a small cylinder and send it to you.
|
|
|
ScienceSquirrel
International Hazard
Posts: 1863
Registered: 18-6-2008
Location: Brittany
Member Is Offline
Mood: Dogs are pets but cats are little furry humans with four feet and self determination! 
|
|
The Benzomatic MAPP Pro gas is essentially pure propene, you might be able to order one off eBay or Amazon and get it shipped to Germany
http://www.bernzomatic.com/subcat.html?id=4
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
I found the MSDS for the Rothenberger MAPP stuff and it contains 10-25% isobutane in addition to propylene, so this is worthless as a refrigerant.
They probably added the isobutane to lower the vapor pressure of the mixture sufficiently to permit filling into aluminium cylinders instead of steel.
There are two additional sorts of MAPP gas being sold on german ebay.
One is from Airgas Inc. and constitutes a complex mixture of propylene, methylacetylene, propadiene, propane, butane and so on.
The other seems to be the MAP PRO gas which is pure propylene. I'm asking the seller for the MSDS.
|
|
|
ScienceSquirrel
International Hazard
Posts: 1863
Registered: 18-6-2008
Location: Brittany
Member Is Offline
Mood: Dogs are pets but cats are little furry humans with four feet and self determination!
|
|
The original MAPP Pro was a mixture of propyne and propadiene.
It burnt very hot indeed when mixed with oxygen and was used as a substitute for acetylene.
|
|
|
Mildronate
Hazard to Others
Posts: 428
Registered: 12-9-2009
Member Is Offline
Mood: Ruido sintetico
|
|
Is there other brands in my country local shops i had only seen propane/butane for soldering?
|
|
|
Intergalactic_Captain
Hazard to Others
Posts: 227
Registered: 4-9-2004
Location: somewhere where i don\'t know where i am
Member Is Offline
Mood: frabjous
|
|
The original MAPP was an tautomomeric clusterfuck - methylacetylene/propane/propadiene... No clue on the manufacturing process, but it was mainly a
methylacetylene/propadiene mess in a bottle. Definitely burned hotter than the current mapp-pro crap on the shelves now.
...That said, the current "MAPP" gas you're lilely to find is going to be mapp/pro (in the US at least)... Much larger proportion of propane versus
the interesting gases - And a much more useless flame when it comes to what propane vs MAPP is supposed to be used for...
...Plant, I find this pretty interesting - Not many (here at least) have actually experimented with MAPP gas... The only thing I've done with it
chemically was an attempt at a mapp vs. acetylene AgNO3 double salt which never worked - And it seems that Axt is the only one here who ever even
attempted that much. I applaud your attempts - I don't know what your plan is, but I'd like to believe it's more of a "what can I do with x" type
scenario - Cool shit, needs to be characterized beyond a the smell test though, for all anyone knows you may have just added a new tool to the amateur
organic toolkit - or not... Tis the way the game is played...
If you see me running, try to keep up.
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
Mildronate, the bottle is yellow, thats the best tip I can give you.
Well, I'm mostly planning to make valuable lab chem with simple labware, and common reagent. I have an interest in making a schiff base. At the moment
there is about 12 derivative of propylene I have planned. If I'm apple to find some ammonium molybdate cheaply I will also try ammooxidation of
propylene to acrylonitrile (and some HCN, that will be recovered in methanol sol. of KOH).
Now that it is propylene, silver salt is impossible, and possibly not energetic like Axt salt. I believe copper I form complex with it tough. I should
make copper I chloride to test. At least the mixture is purer than when I contained methylacetylene.
@Garage chemist:
Sad, I don't live near germany, but thanks anyway!
Good luck for your propylene quest!
I never asked for this.
|
|
|
ScienceSquirrel
International Hazard
Posts: 1863
Registered: 18-6-2008
Location: Brittany
Member Is Offline
Mood: Dogs are pets but cats are little furry humans with four feet and self determination!
|
|
These are the UK ones from Benzomatic;
Blue oxygen
Red propane
Yellow Propene
http://www.bernzomatic.com/subcat.html?id=4
[Edited on 31-5-2013 by ScienceSquirrel]
|
|
|
Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline
Mood: Chemistry: the subtle science.
|
|
Quote: Originally posted by plante1999  | If I'm apple to find some ammonium molybdate cheaply I will also try ammooxidation of propylene to acrylonitrile (and some HCN, that will be
recovered in methanol sol. of KOH).
|
I have made ammonium molybdate from the mineral molybdenite. I will tell how in a separate thread.
Thank you for pointing out the OTC availability of high grade propylene!
The single most important condition for a successful synthesis is good mixing - Nicodem
|
|
|
woelen
Super Administrator
Posts: 7977
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
In Europe we can buy Rothenberger Map/Pro gas. This is 99.5% propylene and 0.5% propane:
http://ebookbrowse.com/rothenberger-map-pro-gas-data-sheet-a...
This gas is supplied in a standard cylinder with CGA 600 outlet. There are multiple companies, selling these cylinders. One cylinder is fairly large
and bulky. It contains 400 grams (I think almost 600 ml in liquid form) of the gas mix. Such a cylinder has a price between 15 and 20 euros. This is
affordable, 400 grams of the gas goes a long way.
Unfortunately I cannot find simple CGA 600 regulators. The only thing I can find are complete torches, which can be connected to a CGA 600 socket and
these torches are expensive (EUR 50 at least, the better ones close to EUR 100).
You have to be careful not to buy the Rothenberger MAPP gas, you really need to buy MAP/PRO. The MAPP gas is somewhat more dense (a cylinder with this
gas holds just over 450 grams of gas) and this is a mix of all kinds of gases. These MAPP gas cylinders also are yellow and also have a CGA 600
outlet. You can easily see the difference, the Map/Pro cylinders have the text "MAP/PRO" in big letters on them, the others have the text "MAPP" on
them.
If someone knows a source for affordable CGA 600 regulators, then I would be really happy and then I'll order such a Rothenburger Map/Pro cylinder.
|
|
|
unionised
International Hazard
Posts: 5102
Registered: 1-11-2003
Location: UK
Member Is Offline
Mood: No Mood
|
|
Whatever the gas is, and whatever you plan to do with it, get a suck-back trap.
If the reagent- say bromine- ends up in the cylinder and corrodes it you have a nasty surprise waiting for you.
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
@Woelen: Where did you see the Rothenberger MAP PRO cylinders? Are these being offered at a hardware store near you, or would you have to order them?
If yes, where?
I'll get two cylinders, at least.
I will also need a suitable regulator for the MAP PRO cylinder.
Do you know whether the CGA 600 regulator is the same as the one that's used for the Multigas 300 (propane-butane) cartridges, described as 7/16" EU
coupling here:
http://www.rothenberger.com/products/rothenberger/bondingsol... ?
And why are the MAP PRO cylinders not listed on the Rothenberger website?
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
| Quote: Originally posted by Magpie | | Quote: Originally posted by plante1999 | If I'm apple to find some ammonium molybdate cheaply I will also try ammooxidation of propylene to acrylonitrile (and some HCN, that will be
recovered in methanol sol. of KOH).
|
I have made ammonium molybdate from the mineral molybdenite. I will tell how in a separate thread.
Thank you for pointing out the OTC availability of high grade propylene! |
Your welcomed, sadly I had looked for molybdenite in the past, and it was quite expensive, much more than I have on hand at the moment.
Unionised, I believe the pressure from the gas flow protect from sucback.
Woelen, I'm impress I can find something here that you have difficulty to get, or at least is much more costly, like 3 times the price here. Usually
it is the inverse.
I never asked for this.
|
|
|
woelen
Super Administrator
Posts: 7977
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
@garage chemist: I just ordered two cylinders of Map Pro gas from eBay:
http://www.ebay.de/itm/140980794096?ssPageName=STRK:MEWNX:IT...
This is the pure propylene gas (the ebay seller also states that it is propylene, which is honest, because for the intended application, MAPP gas is
better than propylene).
I also found quite a few torches, with built in piezo igniter and flame regulator, but I did not yet find a simple regulator, which allows the gas to
flow out of the cylinder into a rubber or PVC tube. I do not want to pay for all the bells and whistles which are on a complete torch system, so I'll
look further.
The same seller also sells freon gases, a few different kinds, also in such cylinders with CGA 600 outlet (this apparently is a standardized outlet).
I only ordered the propylene, which I want to use for chemistry experiments. The CGA 600 connection looks quite familiar to me, so it might be that I
can find a suitable regulator locally. I do not know the Multigas 300 connection, so unfortunately I cannot answer that question.
The Map Gas itself is not available in the Netherlands, over here there is MAPP gas for this application, which is a mix of propyne, propadiene,
propene, propane and some polymerization inhibitor. This MAPP gas also is more expensive (300 ml for EUR 25 or so).
I was pleased to read about the properties of propylene. It is virtually non-toxic (it only is considered an asphyxiation risk, like any gas) and
non-corrosive. MAPP gas on the other hand, is quite toxic, mainly due to the polymerization inhibitor, which makes up appr. 7% of the gas mix. So,
experimenting with propylene must be quite safe (of course, there still is the risk of fire, the gas is very flammable).
[Edited on 31-5-13 by woelen]
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
@woelen: I have a complete Rothenberger Roxy welding torch set that can be used with the Multigas 300 and Maxigas 400 cartridges. I have now found
that the Multigas 300 and MAPP cartridges have the same connection, and since you said that MAP PRO and MAPP also have the same connection this means
that I already have this CGA 600 regulator on my torch set.
I found this regulator available as an individual part here:
http://www.hausundwerkstatt24.de/Gasfeinregulierventil-von-R...
This should be the part that you're looking for- it connects to all disposable Rothenberger gas cylinders.
You will also need this M8x1 hose barb for connecting to a hose:
http://www.hausundwerkstatt24.de/Gewindetuelle-M8x1-RH-4mm
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Thanks plante. Your many contributions to SciMad are impressive and appriciated.
This may be usefull to anyone intrested in methyl acrylate... Depending on how easy the oxidation to acrylic acid is. I havnt researched it.
[Edited on 31-5-2013 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
| Quote: Originally posted by Bot0nist | Thanks plante. Your many contributions to SciMad are impressive and appriciated.
This may be usefull to anyone intrested in methyl acrylate... Depending on how easy the oxidation to acrylic acid is. I havnt researched it.
[Edited on 31-5-2013 by Bot0nist] |
Thanks, I believe acrylonitrile can be hydrolysed to acrylic acid. There is also pathway to methacrylic acid out of propylene itself, by its reaction
with HCl, and then reaction with Mg and then CO2 with subsequent hydrolysis. You could also do more industrial-like way.
I never asked for this.
|
|
|
woelen
Super Administrator
Posts: 7977
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
Thanks for this info, I just ordered from that company (they ship to NL as well). You also ordered two cylinders of propylene? I saw that two more of
these were ordered from the same seller.
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
So, woelen and garage chemist, what experimentation will you do with the propylene?
For some reasons, I can't experiment at the moment.
I never asked for this.
|
|
|
| Pages:
1
2
3 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
