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shr3k
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[*] posted on 30-1-2015 at 19:20
Benzyl Alcohol Extraction


Hi everyone, first post but a long time reader.

I finally decided to dip my toes into chemistry after seeing some cool stuff and ephedrine being extremely rare near me.

Before anyone judges, yes I am aware ephedrine can be used for naughty stuff... I'm not really into that sort of thing, I just like ephedrine for Gym/Weight Loss and late night work as a bouncer.

Anyway...

I found a paint stripper that contains between 40-60 % Benzyl Alcohol according to spec sheet and patent.

I built a small distil using copper pipe through a water bucket and invested in some laboratory glassware. I couldn't afford condenser yet hence copper work.

I heated 500ml of the stripper at 102.2 degrees celcius until liquid from the condenser all but stopped.

And this is where I realised i made a huge mistake... I now have a jar with what looks like blueish water and smells almondy and a thick oily jar smelling extremely almondy.

I have no idea where my Benzyl Alcohol might be and need some help or push in the right direction on where to go from here... if at all possible.

My ultimate goal is to get Benzaldehyde to create l-pac and then hopefully Ephedrine... seamed soo easy on paper!

Thanks
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[*] posted on 30-1-2015 at 19:37


Looked easy on paper? Good luck.

[Edited on 31-1-2015 by Loptr]
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[*] posted on 30-1-2015 at 21:53


Your temp, and hardware were wrong. 202 - 208*f is the range for distillation, and you will need a fractional column w/ the thermometer at the top port.

Run at 200*f for 1/2 hour, and discard everything. Slowly rise to 203, and discard the first 5ish ml. Then rise to 205, and collect until you see the temp raising by itself.
at that point shut down because you have recovered all the Benzyl you can safely get.

Hope it helps.

[Edited on 31-1-2015 by Zombie]




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[*] posted on 31-1-2015 at 13:14


Quote: Originally posted by Zombie  
Your temp, and hardware were wrong. 202 - 208*f is the range for distillation, and you will need a fractional column w/ the thermometer at the top port.

Run at 200*f for 1/2 hour, and discard everything. Slowly rise to 203, and discard the first 5ish ml. Then rise to 205, and collect until you see the temp raising by itself.
at that point shut down because you have recovered all the Benzyl you can safely get.

Hope it helps.

[Edited on 31-1-2015 by Zombie]


Thanks for the advice, 200 *c or *f. Seams that boiling point of the Benzyl is 205 *c.

Not sure how it changes in water etc so just wan't to check!
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[*] posted on 31-1-2015 at 14:13


It has a water azeotrope at close to 100 degrees C. Which is actually more like steam distillation than a true azeotrope. This is good because if your rig is as ramshackle as it sounds, going to 200 degrees might be hard as well as dangerous.

You need to tell how much of the 500ml was distilled and how much was left behind. You need to add a lot of water to make it all come over. The blueish color is copper salt or complex. Does your paint stripper also contain ammonia?
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[*] posted on 31-1-2015 at 14:22


Quote: Originally posted by Cloner  
It has a water azeotrope at close to 100 degrees C. Which is actually more like steam distillation than a true azeotrope. This is good because if your rig is as ramshackle as it sounds, going to 200 degrees might be hard as well as dangerous.

You need to tell how much of the 500ml was distilled and how much was left behind. You need to add a lot of water to make it all come over. The blueish color is copper salt or complex. Does your paint stripper also contain ammonia?


No ammonia, but it does have an Anti-Coagulant(sp).

I just finished today building a more stable rig until I can afford some chemistry equipment end of next month. Should suffice for simple experiments, not as if I will be selling the final product.

It's now a pressure cooker, with copper pipework built off from it, with various ports and connectors, all soldered and ptf-taped so should last a month.

I will test a run shortly and see what happens, I have made a hatch-work fractional condenser out of a thick copper tube with copper padding inside, like a mesh. This should act fairly well until such time I can afford something better, and seams it would do the job.

Another question, not sure if suited for a different thread though. My eventual goal was to try and make ephedrine. Formaldehyde is available pretty much over the counter here at 40% strength. I have read that reacting Benzaldehyde with Formaldehyde will result in Pseudo-ephedrine (Not desired) and Ephedrine. I can't seam to find any exact details on this. I remember reading about Formaldehyde and Ammonia Chloride but that created something not desired.

Thanks for the help so far, this has certainly been a fun but time consuming hobby so far! If all else fails I can always distill some Gin or Whiskey and drown my sorrows away!
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[*] posted on 31-1-2015 at 14:44


Quote: Originally posted by Cloner  
It has a water azeotrope at close to 100 degrees C. Which is actually more like steam distillation than a true azeotrope. This is good because if your rig is as ramshackle as it sounds, going to 200 degrees might be hard as well as dangerous.

You need to tell how much of the 500ml was distilled and how much was left behind. You need to add a lot of water to make it all come over. The blueish color is copper salt or complex. Does your paint stripper also contain ammonia?


My 200* is Fahrenheit ( 200*f) Your 100*c will carry over all the lighter compounds as well as the water. Plus he is well beyond the flash point of Benzyl Alcohol which is 205*f (lower when mixed with the ammonia compounds)
I believe he will then have to re distill or dry the water out in some other manner. Plus deal w/ the compounds carried over from the overheating The boiling point or Benzyl Alcohol being around 205^f he should be able to fractionate it at or near that Temp., and get an easier process w/ a cleaner product. Thus my recommending a long stabilization hold.

From what I found these strippers @ approx. 50% Benzyl contain 5 to 10 % amine or ammonia compounds and, Glycol as a thickening agent. Plus hydrogen peroxide as a lifting agent.

He will need to upgrade his equipment for several reasons. The first is safety, and secondly for purity of product.
The method needed addressing as well as the equipment.

He stated he ran till the source was depleted. Obviously just changing containers via heat, and leaching the copper compounds along the way. Plus whatever molecular changes occurred along the way.
No offense but the entire attempt should be considered a fail.

I think I may have thrown you for a loop with the Fahrenheit reference vs. Celsius. (which I shall use from now on.) ;)

I just noticed something else (besides the pressure cooker)
The Benzyl will boil off before the water, azeotrope or not. That shows the need for a fractional column due to the close boiling point of both water, and alch.

Back to the pressure cooker. Save that for hootch. It will do more harm than good in this application. Please!

References:
http://infohouse.p2ric.org/ref/20/19926/p2_opportunity_handb...

http://www.google.com/patents/WO1997029158A1?cl=en

[Edited on 31-1-2015 by Zombie]

[Edited on 31-1-2015 by Zombie]

[Edited on 31-1-2015 by Zombie]




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[*] posted on 31-1-2015 at 15:05


Quote: Originally posted by Zombie  
Quote: Originally posted by Cloner  
It has a water azeotrope at close to 100 degrees C. Which is actually more like steam distillation than a true azeotrope. This is good because if your rig is as ramshackle as it sounds, going to 200 degrees might be hard as well as dangerous.

You need to tell how much of the 500ml was distilled and how much was left behind. You need to add a lot of water to make it all come over. The blueish color is copper salt or complex. Does your paint stripper also contain ammonia?


My 200* is Fahrenheit ( 200*f) Your 100*c will carry over all the lighter compounds as well as the water. Plus he is well beyond the flash point of Benzyl Alcohol which is 205*f (lower when mixed with the ammonia compounds)
I believe he will then have to re distill or dry the water out in some other manner. Plus deal w/ the compounds carried over from the overheating The boiling point or Benzyl Alcohol being around 205^f he should be able to fractionate it at or near that Temp., and get an easier process w/ a cleaner product. Thus my recommending a long stabilization hold.

From what I found these strippers @ approx. 50% Benzyl contain 5 to 10 % amine or ammonia compounds and, Glycol as a thickening agent. Plus hydrogen peroxide as a lifting agent.

He will need to upgrade his equipment for several reasons. The first is safety, and secondly for purity of product.
The method needed addressing as well as the equipment.

He stated he ran till the source was depleted. Obviously just changing containers via heat, and leaching the copper compounds along the way. Plus whatever molecular changes occurred along the way.
No offense but the entire attempt should be considered a fail.

I think I may have thrown you for a loop with the Fahrenheit reference vs. Celsius. (which I shall use from now on.) ;)


References:
http://infohouse.p2ric.org/ref/20/19926/p2_opportunity_handb...

http://www.google.com/patents/WO1997029158A1?cl=en

[Edited on 31-1-2015 by Zombie]

[Edited on 31-1-2015 by Zombie]


Thank you for the explanation! I understand now, when I looked online originally I had never attempted a distillation in over 3 years... and to think I passed A Level Chemistry somehow... I initially thought, hey Benzyl is 205*c so boil it all at like 105 and I'll be left with Alcohol... Which I know was stupid and forgetting my chemistry lessons!

I have a little better setup to test and as mentioned, the purity isn't massively important. I'm not really that sure that when I finally end up with Ephedrine I will actually try it... Not until I have lab equipment, I just wan't to get there first and see it worked then invest in a little glassware to make some and then try new stuff :)
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[*] posted on 31-1-2015 at 15:17


Soooo why don't you just buy benzyl alcohol?
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[*] posted on 31-1-2015 at 15:21


Quote: Originally posted by Etaoin Shrdlu  
Soooo why don't you just buy benzyl alcohol?


Wasn't available near me :( Seams like a long way to get to ephedrine but Learning is fun :)
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[*] posted on 31-1-2015 at 15:30


Quote: Originally posted by Etaoin Shrdlu  
Soooo why don't you just buy benzyl alcohol?



Lol!!!

Shr... Do yourself a HUGE favor. Spend the 80.00 bucks on Ebay for a 1000ml fractional distillation rig. Add in a 5 pack of keck clips, and a 1000 ml Erlenmeyer flask. All together it will cost about 100.00 bucks.
Deschem it the supplier I have been using.
If you can afford to spend another 30.00 on something from them FREE SHIPPING. If not... Contact seller button, and ask for either a wholesale price break or the free shipping (they do free over 130.00.
Tim is your contact, and I won't mind if you tell him that Ken from SunCoast lab referred you.
Great glass at better prices.

Hell I forgot Dr. Bob. Right here on the forum...
http://www.sciencemadness.org/talk/viewthread.php?tid=15667

Get the right gear brother. It may be your health on the line

Edit: Read back to the first process I listed. The Temps. are important, and can not be guesses or close enough'ed.

[Edited on 31-1-2015 by Zombie]




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[*] posted on 31-1-2015 at 15:37


Quote: Originally posted by Zombie  
Quote: Originally posted by Etaoin Shrdlu  
Soooo why don't you just buy benzyl alcohol?



Lol!!!

Shr... Do yourself a HUGE favor. Spend the 80.00 bucks on Ebay for a 1000ml fractional distillation rig. Add in a 5 pack of keck clips, and a 1000 ml Erlenmeyer flask. All together it will cost about 100.00 bucks.
Deschem it the supplier I have been using.
If you can afford to spend another 30.00 on something from them FREE SHIPPING. If not... Contact seller button, and ask for either a wholesale price break or the free shipping (they do free over 130.00.
Tim is your contact, and I won't mind if you tell him that Ken from SunCoast lab referred you.
Great glass at better prices.

Hell I forgot Dr. Bob. Right here on the forum...
http://www.sciencemadness.org/talk/viewthread.php?tid=15667

Get the right gear brother. It may be your health on the line

Edit: Read back to the first process I listed. The Temps. are important, and can not be guesses or close enough'ed.

[Edited on 31-1-2015 by Zombie]


Thanks but I am in the UK, I can order the stuff right now, but looking at 3 weeks from china anyway, hence I said roughly a month :)

For now I just wan't to play, but yes safely! I bought a High Flow fan from a good friend, he was using it for... Growing purposes, with a new carbon filter, this is set up where I am working and pumping up into the loft and out through a window.

Not ideal but works fairly well.
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[*] posted on 31-1-2015 at 15:42


I used a range hood for quite some time. I know about "starting off"
I'm just getting a grasp on the chemistry myself but distilling I have been doing for close to 40 years. I sort of know that stuff. (a little):cool:

The glass should be much quicker. My last order (about 180.00) took 12 days to Florida .




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[*] posted on 1-2-2015 at 08:38


consider a 29/32 flask of whatever type and a 29/32 destillation bridge, about as cheap as it gets, but it may be tricky to check the temperature of your destillate, otherwise i have seen a paintcan with metal tube attached using molten bottlecaps working for destilling benzene out of NaOH and sodium benzoate, which is also running at a decent temperature
the bottle caps turns into rather heat resistant HDPE, commonly used for storing +95% H2SO4, also seems very hard to melt when it decides to settle




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[*] posted on 1-2-2015 at 09:03


That rig sounds like something I built years ago. Only used it two, three times and it literally had me so dam jumpy and nervous that I tore it apart and threw it in the junk pile. When I hear people building distilling equipment for chemistry I get that feeling of nervousness, very,very dangerous.

[Edited on 1-2-2015 by jhonthebaptist]
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[*] posted on 1-2-2015 at 12:51


I've given up on this idea for the moment, I don't have the right equipment and worth waiting, I could not get the temperature to stabilize at 200*f at the top of the fractional distillation column I built, it kept wanting to sit at 214.2*f

Anyway, learning fast and ordered glassware today, hopefully quick delivery!
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[*] posted on 1-2-2015 at 15:09


29/32 is an obscure grind size. I remember reading about that size in Australia (I think). 29/32 is a little more common, and 29/40 seems to be the most common.
Just sayin'

I hope someone else (in the future finds this thread helpful, cause now I feel like I was left at the alter...
No worries. I'll get over it, someday.:)




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[*] posted on 1-2-2015 at 15:57


Quote: Originally posted by Zombie  
29/32 is an obscure grind size. I remember reading about that size in Australia (I think). 29/32 is a little more common, and 29/40 seems to be the most common.
Just sayin'

I hope someone else (in the future finds this thread helpful, cause now I feel like I was left at the alter...
No worries. I'll get over it, someday.:)


I will in 3 weeks when my fractional kit arrives from China! Not going to learn anything serious by hacking together junk!
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[*] posted on 1-2-2015 at 16:06


It's too late to edit my post because it has been quoted.
My apologies it was misleading.

24/29, and 24/40 were the sizes I meant to state.

24/29 appears to be more common in Europe, and the US. While 24/40 appears to be leading as a global standard.

My apologies... the 29/32 is far less common.




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[*] posted on 2-2-2015 at 09:07


the standard is 29/42. The overseas guys produce a lot of joints that are 29/(some number less than 42). They will all fit together.

You might have to take a small hammer and tap on the end of the glass to get them to fit snugly (just kidding).
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[*] posted on 3-2-2015 at 10:54


Quote: Originally posted by Antiswat  
otherwise i have seen a paintcan with metal tube attached using molten bottlecaps working for destilling benzene out of NaOH and sodium benzoate, which is also running at a decent temperature
the bottle caps turns into rather heat resistant HDPE, commonly used for storing +95% H2SO4, also seems very hard to melt when it decides to settle


That sounds like my video on youtube.




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