| Pages:
1
2 |
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
Then how did cyclonight get such good results?
|
|
|
Panache
International Hazard
Posts: 1290
Registered: 18-10-2007
Member Is Offline
Mood: Instead of being my deliverance, she had a resemblance to a Kat named Frankenstein
|
|
Do we know that? We know he said what he said, as did i, maybe he exaggerated, maybe i downplayed it, maybe i exaggerated and he downplayed it. Sm is
not peer reviewed. Maybe instead of benzaldehyde i'm getting mad kilo's of gold out of the reaction and i'm greedy and want no one else to know.
Maybe he had accepted jesus as his lord and saviour and was blessed by the wholely (or is that holely) spirit.
Maybe his raiki was tuned better into his chakras.
Maybe you should tell your parents to jam it and do an experiment.
One things for certain,
WE WILL NEVER KNOW.
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
very funny lol 
|
|
|
simba
Hazard to Others
Posts: 175
Registered: 20-5-2011
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by questions  | There is no easy way to make benzaldehyde, I think the best way is to get it from a chemical company that use it for their business and try buying it
from them.
I have tried most of the benzaldehyde making methods and they all yeild very little product.
|
Indeed. I managed to buy piperonal this way.
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
Has anybody else actually tried cyclonights cinnamon oil method of making benzaldehyde by slowly dripping the oil into the reaction mix and steam
disstilling the formed benzaldehyde at the sae time?
|
|
|
peach
Bon Vivant
Posts: 1428
Registered: 14-11-2008
Member Is Offline
Mood: No Mood
|
|
I have, but I preferred the persulphate method.
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
was the coversion rate of cinnamon oil to benzaldehyde really like around 75% to 90% like he says?
And how long dd it take to drip all the cinnamon oil through and how much cinnamon oil did you use?
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
was the conversion rate of cinnamon oil to benzaldehyde really like 75% to 90% like cyclonight said?
Also, how much cinnamon oil did you drip into the reaction mix and how long did it take for all the cinnamon to drip in?
you can see how facinated i am by this method
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
Cinnamon oil to benzaldehyde
OK everyone, there has been a lot of hype about making benzaldehyde from tolune. I personaly believe that it may be easier to make benzaldehyde from
cinamon oil that has a high content of cinnamon aldehyde as it has been illustrated by an old user called cyclonight. Unfortunately cyclonight hasn't
been on this site for like ages and I have read his work and have accumulated a lot of questions which I'm trying to find answers to.
I am not in a position to do an experiment as I'm living with my parants and they hate the idea of me playing around with this stuff and we're now in
the process of moving.
Thus every time I ask questions about making benzaldehyde from cinamon everyone gets annoid for they areonly intereste in making benzaldehyde from
toluene, which I have personaly done and have found that process an incredably huge waste of time. I would have theee hot plate stirrers and three
500ml beackers on each and it would take hours to charge the solution with electricity up and then it would take about anoter hour to convert the
toluene to benzaldehyde and the yeildswere very lown and then I would have to disstil the benzaldehyde out under vacuum and after spending a whole
week wrth of work, i'd only have about 50ml to 75ml of pure benzaldehyde. It really wasn't worth the effort.
I have since been trying to find more people who are interested in finding amethod that can be used to makelarge quantities of benzaldehyde and I
believe there is some hope in the cinnamon oil method. Thats right, that very common and cheap cinnamon oil you buy over the counter in any health
food store or even over the internt, that is what is used to make benzaldehyde.
I will provide the link that cyclonight posted and hopefuly we can all pool our experience and knowledg and master the method of making benzaldehyde
from ccinnamon oil (cassia oil).
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
OK everyone, here is the method discovered by cyclonight, apparently this is the bees kness for making benzaldehyde according to cyclonight who has
proven himself to be a very smart and credable person who likes to experiment.
This is what we need to experiment with and work on and hopefully even improve;
Cinnamon oil to benzaldehyde update.
Hi peeps, been off the forum a good while but its good to be back .
I’ve significantly improved the original batch method I posted last year, what follows is my latest method.
This approach uses the same setup as the last steam distillation variation graphically depicted in in this thread.
Basically, the items used were:
hot plate, pressure cooker steam generator & associated tubing, etc
3L 3-neck RBF & mantle
vigreux column, right angle bend & still head
condenser
Vacuum pump & glassware for purfying the final product & recycling unreacted cinnamaldehyde.
chemicals: 2 litres tap water, lecithin, cinnamon oil, NaOH
Essentially, a large reaction vessel and a means of steam & vacuum distilling are all the equipment really required.
Begin by setting up all equipment, add 2 L water & ~1.5g lecithin.
The first variation is to use OTC sodium hydroxide instead of sodium carbonate, simply add the alkali to adjust the pH within the range of 12-13, only
small amounts are required.
The second variation is to slowly drip in the cinnamon oil during the course of the reaction, the benzaldehyde being steam distilled as it forms.
Begin the addition once the pH adjusted solution has heated to boling temperature and the steam is passing though the solution.
The third variation is to stop the cinnamon oil addition after 5 min, then check the distillate. If benzaldehyde is clearly distilling over, then
continue with the addition.
A crude test is to simply taste the steam distillate as it drips into the receiving vessel, if it burns your tongue off, then you're doing well. If it
tastes sweet, then significant quantities of cinnamon are being carried over. Should this not change after a short while, then double check the pH !
Provided that the pH is correct and the cinnamaldehyde content is high (70%+) then benzaldehyde laden distillate should start collecting almost
immediately after the addition has begun.
However, if it is not, wait for the benzadehyde to start collecting, THEN continue with the addition. This prevents unnecessary amounts of
cinnamaldehyde being steam distilled at the start of the process, which is a serious problem with the old batch mode reaction.
Note that by slowly dripping the cinnamon oil instead of adding it all at once to the reaction mix, single run conversion is increased by 20-30%.
Ensure the rate of cinnamon oil drip rate is approximately equivalent to the quantity of oil being steam distilled, thus maintaining high dilution in
the reaction mixture.
After 300 to 500 ml of cinnamon oil had been added, the drip rate is stopped and the steam distillation continued until all the aldehyde has been
steam distilled from the reaction mix. If using less than 2L of water, then adjust proportionally to maintain the same dilution. At this point, dump
the mix and replace with clean pH adusted water with at least ~1.5g lecithin.
This step removes tar and other junk that slows down the reaction and reduces benzaldehyde production. Significantly reduced tar formation will also
result from periodically carrying out this step (very imporant if high yields are desired).
Also note that with this method, the pH tends to slowly drop over time during the course of the steam distillation, so check the pH every couple
hours, and top up with NaOH if and when required. Its preferable to simply add small amounts concentrated NaOH solution when topping up, using a
dropper makes the alkali addition much simpler since NaOH pellets will rapidly collect moisture and stick to the sides of the reaction vessel.
Efficiency is further improved if the steam distillate (after oil separation) is also extracted with DCM, though this isn't absolutely necessary.
Once the the product oil is pooled, vacuum distillation will remove the benzaldehyde - no need to vacuum distill the recycle cinnamon aldehyde, just
drip it into the steam distillation vessel, just as with the cinnamon oil feed. Expect the quantity of unreacted cinnamon aldehyde to be circa 25%,
but if the reaction mix was kept clean during the process then it may be considerably less. The benzaldehyde distillate is clear, & much purer
than the original solvent extraction method that doesn't employ the steam distillation. Give the batch solvent extraction a rest folks, use the steam
distillation variation if producing benzaldehyde from cinnamon oil!
Far, far less work.
Using the above approach, overall molar conversion to benzdehyde is at least 80%.
I’ve managed higher conversion efficiencies (~90%), but the reaction efficiency is subject to variation according to varying reaction conditions,
i.e. feed rate, reaction mix volume (i.e. dilution), and the quantity of cinnamon oil fed to the reaction mix before changing the solution. >80%
seems to be a realistic overall figure.
Also...
Remember to keep the reaction mix free of tar & cinnamon oil impurities as much as possible to give consistent high yields.
If dripping the aldehyde into the mixture isn't practical for any reason, you can periodically add the cinnamon oil in small batches, say 20-50 ml at
a time to give good conversion, but expect a little more cinnamonaldehyde to distill over.
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
OK guys, I have made a thread for making benzaldehyde from cinnamon oil. Clearly you are tunnel visioned by making benzaldehyde from toluene (and good
luck to you), but for those of you who have an interest in this new and not so talked about method whereby cinnamon is used, then come to this new
thead and share your ideas
The thread is called; cinnamon oil to benzaldehyde
http://www.sciencemadness.org/talk/viewthread.php?tid=18351#...
|
|
|
entropy51
Gone, but not forgotten
Posts: 1612
Registered: 30-5-2009
Member Is Offline
Mood: Fissile
|
|
Then you're
doing it wrong. As in the way you misspelled "yield". | Quote: Originally posted by questions | My lab was at my friends house and we did our little experiments in his garage. Unfortunately his mother has found a new guy and he is now living in
the house and has started asking questions about us. I cant experiment in there anymore and it would be far too difficult for me to do it anywhere
else. Also, I'm still living at home with my parents and they'd kill me if they sore me doing those sort of things 
Thus I'm hoping to find people who have already done these things and can help me out, it sucks I know |
Oh, now I understand why.
[Edited on 25-12-2011 by entropy51]
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
Making benzalehyde via oxidisng toluene is the method tha was using and I would only get 50ml to about 75ml per time.
would have o spend hours charging he cell up and then more time to convert the cinamon to benzaldehyde. The process was very corosive as ev
erythingin the garagethat was made of steel was corroding, even the screws in the door that hold the know to the door were corroded out.
Using the toluene method isthe hardest method possible it sucks.
Not just that but it is very time consuming to remove all the benzaldehyde, toluene and byproducts out of the mix after i has been discharged in the
reaction.
Overall I can tell you from 6 months ofsolid practise off this method that it sucks arse
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
It sucks arse because of four main reasons;
1) It is corrosive to things around it
2) It uses up too many reasorces
3) The reaction takes to long to complete
4) The produt obtained is very little given the large amount of work involved
|
|
|
Nicodem
|
Threads Merged
25-12-2011 at 03:02 |
Nicodem
|
Thread Moved
25-12-2011 at 03:09 |
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
I managed to do my first experiment in converting the cinnamon oil to benzaldehyde at my mates house while his mum went to queensland
basically we added 200 ml of cinnamon oil to 2L of boiling water with NaOH in it at ph of about 12.88 and boiled it for 7 hours n a round bottom
flask. The reaction went for seven hours and it was then that we ecided to stop the reaction and see the yeilds and much to our dissmay, we found that
about 60% of the cinamon oil had turned to tar, the other 30% had turned into benzaldehyde and the other 10% was unreacted cinnamon oil.
I have discovered that there is basically one thing wrong with this reacion that is making it such a pain in the arse for everyone.
Basically as the cinnamon aldehyde turns into benzaldehyde, the benzaldehyde emediatly starts to turn into tar and sludge-like-shit.
The problem here is that we need a way to preserve the formed benzaldehyde as it remains in the solution as it is formed so to stop it from turning
into shit after it has been made from the cinnamon aldehyde.
Do you have any such ideas that would help minimise the benzaldehyde from turning into tar durring the course of the reaction?
Asking questions is the best way to understand anything.
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
I love benzaldehyde, not just for it's broad uses, but because of it's signature smell and oily texture, it's also very xpensive as well I hear.
I've been doing a lot of research into the reaction of cinnamon aldehyde in a boiling solution of water with ph 11 to 13 and antifoaming agent.
I've tried the experiment and have found that the more benzaldehyde is made, the more tar is formed in the reaction.
After an 7 hour reaction of 200ml of cinnamon aldehyde in a 2L solution of boling water with a steady ph of 12.5 and antifoaming agent, only 30% was
benzaldehyde, 20% was unreacted cinnamon and the other 50% was all this tar shit.
I think that the aceteldehyde is reacting with the benzaldehyde in this base solution and that is what is making all this tar shit. Because I don't
believe that this tar shit is a product of the cinnamon turning into benzaldehyde and acetaldehyde, I think that shortly after the benzaldehyde has
formed, it reacts with the acetaldehyde that has formed. I cant think of any other explanation and I certainly dont think that the benzaldehyde is
reacting with the cinnamon, could it????
If it is such that the formed benzaldehyde is reacting with the formed acetaldehyde, what can we put in place to stop or even minimise this from
happening?
Asking questions is the best way to understand anything.
|
|
|
questions
Hazard to Others
Posts: 103
Registered: 12-2-2011
Location: Australia
Member Is Offline
Mood: curious
|
|
Yep, the acetaldehyde is definately reacting with the presious benzaldehyde thats fored in the reaction with cinnamon oil in boiling water with ph 12
as illustrated in point 2)
http://web.pdx.edu/~wamserc/CH332W97/homework/H11ans.htm
Asking questions is the best way to understand anything.
|
|
|
jsc
Hazard to Self
Posts: 65
Registered: 16-3-2011
Member Is Offline
Mood: No Mood
|
|
What are you, some kind of almond freak?
Why can't you be a normal kid and make explosives?
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
