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Author: Subject: extracting oil from large amounts of bark/woodchip
BILLBUILDS
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[*] posted on 31-1-2017 at 18:17
extracting oil from large amounts of bark/woodchip


I was just hoping to get advice on extracting essential oil from a large amount of bark (camphor laurel).

options:

-have a 50-200L still custom fabricated by a local company for relatively cheap (already sent out some enquiries)

-buy a still from a specialty company for a relatively massive price
steam distill using glassware

-boil it up with a relatively small amount of water in a 24L pressure cooker (i have one already) and then use a separatory funnel to extract the oil

-solvent extraction using a cheap solvent (methylated spirits ect) and recover the solvent

-Using a Soxhlet extractor. This would includePowdering the bark and then using a soxhlet to extract the oil would significantly reduce the volume of solvent needed but also massively increase the time needed to dry the bark, powder the bark (how do i do this? i already broke the blender by doing this previously), and much smaller extraction runs

any other suggestions?

im going to need to process a large volume of material since most materials contain around 0.5-2% oil so to get 1Kg of oil from a product contain 1% oil ill need to process over 100kg of material and using a 2L flask just does not seem feasible

anyhow ill do some experiments in the meantime and let you know how it goes.

Also

I've ordered a 1L soxhlet extractor and have the glass to set up a steam distillation setup as well. I also might try the pressure cooker although a piece is missing from it which will allow steam to escape
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[*] posted on 31-1-2017 at 18:34


I am interested in this too.
My town has a large number of camphor laurels and there is a big one in front of my house. I was going to target the leaves rather than the bark. I figured that I would get camphor rather than an essential oil but I might be mistaken there.

I have ordered a soxhlet also which I was going to fill with dry crushed leaves. I have not yet decided on a solvent to use.
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RogueRose
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[*] posted on 31-1-2017 at 18:45


I would go with what you have and try the pressure cooker. IDK what size the chips are but I would think that grinding them with something like a leaf shredder might give better yeilds. If the leaf shredder isn't strong enough it might work better if they were pressure cooked first and then shredded while hot and still moist - or maybe steamed first then shredded.

I think the pressure would help remove the oils better and the higher temp is usually a good thing but I'm not sure the temp will be high enough to melt camphor but if there are essential oils that might be freed at those temps and pressure.
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Sulaiman
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[*] posted on 31-1-2017 at 19:49


there is an old article https://todayinsci.com/D/Duncan_Robert/DuncanRobert-Camphor....
(complete book here https://archive.org/details/somechemicalpro00duncgoog )
in which it gives camphor content;
Wood, 0.61% of Crude Camphor
Twigs, 1.05% of Crude Camphor
Green Leaves, 2.37% of Crude Camphor;
Dried Leaves, 2.52% of Crude Camphor
Dead Leaves, 1.39% of Crude Camphor

and there is a drawing of a japanese camphor still,
and more significantly, mention of a US Agricultural Department at Washington still design.




CAUTION : Hobby Chemist, not Professional or even Amateur
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[*] posted on 31-1-2017 at 21:24


Cool. I wondered if you would chime in, Sulaiman.
The trees drop small branches regularly and the leaves dry out pretty quickly. When you crush them there is a strong smell. I figured dried/dead would be best since there is less chance of collecting the chlorophyll and other pigments with the camphor.

According to those figures, I am well served to go with my current plan of collecting some tree-fall branches while they are green and letting them dry out. Then I can strip the leaves and crush them up. The leaves crush to a flaky powdery substance easily.

I would guess that the product gained by starting with bark and wood would be quite a bit different.
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JJay
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[*] posted on 31-1-2017 at 21:41


I think I would go with the pressure cooker too. There are a few papers comparing the results of steam distillation and Soxhlet extraction on similar species. There are certainly tradeoffs, but most people have better luck extracting oils with steam distillation. In addition, you can load perhaps several kilograms at a time into a pressure cooker, and it would take a very large Soxhlet to handle more than a hundred grams or so at once.





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ziqquratu
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[*] posted on 31-1-2017 at 21:58


Large-scale steam distillation isn't too hard. You just need a system which allows you to add water as needed, whilst being sealed well enough to avoid loss of steam (and some system for condensing the distillate, of course).

I saw, many years ago, an article where someone used a 44 gallon drum, with a tap on the side to add water as needed and some tubing attached into the lid for a condenser (copper, I think - but that's just a vague memory, and I can't find it now). I remember they showed photos where they did steam distillation of basically a whole Christmas tree in there...

I *did* find this in whilst searching for the page I remember: http://www.instructables.com/id/Build-Your-Own-Essential-Oil... They use a turkey fryer pot, with a perforated steel insert. Might give you some ideas.
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Amos
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[*] posted on 1-2-2017 at 12:26


Any intent on separating the oil into its components? Sounds like a reasonable way to get a fair quantity of safrole.

[Edited on 2-1-2017 by Amos]
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JJay
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[*] posted on 1-2-2017 at 12:38


Safrole is only a minor constituent of raw camphor oil, comprising a few percent.



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[*] posted on 2-2-2017 at 01:44


They are both the same article

i plan to use the safrole to make pipronal butoxide so that i can extract more camphor without the expected leeches (;)

well i put the bark out to dry and it rained for two days so i got a cleaver and split it as thin as possible before breaking into chips. i put about 20L of the smallest bits in with boiling water (whilst i also did an extraction of CCl2H2 from paint stripper) and im going to leave them to leave them for a week. the batch im doing now is 70% root bark and the remaining bark ive got is just trunk bark which takes longer to walk to the tree than to strip it. a 1m^2 area weighs about 20kg. of course only do this in your local bushland, you will be arrested/finned for stripping trees along the street. alternately you could strip the street trees of the bark and then ask the council for the wood when they spend tens of thousands cutting it down and chipping it up.

ive found the best way to extract material is to get a hunting knife (with a rounded front edge for skinning) and use it to pry off the bark. i collected 10kg of bark in as many minutes. i dont feel bad for taking the bark as they are a massive pest and are taking over the local bushland. an extra tip, follow the creeks and steams and you can extract the root bark without having to dig up any holes. you can use bug spray but then the leaches just end up in your but crack (thats not a joke) - just have a shower and take the leaches off after each expedition.

My solhex extractor and rest of steam extraction equipment will arrive soon so ill update when i do more experimenting. i might trying adding 10% ethanoic acetate to the boiled bark as it might help with extraction and i wont be too fussed if i cant recover it. ill post some pictures soon
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[*] posted on 2-2-2017 at 01:51


Quote: Originally posted by JJay  
Safrole is only a minor constituent of raw camphor oil, comprising a few percent.


actually its ~50% of the essential oil. there are something like 12 chemotypes which have characteristic oils some with none some with 90%. luckily australia only has 2 cchemotypes from the research ive from all the reading ive done there is no way to tell other than experience but just take bark from a selection of trees and your bount to hit some gold
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JJay
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[*] posted on 2-2-2017 at 02:02


Quote: Originally posted by BILLBUILDS  
Quote: Originally posted by JJay  
Safrole is only a minor constituent of raw camphor oil, comprising a few percent.


actually its ~50% of the essential oil. there are something like 12 chemotypes which have characteristic oils some with none some with 90%. luckily australia only has 2 cchemotypes from the research ive from all the reading ive done there is no way to tell other than experience but just take bark from a selection of trees and your bount to hit some gold


I don't believe that is the case - do you have a source to cite?




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Corrosive Joeseph
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[*] posted on 2-2-2017 at 02:10


Snippets -

https://erowid.org/archive/rhodium/chemistry/safrolefaq.html




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JJay
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[*] posted on 2-2-2017 at 02:45


I think that source is questionable. It's true that there exists a distillate called "brown camphor oil" which is derived from Cinnamomum camphora, but it's a refined product comprising something like 20% of the raw essential oil. Typical values for brown camphor oil's safrole concentration are more like 10-30%, AFAIK, but it could be up to 100% safrole if sufficiently refined... of course it would require a great deal of raw essential oil to produce such a product, and most people wouldn't have the licenses required for handling it.

[Edited on 2-2-2017 by JJay]




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[*] posted on 2-2-2017 at 22:59


these are just the ones on my computer. thers many more

Quote:

GCˆGC-TOFMS Analysis of Essential Oils Composition from Leaves, Twigs and Seeds of Cinnamomum camphora L. Presl and Their Insecticidal and Repellent Activities
Hao Jiang 1,2,3,†, Jin Wang 2,*,†, Li Song 2, Xianshuang Cao 2, Xi Yao 2, Feng Tang 2 and Yongde Yue 2,*
1 2
3
*

College of Plant Protection, Anhui Agricultural University, Hefei 230036, China; ahjh88@163.com
SFA Key Laboratory of Bamboo and Rattan Science and Technology,
International Centre for Bamboo and Rattan, No. 8 Futong Dongdajie, Wangjing, Chaoyang District, Beijing 100102, China; songliicbr@163.com (L.S.); caoxianshuang123@163.com (X.C.); yaoxi@icbr.ac.cn (X.Y.); fengtang@icbr.ac.cn (F.T.)
State Key Laboratory of Tea Plant Biology and Utilization, Anhui Agricultural University, Hefei 230036, China
Correspondence: wangjin@icbr.ac.cn (J.W.); yueyd@icbr.ac.cn (Y.Y.);
Tel.: +86-10-8478-9818 (J.W.); +86-10-8471-3741 (Y.Y.)
These authors contributed equally to this work.


Sesquiterpenoids Sesquiterpenoids
in the Leaf Oil of Camphor Trees. II.
of Safrole
Trees1) and Sesquiterpene Trees1)
Mitsuru HIROI
Departmenotf ChemistryF,acultyof Literatureand ScienceE,himeUniversityM, atsuyama
(ReceivedMarch8, 1967)

To cite this article: Pham Van Khiên , Hô Trung Chiên , Nguyên Xuân Dung , Antoine X. Leclercq & Piet A. Leclercq (1998) Chemical Segregation of Progeny of Camphor Trees with High Camphor c.q. Linalool Content, Journal of Essential Oil Research, 10:6, 607-612, DOI: 10.1080/10412905.1998.9700987

Mitsuo Miyazawa , Yuya Hashimoto , Yasuo Taniguchi & Kouji Kubota (2001) Headspace Constituents of the Tree Remain of Cinnamomum camphora , Natural Product Letters, 15:1, 63-69, DOI: 10.1080/10575630108041259

Joseph J. Brophy , Robert J. Goldsack & Paul I. Forster (2001) The Leaf Oils of the Australian Species of Cinnamomum (Lauraceae), Journal of Essential Oil Research, 13:5, 332-335, DOI: 10.1080/10412905.2001.9712225

The Essential Oil of Cinnamomum camphora (L.) Nees and Eberm.—Variation in Oil Composition Throughout...
Article in Journal of Essential Oil Research · May 2004

Saviour to Scourge: a history of the introduction and spread of the camphor tree (Cinnamomum camphora) in eastern Australia
Brett J. Stubbs
School of Environmental Science and Management, Southern Cross University, Lismore, NSW 2480

A Comparative Study on the Anatomy and Development of Different Shapes of Domatia in Cinnamomum camphora (Lauraceae)
SACHIKO NISHIDA1,*, HIROKAZU TSUKAYA2,†, HIDETOSHI NAGAMASU3 and MASUMI NOZAKI1
1The Nagoya University Museum, Furo-cho, Chikusa-ku, Nagoya, 464-8601, Japan, 2National Institute for Basic Biology, Okazaki Institute for Integrated Bioscience, Myodaiji-cho, Okazaki, 444-8585, Japan and 3The Kyoto University Museum, Kyoto, 606-8501, Japan

Brett J. Stubbs & Don Brushett (2001) Leaf Oil of Cinnamomum camphors (L.) Nees and Eberm. from Eastern Australia, Journal of Essential Oil Research, 13:1, 51-54, DOI: 10.1080/10412905.2001.9699604

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JJay
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[*] posted on 2-2-2017 at 23:10


I didn't read through every one of these, but I'm not seeing one that says that a large percentage of the essential oil derived from camphor laurels is safrole.



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[*] posted on 3-2-2017 at 06:37


results so far

bark


outter bark


inner bark


side on view


some chips from yesterday i boiled today


pressure cooker


some water from the boil is that a slight oil layer or just a miniscus


tools needed



the seperated outter and inner bark


yesterdays boiled and then pulped mixture
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[*] posted on 10-2-2017 at 16:59


Ok so update. i now have around 200L of a dark brown/caramel coloured liquor.
I am now planning on using a 2L separating funnel to go through the liquor litre by litre, ill probably grab a few bags of cheap salt to help with separation.
I will first do it normally (water-oil separation) but something tells me that that i will have a hydrosol rater than a two phase liquid. so....
Then ill then separate again with a non miscible solvent (probably 50-100ml per 100ml) and then pool all the solvents and remove them via distillation

Can anyone recommend a good solvent? i have around 600ml of CCl2H2 which i separated from paint thinner (and another 4L of paint thinner 870 methelyene chloride/130 methanol which needs separating first). I also have 6L toluene, 1L xylene both of which i can buy more of if you think they will work best. 4L Ethyl acetate which im thinking as my best option as its cheap and dosent have to many other uses. also 10L mentholated spirits, 5L methanol, 5L ethanol, 5L acetone, 5L Methyl-iso-buty-ketone, 1L methyl-ethyl-ketone, 5L isopropyl alcohol, 5L petroleum spirit (naptha, low BP)

go for the methylene chloride which will be easiest to remove but costs alot more or ethyl acetate which is cheap and a bit harder to remove (also adds perfume notes to the final product) or toluene which is a bit more expensive and a bit harder to remove.

thoughts
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Dan Vizine
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[*] posted on 15-2-2017 at 14:09



I'd use the methylene chloride. Just don't assume it's the "non-toxic" version of chloroform. It's just less toxic. If you can't...

Ohhhhh.....saffrole. I was asking myself why anyone would want to work at this scale unless they had an objective in mind. And a few % is about the best you're going to find in easily available plants. At least you didn't just join the forum the same day you posted this. Now THAT would look suspicious.




[Edited on 2/15/2017 by Dan Vizine]





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[*] posted on 25-3-2017 at 13:03


ok so that whole experiment was a huge failure. i tried extracting 800ml with 100ml of methylene chloride and obtained nothing. also just putting batches though a sep funnel didnt work. i should of used the same water to boil each batch of bark.


ok so now im trying a different method. ground up leaves through simple /watere steamdistilationg. its amazing how much camphor there is, after just 3 runs my condensor (anlin) was caked solid with camphor to the point where i had to undo my aparatus and extract the condensor with ethanol - there were BIG chunks of it. ill let you know the final result
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JJay
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[*] posted on 25-3-2017 at 14:51




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[*] posted on 26-3-2017 at 19:15


ok i need some advice. i had about 40g of camphor in methanol yesterday and apparently its also ethanol volatile. i got another 40g of camphor in ethanol and i was thinking of just drumping the crystals out by adding a heap of water then filtering. would this work?
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[*] posted on 26-3-2017 at 20:50


You might do an experiment with a small amount in a test tube.



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[*] posted on 27-3-2017 at 11:17


ok i need some advice. i had about 40g of camphor in methanol yesterday and apparently its also ethanol volatile. i got another 40g of camphor in ethanol and i was thinking of just drumping the crystals out by adding a heap of water then filtering. would this work?
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