EXTRACTION METHODS USING SUPERCRITICAL FLUIDS

    EXTRACTION METHODS USING SUPERCRITICAL FLUIDS

    post #1 of 9
    Thread Starter 

    Hello everyone,

    I'm new to the forum, I would like to know if anybody knows about Mane's Jungle Essence method of extraction, see below

    http://www.mane.com/jungle-essence

    They seem to use a quite safe supercritical gas that does not need much equipment. Anybody knows what gas that is? I'm studying the butane extraction method, like Butaflor from Robertet, but it seems a bit difficoult and more Dangerous, although not impossible for a DIY perfumer... I belive that using CO2 is still not so much accessible for minor companies or single perfumers to use on their own! Please help me out! Any suggestion on other gases that i could use as a solvent!?

    post #2 of 9
    Thread Starter 

    by the way, do you people think that a butane extraction could also extract fresh fruits notes as the Jungle essence method does????

    post #3 of 9

    Hi Vincent, I have some experience in this field so I'll try to answer your questions as best I can. From watching the video clip that you posted, I can tell you that the extraction vessel is similar to a Dewar flask or Thermos, in that it has a double wall to insulate the liquid gas. The main difference is that they've added a valve at the top, which will keep the liquid gas under pressure. Whether or not this is enough pressure for it to be in a supercritical state is a different issue. I would suspect not, despite their claims. Supercritical liquids have the ability to penetrate solids more like a gas would and they can therefore extract cellular contents more easily. Some Dewar flasks are designed to hold liquid gases under high pressure. It would be possible to adapt a Thermos to perform in a similar manor but you'd need to have some engineering experience.

     

    Butane is a good solvent to use because it's highly non polar and it therefore leaves behind most of the unwanted cell contents. It will extract waxes and fats but a secondary extraction with something like ethanol will remove them. This is what the secondary solvent extraction mentioned in the video is addressing. The primary extract would be called a concrete and the secondary extract an absolute.

     

    CO2 extraction is beyond the reach of most amateur perfumers because of the high pressures involved and the equipment needed. You can, however, do butane extractions with some fairly basic equipment and a little know-how. If you'd like to know more, you can read about the Thermos method below. I've been using this, along with other methods since 2006 and it works well.

     

    http://www.basenotes.net/t/320423/making-an-absolute-process-lessons-learned-and-recommendations#post_2823442

     

    http://www.basenotes.net/t/320423/making-an-absolute-process-lessons-learned-and-recommendations#post_2826263

     

    Pears


    Edited by Pears - 9/14/13 at 9:54am
    post #4 of 9
    Quote:
    Originally Posted by Vincent81 View Post
     

    by the way, do you people think that a butane extraction could also extract fresh fruits notes as the Jungle essence method does????

     

    Yes, it would. The only issue is that liquid gases freeze fresh plant materials solid and you therefore ideally need the liquid gas to be under pressure, so that it can penetrate the frozen cells more easily. If the butane isn't under pressure it will still extract some of the frozen cellular contents but not as efficiently as butane that's under pressure. However, if the plant materials that are selected contain most of their odorous material within the external cuticles or trichomes, they will be extracted very efficiently, regardless of whether the butane is under pressure or not. Thyme would be a good example, containing much of it's essential oil in the external trichomes. Also, if the plant material is dried, the butane will penetrate the cells relatively easily, even if it's not under pressure.


    Edited by Pears - 9/15/13 at 1:47am
    post #5 of 9
    Thread Starter 

    Thank you guys for quik answers!!!

    What I really do not understand is if there are other gases available to use that are a bit safer than butane! Do you belive that Butane would extract the essence of a fig or of a pineapple for example?

    I have found out that some ready made extractors are sold, but they're very expensive for the small capacity of raw materials they contain!

     

    http://www.youtube.com/watch?v=ZKwXDLkkio4

     

    Would this extractor maintain the supercritical state of the butane?

    By the way, Pears, I have found a 70 L thermos that I was thinking of adapting, How long should a delicate material like Jasmine flowers remain soaked in Butane? My few experiments extracting have been maybe too short...

    thank you again!

     

    Vincent.

    post #6 of 9

    Hi Vincent, if when you say safe you mean inflammable, there are many refrigerant gases that are inflammable and that can be used for extraction purposes. Hydrofluorocarbons (HFCs) are used for this purpose but it's illegal to knowingly vent some of them into the atmosphere. It might be a good idea to contact the makers of Jungle Essence to find out which gas it is that they use. It may be R-134a, which is inert and doesn't harm the ozone layer. It's one of the more commonly used HFCs for extraction purposes. As you know, Butaflors are made with butane. Extracts made with HFCs are called Florasols. They actually call both the extracts and the HFCs themselves Florasols, infact.

     

    To be honest, I'd forget about supercritical extraction if I were you. N-butane's critical point is 152 °C. You'd destroy the more heat sensitive aroma compounds at that temperature. Not only that but you'd need a heavy duty tank to withstand the pressure. I'd suggest that the makers of Jungle Essence are actually being a little dishonest. To my knowledge there aren't any liquid gases that have a critical point anywhere near room temperature and at "low pressure". Even R-134a has a critical point of 101 °C. The gases with critical points even close to room temperature, have vapor pressures far too high for them to be contained within the canister shown within the video. A heavy duty tank would be required to withstand the pressures involved.

     

    That's not to say that a solvent in a closed system, under relatively low pressure wouldn't still extract more efficiently than if it were in an open vessel. It would but not as efficiently as if it were supercritical. Closed systems tend to be expensive and most people lack the engineering experience to safely make their own. A Thermos is a practical and affordable alternative for the amateur perfumer.

     

    I haven't extracted from fruit before, so you'll have to try it for yourself. I'd recommend that you use a Thermos to begin with, before investing heaviliy in a closed system. If the fruit smells extremely bland after extraction (upon returning to ambient temperature and being freshly cut), then you know that it's been extracted thoroughly enough. I hope that this was helpful.

     

    Pears


    Edited by Pears - 9/15/13 at 4:46am
    post #7 of 9

    Extracting limonene using liquid carbon dioxide

    http://www.youtube.com/watch?v=o2aIUemy9Xw

     

    It's fairly safe, provided you use a deformable container or incorporate a pressure relief valve in your vessel.

     

    -

    post #8 of 9

    That's a nice demonstration, Skelly. CO2 is one such solvent that will enter a supecritical state with the additional of very little heat. It's critical temperature is 31 °C. For small amounts you can get away with using a plastic test tube but if it's a large amount, you really need to use a gas tank or a high pressure autoclave.


    Edited by Pears - 9/16/13 at 1:27am
    post #9 of 9

    CO2 liquifies at about 12 bar, and normal operating pressure is 15 bar.  A couple of cylinders connected with a suitable hose should work.  Put your material in the lower bottle, liquid CO2 in the top, and equalise gas pressure, then decant into the LB (drop the pressure by a bar or so in the LB to help) Let the CO2 do its stuff then blow it down (I haven't worked how you'd stop your extract from going with it)

     

    I used to move tonnes of the stuff from tank to tank.  It's not difficult.  A competent engineering hobbyist should be able to make a suitable rig.

     

    Edit:  The big (20+tonne) static tanks have fridge units to keep it at 15 bar.  I can't remember the pressure in an un-refridgerated welding bottle sized tank.  Probably somewhat higher.

     

    -

    class="

    9/14/13 at 7:22am

    Vincent81 said:



    Hello everyone,

    I'm new to the forum, I would like to know if anybody knows about Mane's Jungle Essence method of extraction, see below

    http://www.mane.com/jungle-essence

    They seem to use a quite safe supercritical gas that does not need much equipment. Anybody knows what gas that is? I'm studying the butane extraction method, like Butaflor from Robertet, but it seems a bit difficoult and more Dangerous, although not impossible for a DIY perfumer... I belive that using CO2 is still not so much accessible for minor companies or single perfumers to use on their own! Please help me out! Any suggestion on other gases that i could use as a solvent!?

    9/14/13 at 7:23am

    Vincent81 said:



    by the way, do you people think that a butane extraction could also extract fresh fruits notes as the Jungle essence method does????

    9/14/13 at 8:48am

    Pears said:



    Hi Vincent, I have some experience in this field so I'll try to answer your questions as best I can. From watching the video clip that you posted, I can tell you that the extraction vessel is similar to a Dewar flask or Thermos, in that it has a double wall to insulate the liquid gas. The main difference is that they've added a valve at the top, which will keep the liquid gas under pressure. Whether or not this is enough pressure for it to be in a supercritical state is a different issue. I would suspect not, despite their claims. Supercritical liquids have the ability to penetrate solids more like a gas would and they can therefore extract cellular contents more easily. Some Dewar flasks are designed to hold liquid gases under high pressure. It would be possible to adapt a Thermos to perform in a similar manor but you'd need to have some engineering experience.

     

    Butane is a good solvent to use because it's highly non polar and it therefore leaves behind most of the unwanted cell contents. It will extract waxes and fats but a secondary extraction with something like ethanol will remove them. This is what the secondary solvent extraction mentioned in the video is addressing. The primary extract would be called a concrete and the secondary extract an absolute.

     

    CO2 extraction is beyond the reach of most amateur perfumers because of the high pressures involved and the equipment needed. You can, however, do butane extractions with some fairly basic equipment and a little know-how. If you'd like to know more, you can read about the Thermos method below. I've been using this, along with other methods since 2006 and it works well.

     

    http://www.basenotes.net/t/320423/making-an-absolute-process-lessons-learned-and-recommendations#post_2823442

     

    http://www.basenotes.net/t/320423/making-an-absolute-process-lessons-learned-and-recommendations#post_2826263

     

    Pears


    Edited by Pears - 9/14/13 at 9:54am

    9/14/13 at 9:20am

    Pears said:



    Quote:
    Originally Posted by Vincent81 View Post
     

    by the way, do you people think that a butane extraction could also extract fresh fruits notes as the Jungle essence method does????

     

    Yes, it would. The only issue is that liquid gases freeze fresh plant materials solid and you therefore ideally need the liquid gas to be under pressure, so that it can penetrate the frozen cells more easily. If the butane isn't under pressure it will still extract some of the frozen cellular contents but not as efficiently as butane that's under pressure. However, if the plant materials that are selected contain most of their odorous material within the external cuticles or trichomes, they will be extracted very efficiently, regardless of whether the butane is under pressure or not. Thyme would be a good example, containing much of it's essential oil in the external trichomes. Also, if the plant material is dried, the butane will penetrate the cells relatively easily, even if it's not under pressure.


    Edited by Pears - 9/15/13 at 1:47am

    9/14/13 at 9:46am

    Vincent81 said:



    Thank you guys for quik answers!!!

    What I really do not understand is if there are other gases available to use that are a bit safer than butane! Do you belive that Butane would extract the essence of a fig or of a pineapple for example?

    I have found out that some ready made extractors are sold, but they're very expensive for the small capacity of raw materials they contain!

     

    http://www.youtube.com/watch?v=ZKwXDLkkio4

     

    Would this extractor maintain the supercritical state of the butane?

    By the way, Pears, I have found a 70 L thermos that I was thinking of adapting, How long should a delicate material like Jasmine flowers remain soaked in Butane? My few experiments extracting have been maybe too short...

    thank you again!

     

    Vincent.

    9/14/13 at 4:43pm

    Pears said:



    Hi Vincent, if when you say safe you mean inflammable, there are many refrigerant gases that are inflammable and that can be used for extraction purposes. Hydrofluorocarbons (HFCs) are used for this purpose but it's illegal to knowingly vent some of them into the atmosphere. It might be a good idea to contact the makers of Jungle Essence to find out which gas it is that they use. It may be R-134a, which is inert and doesn't harm the ozone layer. It's one of the more commonly used HFCs for extraction purposes. As you know, Butaflors are made with butane. Extracts made with HFCs are called Florasols. They actually call both the extracts and the HFCs themselves Florasols, infact.

     

    To be honest, I'd forget about supercritical extraction if I were you. N-butane's critical point is 152 °C. You'd destroy the more heat sensitive aroma compounds at that temperature. Not only that but you'd need a heavy duty tank to withstand the pressure. I'd suggest that the makers of Jungle Essence are actually being a little dishonest. To my knowledge there aren't any liquid gases that have a critical point anywhere near room temperature and at "low pressure". Even R-134a has a critical point of 101 °C. The gases with critical points even close to room temperature, have vapor pressures far too high for them to be contained within the canister shown within the video. A heavy duty tank would be required to withstand the pressures involved.

     

    That's not to say that a solvent in a closed system, under relatively low pressure wouldn't still extract more efficiently than if it were in an open vessel. It would but not as efficiently as if it were supercritical. Closed systems tend to be expensive and most people lack the engineering experience to safely make their own. A Thermos is a practical and affordable alternative for the amateur perfumer.

     

    I haven't extracted from fruit before, so you'll have to try it for yourself. I'd recommend that you use a Thermos to begin with, before investing heaviliy in a closed system. If the fruit smells extremely bland after extraction (upon returning to ambient temperature and being freshly cut), then you know that it's been extracted thoroughly enough. I hope that this was helpful.

     

    Pears


    Edited by Pears - 9/15/13 at 4:46am

    9/15/13 at 9:14am

    Skelly said:



    Extracting limonene using liquid carbon dioxide

    http://www.youtube.com/watch?v=o2aIUemy9Xw

     

    It's fairly safe, provided you use a deformable container or incorporate a pressure relief valve in your vessel.

     

    -

    9/15/13 at 5:56pm

    Pears said:



    That's a nice demonstration, Skelly. CO2 is one such solvent that will enter a supecritical state with the additional of very little heat. It's critical temperature is 31 °C. For small amounts you can get away with using a plastic test tube but if it's a large amount, you really need to use a gas tank or a high pressure autoclave.


    Edited by Pears - 9/16/13 at 1:27am

    9/16/13 at 11:31am

    Skelly said:



    CO2 liquifies at about 12 bar, and normal operating pressure is 15 bar.  A couple of cylinders connected with a suitable hose should work.  Put your material in the lower bottle, liquid CO2 in the top, and equalise gas pressure, then decant into the LB (drop the pressure by a bar or so in the LB to help) Let the CO2 do its stuff then blow it down (I haven't worked how you'd stop your extract from going with it)

     

    I used to move tonnes of the stuff from tank to tank.  It's not difficult.  A competent engineering hobbyist should be able to make a suitable rig.

     

    Edit:  The big (20+tonne) static tanks have fridge units to keep it at 15 bar.  I can't remember the pressure in an un-refridgerated welding bottle sized tank.  Probably somewhat higher.

     

    -