Heating a still charge at 100% reflux to boost esterification?

[PLAYMP]

I’m going down a bit of an esterification rabbit hole in preparation for an upcoming rum project. I’ve made a number of other spirits to date, AG, Brandy, neutrals, Botanical spirits, etc so it feels weird I’ve never seriously tried rum but alas.

A commercial distiller (but former moonshiner) I follow mentioned something interesting in this video:



Specifically how “cuts” in a commercial setting don’t really scale from the types of small rigs us home distillers we work with. One of the things he mentioned was time under heat leading to esterification that cuts down on the amount of heads they collect. I’m not even super sure there’s much too that and I know there’s a million reasons the commercial guys will take wider cuts but it did get me thinking, because heat is certainly instrumental in esterification and that led me back to high school chemistry class, summed up here:

https://scienceready.com.au/pages/ester ... 0flammable.

In this reaction they are heating their “charge” to 140-180 degrees at full reflux.

So it leads me to my question. Might there be any benefit to a period of “deliberate esterification” prior to distillation where the still holds temp at 140-180 at full reflux (not necessarily with packing/plates). If ester formation can occur post-distillation as part of aging, can any of that be cleaned up in the still through this step and potentially even shorten the aging time for us home distillers?

[30xs]

Check out the “butter rum” thread.

[NZChris]

I do it. Make sure you have the required precursors in the still.

[PLAYMP]

I do it. Make sure you have the required precursors in the still.

Amazing. Do you hold it for a set amount of time?

Edit: and to add have you thought about how this practice might lead to cutting down on the aging time of your spirits? Or are those totally independent things?

[NZChris]

At least an hour when stripping, longer if I have a still loaded with precursors, lime salts, acid, etc., for a spirit run.

I don't use a reflux still for making rum.

[shadylane]

Just my humble drunken opinion.

Big words like esterification can be misleading.
I don't like what happens when yeast is boiled for an extended time.

Also, as the commercial distiller on the video pointed out.
Hobby sized distilling doesn't always scale down.
What we get after cuts, is what it is.
Not what some formula or percentage he thought it should be.

[NZChris]

I haven't watched the YouTube that you posted, but the shiny SS bling behind him isn't a good indication that he knows his stuff. YouTube and forums are great places to get ideas from, but you really need to do due diligence before investing a lot of time and effort and money into equipment and ingredients before using advice from those sources.

[Demy]

I've only had a few rum runs so I don't know much about it, what I do with spirits like that is a slow warm up of the boiler charge....always beneficial in grain based spirits in general too.

[Yummyrum]

Just my humble drunken opinion.

Big words like esterification can be misleading.
I don't like what happens when yeast is boiled for an extended time.

Easy Shady , run your wash through one of these bad boys and esterfy away

https://www.gea.com/en/products/centrif ... xtract.jsp

[NZChris]

I've only had a few rum runs so I don't know much about it, what I do with spirits like that is a slow warm up of the boiler charge....always beneficial in grain based spirits in general too.

Using high powered elements to save on heat up time isn't always the best option, especially for flavored products. I have two elements, but mostly use both on full power when heating a sugar wash neutral up to stripping temperature.

[Saltbush Bill]

Interesting bits that I picked up on watching that were the part from 7.11 to 7.34, were he talks about rubbing the spirit between your hands to cause friction, Ive done it that way for years .......I find it really helps to intensify the different smells that are coming off the spirit.....particularity for smelling out very early tails.
Also the part at around 8.25 where he talks about recycling heads and how or if the different components build up over time.

[googe]

I've tried long and short time prior to distillation and the difference is so minimal its not worth it. The thing about holding vapors in large open copper column has always interested me though, hard to do on hobby level.

[Bradster68]

I now do slow heat ups for both spirit and strip for my bourbons and rums. Just started doing this, so we'll see

[bunny]

In this reaction they are heating their “charge” to 140-180 degrees at full reflux.

So it leads me to my question. Might there be any benefit to a period of “deliberate esterification” prior to distillation where the still holds temp at 140-180 at full reflux (not necessarily with packing/plates).

Just curious:
What does full reflux look like at 140-180*?

I usually only get a stray drop or two coming over below 180*, nothing that looks like a volume I would consider full reflux. Or is this what you are talking about?

[PLAYMP]

Just curious:
What does full reflux look like at 140-180*?

I usually only get a stray drop or two coming over below 180*, nothing that looks like a volume I would consider full reflux. Or is this what you are talking about?

I guess when I say reflux I mean "capping the boiler with a condenser" so I don't lose any vapor at that stage. I don't know really know what will get condensed at 140-180 or what kind of volume I could possibly expect (probably small). Out of my sight glass I'll certainly see vapor coming off the liquid as early as the lower end of that range I'm pretty sure. I've also stopped my controller around 180 just to warm things up before a run and if I come back 10 minutes later the whole rig including condenser will be hot, so I think it's safe to assume at least some vapor is capable of travelling a good amount of distance at those temps.

It's a little confusing because when we think reflux we're thinking plates and packing and reflux ratio and the like but if I understand the article I linked to it's purely just so we don't lose any of the contents of the boiler before and after the reaction.

[NZChris]

Run your hand up the riser. If it's hot at the bottom and little to nothing is coming over, it's about right. I know approximately how many Watts that takes, so can set the power to hold it in full reflux.

Note that Googe didn't notice much difference. If you don't have the precursors present in the wash or Low Wines, there is not much to be gained. Commercial distillers, when making high ester rums, use trickery to make sure that everything needed is in the pot or retort.

[Yummyrum]

When they make Esters at work ,they put acid and alcohol in a flask and put a reflux condenser on it . Then they boil the crap out if it . It is as you say PLAYMP simply to keep it all in the boiler while the reaction is taking place .

Now they make all sorts of fruity esters . I’m not sure what the advantage is between boiling and just holding a lower temp before boiling . But certainly boiling does produce Esters .

Maybe doing it at a lower temp for longer prevents the yeast issues Shady suggested .

[Tōtōchtin]

Just my humble drunken opinion.

Big words like esterification can be misleading.
I don't like what happens when yeast is boiled for an extended time.

Shady what happens to the yeast left in the wash?
Tōtō

[Tōtōchtin]

Run your hand up the riser. If it's hot at the bottom and little to nothing is coming over, it's about right. I know approximately how many Watts that takes, so can set the power to hold it in full reflux.

Note that Googe didn't notice much difference. If you don't have the precursors present in the wash or Low Wines, there is not much to be gained. Commercial distillers, when making high ester rums, use trickery to make sure that everything needed is in the pot or retort.

NZChris do you that a thread where you describe one of your heavy rum runs? It's too much to go through 12000 posts of your's.

[shadylane]

Shady what happens to the yeast left in the wash?
Tōtō

Peppery cardboard tails.

[HDNB]

i heat my still the day before a run and leave it overnight for this very reason. does it work? dunno, but my whisky is pretty popular.

side benefit, heat up time is reduced on day of, so the run goes faster and easier.

[Tōtōchtin]

Shady what happens to the yeast left in the wash?
Tōtō

Peppery cardboard tails.

I can do without that, thank you. Is that is most washes and mash in general, or for rum washes?
Tōtō

[shadylane]

Just my opinion.
All sugar washes, that includes Rum.
Get rid of some the spent yeast before distilling and wider cuts are possible.
For Rum, that means the funky esters you want to save aren't polluted with cardboard tails.

[Saltbush Bill]

If you let a Rum wash settle properly , you shouldn't get any yeast in the boiler, or if you do its so little that it wont matter.
Build your fermenting vessels so that the tap for drawing off finished wash is an inch up from the bottom.

[NZChris]

NZChris do you that a thread where you describe one of your heavy rum runs? It's too much to go through 12000 posts of your's.

No, it's not that simple and I'm still learning. Every series of rums I do is different and makes use of what I have learned since the last one, what I have available at the time, how well the ferments go etc.. When I need to know more, I search the documents I've downloaded while scouring the web for more info.

When you're new at the game and haven't got much in the drinks cabinet, you should be aiming to make simple products that are ready to drink without years of aging. High ester rums are probably best left until you have something to drink while it ages.

Meanwhile, don't discard the feints from your rums, save them for future rum experiments.

[shadylane]

[Texas Jim]

Run your hand up the riser. If it's hot at the bottom and little to nothing is coming over, it's about right. I know approximately how many Watts that takes, so can set the power to hold it in full reflux.

Note that Googe didn't notice much difference. If you don't have the precursors present in the wash or Low Wines, there is not much to be gained. Commercial distillers, when making high ester rums, use trickery to make sure that everything needed is in the pot or retort.

What are the necessary precursors?

[PLAYMP]

i heat my still the day before a run and leave it overnight for this very reason. does it work? dunno, but my whisky is pretty popular.

side benefit, heat up time is reduced on day of, so the run goes faster and easier.

Funny enough I actually am realizing that I also preheat things. I usually get heated up in the morning before work then insulate so I can get right into my run in the evening after my daughter goes to bed.

[HDNB]

What are the necessary precursors?

long chain fatty acids and alcohol. heat hastens the process, as in most chemical reactions.

that's my limit, from here you need a biochemist.

[NZChris]

Run your hand up the riser. If it's hot at the bottom and little to nothing is coming over, it's about right. I know approximately how many Watts that takes, so can set the power to hold it in full reflux.

Note that Googe didn't notice much difference. If you don't have the precursors present in the wash or Low Wines, there is not much to be gained. Commercial distillers, when making high ester rums, use trickery to make sure that everything needed is in the pot or retort.

What are the necessary precursors?

There is a simple description here on page 429. Download it, links can disappear.
https://iiif.wellcomecollection.org/pdf/b21537379