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Holzbranntwein

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Holzbranntwein

Postby Kareltje » Tue Mar 06, 2018 11:56 am

On some other forum a member mentioned sawdust brandy and someone came up with this lemma:
https://en.wikipedia.org/wiki/Sawdust_brandy

It is a translation of a German lemma: https://de.wikipedia.org/wiki/Holzbranntwein

These lemmae mention making sugar out of cellulose with sulfuric acid, but the TS mentioned a recipe with hydrochloric acid.
After checking the maths, that can not be correct.
I browsed a bit on the internet and found a few links.

A broad overview of different methods to use cellulose:
http://www.theseus.fi/bitstream/handle/ ... sequence=1

Comparing experiments with hydrolysis of sawdust with acid:
http://engineeringjournals.stmjournals. ... le/449/228

Edit:
A discussion on another forum:
http://www.schnapsbrennen.at/diskussion ... 4701-01-02

And some links that I can not access fully from my home computer, but have a nice first page:

Often cited is:
https://pubs.acs.org/doi/abs/10.1021/ie50421a005

A few years more recent is:
https://pubs.acs.org/doi/abs/10.1021/ie50511a060

The second article compares different fine tunings of teh process with the conclusion that the best results are found with:
sawdust of 2 mm, 5 % hydrosulfuric acid, kept for 180 min at 100 dg C. This would result in about 70 %w/w of sugar and after fermenting the alcohol yield was about 70 %v/v.
It is not mentioned how much of the sawdust in relation with the fluid is used, but we maybe try to guestimate that.
Dry wood to be sawn contains about 10 tot 15 % water, so min 85 % dry matter. Of this dm 40 to 50 % is (hemi)cellulose and this will be converted into sugar. So if 1 kg of fluid contains 700 grams of sugar, this sugar comes from about 1490 gr of dry matter and 1750 gr wood. The 1 kg of fluid also contains about 300 gr of water and acid.
So about 1800 gr of sawdust plus 300 gr acidic water is used.
Now it is uncertain whether the 5 % acid is calculated over the whole mass or only over the water, but that can easily be tested: the difference is so large, that only one test is needed.

I am not sure about this calculation, though, as 70 % sugar can not be fermented without dilution and a yield of 70 % sugar compared with the wood also is impossible. A fermenting yield of alcohol of 70 % of the volume of the wood also seems to make little sense. The kind of still is not described, but a distillate of 70 %ABV is also unlikely.

The German wikipedia lemma clearly states that the resulting alcohol does not contain any methanol and is safe and sound to drink. It only is forbidden in Germany because of laws regarding agriculture.
Seeing the 5 % sulfuric acid this is also no problem: I have no car but just looked it up: battery acid contains 37 % H2SO4.

Anybody any comments on this?
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Re: Holzbranntwein

Postby firewater69 » Tue Mar 06, 2018 1:03 pm

I read that thread on hd, it's interesting but it seems a lot easier and safer to get the sugar from grain or a bag. But to each their own.
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Re: Holzbranntwein

Postby Y1969 » Tue Mar 06, 2018 2:30 pm

I will comment.
Hydrolysis alcohol was widely distributed in the USSR. Basically it was used as a technical one. There are a lot of literature on this subject. The above calculations will not be evaluated, I will have to read many reference books. These books are, I can send.
Omitting many scientific calculations, experimental data, and other scientific delusions, I can summarize.
a) 1 metric ton of absolutely dry aspen yields 180-200 metric liters of alcohol.
b) hydrolytic alcohol is distilled as technical, so it tastes bad, and when drinking, it is poisonous.
c) if proper rectification is carried out, then it can be brought to GOST "alpha".
d) The most promising way of hydrolysis is hydrolysis with very dilute sulfuric acid at 200 degrees Celsius and at 12-18 bar. This is obviously for the most screwed moonshakers.
---
In general, hydrolytic alcohol is a remnant of WW2. Grains are few. Potato is small. Alcohol was needed as a basis for the synthesis of rubber. For antifreeze. Well, as an incidental result - for drinking. This is from the category of synthetic gasoline by Fischer-Tropsch and other engineering solutions such as gas-generating vehicles.
By the way, in the North Korea cars on wood are still used. There is an excellent show of National Geographic "Truck on wood"
https://alter-vij.livejournal.com/220125.html
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Re: Holzbranntwein

Postby Kareltje » Tue Mar 06, 2018 7:24 pm

I tried to recalculate the results.
1 kg of wood consists of 10 % water, 40 % cellulose and 50 % dry matter.
1 kg of acid water contains 10 % of sulfuric acid.

Boiled at 100 dg C for 3 hours would result in:
2 kg of 25 % dry matter, 20 % sugar, 5 % sulfuric acid and 50 % water.

Neutralizing of the sulfuric acid to a proper pH may pose the problem of filtering.
One can filter and ferment on the filtrate of ferment on the whole wood. I have no clue of the distribution of soluble fractions over filtrate and filterrest.
As sugar is completely soluble in water, the ratio of sugar and water in the filtrate will be 20 : 50. So for proper fermenting it will have to be diluted to a SG of 1.075 to 1.080: about 20 % sugar.

If the whole wood is fermented, the mass can be filtered and distilled or be put in a thumper as such.
If the filtered mash is fermented, the result will be about 2 litres of 11 or 12 % ABV and can be distilled as such.

So indeed: 1 kg of dry wood can result in about 200 millilitres of pure alcohol.

The Ethiopian article suggests the best way is 100 dg C for 3 hours.
This can be done, while 200 dgr C and 12 to 18 bar is not possible at home. At least not my home.
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Re: Holzbranntwein

Postby Y1969 » Wed Mar 07, 2018 10:55 am

Kareltje wrote:This can be done, while 200 dgr C and 12 to 18 bar is not possible at home. At least not my home.

Why not? Pre-call rescuers, doctors, call a local TV channel, invite bloggers .... If it explodes - the top Youtube and the first band "De Telegraaf" is guaranteed. "The maker of moonshine blew up his apparatus! Mass casualties! The house is extinguished from the helicopter!". And if it does not explode, hydrolysis alcohol will be produced.
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Re: Holzbranntwein

Postby Kareltje » Wed Mar 07, 2018 5:52 pm

De Telegraaf? You know de Telegraaf? (For bystanders: De Telegraaf is the largest paper in the Netherlands, quite right wing and not very interested in telling the truth but more in making a lot of fuzz.) I never read it.

The basic recipe of making Holzbranntwein seems not very difficult or dangerous.
Today I read about a recipe with hydrochloric acid and 50 dg C heating. One of the problems is to find a container that can withstand a very acid and hot solution.

There is ample literature about making ethanol from straw of a lot of other cellulosic sources: bioethanol of the second source.
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Re: Holzbranntwein

Postby Y1969 » Thu Mar 08, 2018 2:35 am

Of course I know. Yellow newspaper. It makes me vomit. It often cites the links of European news agencies.
---
If you look in the barn, for the needs of hydrolysis, you can find only an old enamel pot. Other options are either expensive, or toxic. You can try a stainless pan. But there is a fear that it will corrode in hot acid.
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Re: Holzbranntwein

Postby Kareltje » Thu Mar 08, 2018 6:30 pm

My thoughts exactly. On both subjects. But it surprises me that someone in Moscow knows Dutch newspapers.
The end-editor of de Volkskrant has lived some time in Moscow and the former editor of the weekly magazine de Nieuwe Revu has lived in Moscow and was the editor of the Russian Playboy, if my memory serves me well.

Today I found http://www.aidic.it/cet/14/38/073.pdf , an Italian article about hydrolysis of cellulose from bagasse, the fibery part of sugar cane.
The compounds of this waste product seem to be similar to wood.
The procedure has several steps:
1) Pre-treatment: 1 % H2SO4 (w/v) in 1:10 solid:liquid at 121 dg C for 20 min, filtration, washing and drying. The dry mass is treated with 1.5 % w/v NaOH, 1:20 solid:liquid at 10 dg C for 1 hour. The mixture was filtered, washed thoroughly with water and dried.
2) The resulting cellulose and a watery H2SO4-solution were then in 1:8 solid:liquid ratio put together and heated to a high temperature for some minutes.
Depending on the variables (concentration H2SO4, time and temperature) there occured a more or less efficient hydrolysis into sugar.
The resulting sugar solution was detoxed with activated charcoal.
3) This detoxed sugary fluid was fermented with various nutrients and a specific kind of yeast.
Distilling is not mentioned.

The pre-treatment of the bagasse with H2SO4 followed by NaOH is not mentioned in the earlier found Ethiopian article.
This might be due to the raw material.
The actual hydrolysis in this article is carried out at 155 to 175 dg C during 10 to 30 minutes and with 2 to 6 % w/v H2SO4.
The strength of the acid seems to be similar in both articles. The Italian article made a Pareto chart for some parameters and it seems like temperature and time both are very important.
It seems that the more quiet treatment, both in temperature and time, results in better sugar formation.

This makes the 100 dg C and 3 hours cooking trustworthy, in my opinion.

I will go and find an cheap enamel or ss pot!
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Re: Holzbranntwein

Postby Pikey » Thu Mar 08, 2018 9:15 pm

K - are you tinking Stainless wil be ok at low PSI ?

I have a big stainless cook pot for sale on feebay just now & I'm thinking if we can get a 20% by weight return out of biomass - Jeez ! :D
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Re: Holzbranntwein

Postby Zymurgy Bob » Thu Mar 08, 2018 10:50 pm

A long time ago, during the gasoline crisis of the 1970's, I lived in Oregon's Rogue Valley, where we were surrounded by an old timber industry, and it was easy to find multi-acre piles of softwood sawdust rotting unattended and unwanted in the woods.

As a longtime stiller, I looked really hard at the hemicellulose/sugar/ethanol path for fuel. I knew about the high-temp, high-pressure, low pH industrial methods, but they all seemed out of my practicality range. Having been fascinated by the powers of industrial microbiology and the story of Chaim Weizmann, I took a microbiology course from a micro PhD who'd moved tot he Rogue Valley to teach and run whitewater rivers, and started hunting for an appropriate microbial soup to do enzymatically what I didn't want to do with high-tech equipment.

Unhappy ending is that I never found the bugs I sought, but I'm pretty sure some others have.
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Re: Holzbranntwein

Postby Kareltje » Fri Mar 09, 2018 4:38 am

@Pikey: I do not know if ss can resist hot diluted sulfuric acid, but I can buy a pan for EUR 2 or so and try it. When it is eaten, nothing is lost.

@Zymurgy Bob: The newest article (I mistook it for Italian, as it is published in an Italian periodical, but it originates from Brazil!) states: "Regardless of intense research on cellulose hyrdolysis process by enzumatic way, te amount of hydrolyzate ontained in this process is still less than the amount required for subsequent studies on the fermentation of this hydrolyzate..."
So it seems no one yet has found the right bugs.

I think I will buy some battery acid and sink cleaner. I have a bowl of sawdust sitting here for some years to experiment with. See if it can work.
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Re: Holzbranntwein

Postby Y1969 » Fri Mar 09, 2018 9:37 am

I like to read European newspapers. As our Russian news sites are one continuous vomiting, sometimes you want imported feces. American news sites are not interesting. there's only baseball, Trump and a crop of oranges in California. There are no scandals such as "grandfather-transvestite gave birth to a grandson-addict".
---
About hydrolysis. Do not forget that often the target product is not ethanol, but fodder yeast or other microbiology. Vitamins, drugs and many other things produced by microorganisms.
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Re: Holzbranntwein

Postby Zymurgy Bob » Fri Mar 09, 2018 12:24 pm

Y1969 wrote:About hydrolysis. Do not forget that often the target product is not ethanol, but fodder yeast or other microbiology. Vitamins, drugs and many other things produced by microorganisms.

I agree most enthusiastically with the range of possible fermentation products. Trying to control that output is what makes industrial microbiology interesting.
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Re: Holzbranntwein

Postby Kareltje » Fri Mar 09, 2018 7:16 pm

Oh, yes I know the traps of literature! Title claiming one statement, tables and graphs showing the opposite!
There often is a twist between the science and the reporting of it. Even in scientific periodicals, let alone in newspapers.

I found some articles and thesisses (is that the correct multitude of thesis??) about hydrolysis of cellulose. Life Cycle Analysis and Life Cycle Cost Analysis.
Been there, done that. I will study more and I will report.
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Re: Holzbranntwein

Postby Zymurgy Bob » Fri Mar 09, 2018 8:05 pm

The plural of thesis is theses, pronounced thee-seez. In an attempt to make our language legitimate, we honor the Greeks when pluralizing (is that a word?) the words we stole from them.
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