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scienceboi
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[*] posted on 22-9-2020 at 14:06
Using industrial chemical processes at home


Maybe its a bit optimistic, but is there any way to cheaply do the following things at home? I'd think it would be a nice way to consistently get useful chemicals. It does use a lot of energy though.

Sabatier reaction - produces methane and water from CO2/CO and H2
Haber process - produces ammonia from N2 and H2
Ostwald process - produces nitric acid from NH3 and O2
Contact process - produces sulfuric acid from S and O2
Chloralkaline process - produces Cl2, H2, and NaOH from H2O and NaCl

I feel like if I make it myself I wouldn't have to go through the sometimes tedious process of ordering it from a legit vendor willing to sell to a house residence, buying it from sketchy vendors on ebay, or purifying it from hardware store products. However, some of these processes need high temps/pressures so they need to have a strong chamber to be in.

Anyone got any ideas?


[Edited on 9-23-2020 by scienceboi]




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njl
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[*] posted on 22-9-2020 at 14:35


I have seen all but the Sabatier process done by amateurs, either on this forum or on youtube.
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Dr.Bob
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[*] posted on 22-9-2020 at 16:12


The first two are the hardest, I think, the last two are more doable. Don't know the Ostwald enough to know. But nitric can be made from sulfuric acid more easily, on a small scale, I believe. Simple electrolysis is fun, moving to chloralkylye might be not so hard in similar setup. Many common chemicals are just cost prohibitive to make at home, compared to buying. So I try to make things that are expensive, I only need small amounts, and are makable from (relatively) common chemicals. So making phenolthalein, luminol, sulfa drugs, peroxyoxalates (light sticks) and lidocaine are all neat things to make from more common chemicals that actually have some value as chemicals, and that are within the realm of amateurs. Even some polymers are doable, and some are really fun or useful. Gorilla glue and foam in a can are just diisocyanates, and many other polymers are made from simple chemicals.

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Herr Haber
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[*] posted on 22-9-2020 at 17:03


I'd say the last three ones are doable in any kind of home.
The first two... Well, I'd rather have a barn, a garage or something of the kind away from other things...

I would looooove to build with modern materials an "upgraded" version of Haber's prototype (in case the nickname didnt betray me).
But then what ?

I wouldnt know what to do with all that NH3 :)
Ostwald then ? Why not but we're now talking 2-3 people working on a project if you want to proceed at any speed.
I thought of visiting a big hackerspace in town to see what kind of people I could bond with there.




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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scienceboi
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[*] posted on 22-9-2020 at 17:20


Quote: Originally posted by Herr Haber  

I would looooove to build with modern materials an "upgraded" version of Haber's prototype (in case the nickname didnt betray me).
But then what ?

I wouldnt know what to do with all that NH3 :)


Could you sell any excess?
I would be really interested to build one too! Maybe some engineer types could help out?




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stoichiometric_steve
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[*] posted on 23-9-2020 at 04:17


Quote: Originally posted by scienceboi  

I feel like if I make it myself I wouldn't have to go through the sometimes tedious process of ordering it from a legit vendor


If you can't get the respective reagents due to restrictions pertaining to age, profession or skill, then that already speaks for itself. Consider working on that before you even dream of producing chemicals via processes that require a seriously skilled operator. Judging by your post history, you're simply unfit for an undertaking of that type. Don't waste your money and other member's time on entertaining such a pipe dream.

[Edited on 23-9-2020 by stoichiometric_steve]
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Herr Haber
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[*] posted on 23-9-2020 at 04:36


I may be wrong but I seem to remember his latest prototypes produced around 200ml / hour

Which is great but probably very far from being economical at this scale.
Also, I would go for bottled H2 which would cut any margin by a lot. Naah, that's a project that would never be economically interesting but for the beauty of it ? Yeah, sure.




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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[*] posted on 23-9-2020 at 05:14


There have been attempts at the Ostwald by a few members. I know of at least chemetix's and WGTR's attempts and my own. Though as far as I know nobody has really managed to make useful quantities of HNO3 this way
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[*] posted on 23-9-2020 at 06:24


I once got the part of Ostwald process to work- badly.
I was trying to get nitrogen for a laser. Since it works with air I didn't need great purity so I figured I could run air and ammonia over hot copper/ copper oxide to get nitrogen and water- which I could strip out easily enough.
My plan was to recirculate a bag full of air through a solution of ammonia and the furnace tube until the ammonia was all gone.

There was enough NO /NO2 in the output stream to make the gas brown and smell a bit like chlorine.
So it's possible to do it badly by mistake.
I'd imagine doing it better isn't too big a problem.
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Fyndium
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[*] posted on 23-9-2020 at 10:42


Cheaply? Unlikely.
Possibly? Sure.

But you will need serious dedication, a lot of preparative work and optimization of the equipment. It also should be purpose built. Obtaining pumps that can generate hundreds of bars of pressure in small scale and also possibly handle some chemicals that are reactive can be also a challenge. I guess using pressurized cylinders as batch production could also count.

And I'm talking here a working plant that can actually produce useful quantities of reagents you have mentioned. Many here and elsewhere have proven the concept of making all kind of stuff by industrial methods, but that's about it. They drip in something, distill it over catalyst heated with a torch and manage to get few mL of contaminated liquid that resembles the wanted product? Nope. Bring in a bucket of it, and then you win the grand prize.

You will need:

metalworking tools like lathe, mill, tig welder
metal alloys like 316 and cobalt to handle chemicals
teflon for gaskets
platinum and other nobles for catalysts
adjustable heat source and insulation materials
high pressure and vacuum pumps
a lot of all kinds of specialty tools and some safety gear too

I'm not shooting down anyone here. The quest was to get chemicals via these methods at home not needing to order them. If I were for such a venture, I might actually look into some reagent that is of high demand, of high value and difficult enough to make that any amateur/small scale doesn't bother to make it, and hit a buck by making it in good quantities. Something like phosphorus, borohydrides, etc. High return of investment warrants larger initial costs for the plant.

[Edited on 23-9-2020 by Fyndium]
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macckone
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[*] posted on 23-9-2020 at 10:46


Ostwald process is doable.
You need good process control. ie. stochiometry and temperature
Silver is more accessible to the home chemist than platinum as a catalyst.
Copper can be used as well apparently but is much less efficient.
The birkeland-eyde process is relatively easy but yields are low and it isn't very cost effective.

The chloroalkali and contact processes are much more forgiving.
The first two are much more demanding and although I would love to do a small scale haber plant, it isn't practical unless you have a full machine shop to access.
methane is much easier to synthesis from waste for the home chemist. Bacteria do all of the work.
A haber plant could be easily converted to produce methane, the major difference is the catalyst and carbon dioxide instead of nitrogen.
The Sabatier process uses a lower pressure so a home chemist might be able to do it without extensive equipment.
But many houses have natural gas piped in, so the utility for most of us is questionable.
For small scale usage methanol is generally more useful as a starting material.

There are also newer methods that are more practical for the home chemist:
https://pubs.acs.org/doi/10.1021/acs.jpcc.5b01574
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Herr Haber
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[*] posted on 23-9-2020 at 16:30


Quote: Originally posted by Fyndium  
Cheaply? Unlikely.
Possibly? Sure.


I'm not shooting down anyone here.

[Edited on 23-9-2020 by Fyndium]


No no, you are perfectly right in everything you say. That's why I say it can be done for the beauty of it but would never be economical.

I dont know about your local fablabs / hackerspaces but I've got one with just about any tool, machine and like minded people with skills that I dont have that any mad scientist could dream of.
So yeah, I've been thinking a lot about tourism related with the Haber Bosch process (Breslau / Wroclaw and BASF museums) getting contacts and all the "old" documents I could find.

That could take some years and significant resources.
Beautiful but pointless unfortunately.




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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Fyndium
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[*] posted on 24-9-2020 at 06:38


For the aspect of economics, it's just how much you are willing to pay per unit. If you desire 100kg of product X, the price per kg will be everything + possible feedstock and running costs. I understand that in some instances the price can be pretty high if the need surpasses it. Let's say that the reagent x costs 170€/$/£ per kg if you order it somewhere, and there may be associated risks, limits, regulations and/or some sort of paperwork you are unable or unwilling to match, you got your bottom line break even there, and you are probably willing to pay more than that to get it if it's about that.

For the matter of it, I believe that in less official parts of the industrious world there are facilities that churn out pretty fancy stuff in such scale it can be fed into the again less official markets.

The official plants are of course facilities sized of separate districts in cities that churn out thousands or millions of tons of stuff. On the other hand, they also sell it for the market price which can be sub dollar per kg, insisting you buy tanker/train/shipload of it. And when you buy it from your supplier, it costs 40$ per kg.

[Edited on 24-9-2020 by Fyndium]
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[*] posted on 24-9-2020 at 07:15


These processes are industrial processes and they are so for a good reason. Some processes simply are not suitable for small scale. E.g. a system, allowing pressures of 100+ bar at temperatures of 1000+ C are standard things on an industrial scale, but having such in a suitcase size is nearly impossible. Heaters, thick walls, metal constructions, they require a minimum size. So, personally, I think that the very cheap bulk chemicals like H2SO4, HNO3, NH3, just should be purchased, or should be made from other chemicals.

Making H2SO4 from NaHSO4 can be feasible, at least that does not require high pressure or expensive and difficult to use catalysts.
Gaseous NH3 can be made from ammonium salts like NH4Cl or (NH4)2SO4 (fertilizer!) and NaOH. Available at very low cost in many countries.
HNO3 can be made from H2SO4 and KNO3 or NaNO3. If H2SO4 becomes less available (e.g. in the EU), then still, HNO3 can be made, from NaHSO4 and KNO3 or NaNO3, or from NaNO2 and an acid, which produce NO2 + NO, which can be bubbled through water to make HNO3 (if you have H2O2 then it is even easier).

So, try thinking more away from the big industrial processes, and try thinking about alternatives, which can be used in a home lab setting on a workbench, suitable for making 100's of ml or maybe a few liters.




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njl
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[*] posted on 24-9-2020 at 07:22


Speaking specifically to nitric acid, Nurdrage has several videos on how to make it in high yields with cheap reagents
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Fyndium
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[*] posted on 24-9-2020 at 09:17


I'm yet to find a good otc source of any nitrate in such form in my country that it is easy to extract the acid from it. Calcium nitrate can be ordered from few places, but seems to be out of stock all the time.
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njl
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[*] posted on 24-9-2020 at 09:42


Does that mean that there are available nitrate sources, but they're hard to process into nitric acid?
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[*] posted on 24-9-2020 at 12:15


njl,
Most fertilizers contain some nitrate.
Extracting it from compost is not how most of us want to spend our days.

Fyndium,
Birkeland eyde is easier but yields are low.
The commercial units produce 60-120g/kwh.
A home unit is lucky to produce a tenth of that.
I have a 15k/120ma transformer which is 1800w but I am not getting near that and getting it absorbed is another issue.
The other day I flooded my basement with NOx.
A flyback transformer can easily generate 240w of output at 10khz.
A microwave oven transformer can do 1kw easily but the voltage will be lower.
The trick is getting a nice continuous arc of plasma.
Once electrons are flowing through air the nitrogen and oxygen are getting converted.
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Fyndium
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[*] posted on 24-9-2020 at 23:16


Birkeland is indeed a device on it's own, but the low yield is of an issue. 10kwh per kg is practically turning a liter of fuel oil into a liter of nitric acid in 100% efficiency.

Getting nitrates from pissed off composts sounds a bit arduous. NileRed processed a gallon of his own piss and got only a pinch of urea out fro it, so even if it contains anything of value, purifying it from all the other gunk would be a job on it's own.

There are all kinds of trash fertilizers for consumers that basically contain fillers. I got two bags years ago from clearance sales for very big discount and I dissolved them in hot water with power drill and concrete mixer rod and filtered it through sand to obtain a clear solution, which I concentrated by boiling into a white sludge and now it's been sitting for ages in a bucket. Now that I'm back in business I might do a test with Ca nitrate precipitation to figure out how much it contains sulfates, vacuum filter it, dry it to find out the approximate mass and then test with sulfuric acid to see how much it contains nitrates. If there is urea, I'm not sure what will happen, but if it decomposes into CO2 and NH3 like with alkali hydrolysis, it should react with sulfuric acid to make ammonium sulfate and not to distill over with HNO3.

They sell 25kg bags of pure Ca(NO3)2 in farming stores but they are dedicated for professional farmers and I'm not quite sure what might happen if I showed up there to buy that one bag, even though I have a company.
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[*] posted on 25-9-2020 at 16:31


Fyndium,
Calcium nitrate is a critical growth element for tomatoes.
It is sold in most gardening shops in the US as 4 lb bags.
It may have to be cleaned up but it will be available as 'tomato food' or something similar.
If you go into a farm supply be well versed on tomatoes and tell them you only need one bag because you are using it in your garden.
You might have some pictures of your tomato plants on your phone for evidence.
And if you grow a couple of tomatoes they are delicious.
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