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Antiswat
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[*] posted on 4-4-2021 at 00:14
Low effort DIY chemical productions


i was wondering, what kind of chemicals can you produce with little effort? sort of "set and forget" as in, low maintenance, where you only really get it running and then you reload reaction chamber and purify the product, of what im seeing theres:
nitrate production from urine or urea
chlorate/perchlorate production by electrolysis
persulfate production by electrolysis
NO2 production by ostwald process
metal oxide / hydroxides production by electrolysis
reactions like copper acetate + lead metal = lead acetate
copper chloride from HCl and copper metal
hydrogen peroxide by electrolysis of H2SO4

and, this sort of doesnt count as its not producing a chemical but rather a structure: crystallizing various chemical compounds by letting solution slowly evaporate




~25 drops = 1mL @dH2O viscocity - STP
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https://en.wikipedia.org/wiki/Solubility_table
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[*] posted on 4-4-2021 at 10:22


Beer?
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Fyndium
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[*] posted on 4-4-2021 at 10:28


This can be applied to almost anything that can be batch produced and does not need manual addition of chemicals, and the easiness is very relative term. Even very complex synthesis can be run concurrently in a dedicated setup.

For example, I've ran a synthesis in 4N RBF reactor(reflux, thermoprobe, stirrer, dropper) where I charged the ingredients, heated up to reaction temp treshold, charged in the limiting reagent at controlled rate, buffered with water bath and let the stabilized reaction run for 4 hours, cooled by changing cold water to bath and circulating with pump, drain the bottom layer with suction to sep funnel, drain the rest off and immediately charge a new load. By preheating the bath water and using pump to circulate coolant afterwards shortens the lead-in and lead-out time from hour to as short as 15 minutes. I made some tests in this area because I had to run it a few times due to failed reaction and had too much time waiting for new reagents to arrive. Diligent operator could run three batches in one day, and an industrious one could add infinite amount of parallel setups with desired reactor volume. This is pretty much the standard it is done in the chemical industry in small batches, the equipment may be more sophisticated.

Batch production is basic. Try to run a continuous reaction so that you can constantly add stuff and extract stuff and have 24h uptime, then you're talking about mass production. The major issue with a very big margin for the amateur is the inherent complexity and cost of these equipment, and also the question where that large amount of output would be used for. One could make tabletop haber-bosch machine that makes ammonia and runs 24/7 with enough determination, but even that setup could churn several liters of ammonia per day. The exact mechanisms of these are also trade secrets, and calibrating one to operate reliably is basically a career job for many people over their lifetime, not a wiki-how-to trick that can be done by any preschool experimenter.

On the other hand, for amateur and some other uses the low yield can still well warrant the synthesis of some reagent, because the alternative is either not to able to do the reaction at all or buy a very expensive reagent instead. The other extent to this matter is trying to make some seemingly simple reactions work, like making acetaldehyde and formaldehyde by putting methanol or ethanol vapor over heated copper catalyst. People seen to have got something done, but if you say that one needs 5kg of pure reagent by the end of the week, you're gonna have hard time getting that to work.

Process economics is one of my favorite aspects of this hobby, so I've tinkered on it for some time. It's not if something can be done (with specialty fine reagents that are unlimited for any large institutional research lab but 99.9% ACS unobtanium grade with 400$ per 100g for the amateur), but can it be done from something very cheap with high efficiency?
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[*] posted on 5-4-2021 at 03:47


Chloroform is pretty hands off. I do it like Doug's Lab shows, directly in the bleach container.

[Edited on 4-5-2021 by monolithic]
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Fyndium
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[*] posted on 5-4-2021 at 04:19


Imo this method is much better:

https://www.youtube.com/watch?v=heqMdYqqMGs
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[*] posted on 5-4-2021 at 13:15


In my opinion there are key markers that make a chemical reaction "low effort". The biggest one is a reaction with easily identifiable products. One example would be the chloroform reaction already mentioned. This is because one can see the reaction mixture separate into two layers. It is easy to see if the reaction is occurring, it is easy to see when it has finished, and it is easy to identify the products based on their separation into layers. One thing that I see often is an experimenter mixing several chemicals together and stating that they got a product, but with no analysis or means of isolating or identifying their product. In their defense, with many reactions it can be difficult to identify the products without expensive analytical equipment.

Another marker is that the reaction products are easily recovered in fairly pure form without using highly specialized or expensive equipment. Again, the chloroform reaction fits this requirement since it is easy to remove the organic layer with a pipette.

An additional marker would be that the desired reaction will still proceed under a wide variety of process conditions. Failing this, the reaction would need to give obvious clues as to when these conditions are met. The chloroform reaction is still a good example, as the reaction temperature will rise quickly and the mixture will grow cloudy when the reaction begins.

Just because the reaction is conceptually simple doesn't make it low effort. One example is the synthesis of glyoxal. It is the simplest double aldehyde and can be made from the nitric acid oxidation of ethyl alcohol at room temperature. The problem is knowing that the reaction is occurring, when it is finished, and separating the product from half a dozen or so side products. Even characterizing it can be complicated, as glyoxylic acid is a side product, and this acid gives a positive silver mirror test just like glyoxal does.

The Ostwald Process that Antiswat mentions is technically complicated to set up, but I have found it to be a well-behaved process. The NO2 product is easily identifiable visually. With a constant feed of ammonia and air through a simple tube furnace, the process can continue for weeks at a time without any real intervention. For those reasons I consider that process to be fairly low effort.

Of course, all of the above is completely subjective...




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[*] posted on 6-4-2021 at 01:04


Absolutely right. Now that I think it, a good or easy reaction is one with wide tolerances for temperature and time(one that proceeds fast, produces little side reactions and does not degrade if excess time or temperature is applied, within reasonable limits ofc), is not exothermic, gives clear indications in form of precipitate, color or temperature that it has been completed and the product is easy to recover in pure form, or is readily purified by simple wash or recrystallization and filtration from specific solvent.

Other factors I consider are availability and cost of reagents, and a very big one: toxicity. If something can be done with little more work using less toxic stuff, I choose that. For example, there is a synthesis which calls for cyanide, but it can be accomplished via other, non-toxic means with an extra step.
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[*] posted on 6-4-2021 at 07:18


Thank you for this input Fyndium! I agree that reagent cost, availability, and toxicity are important factors as well. I like your expansion on process tolerances. It looks like we are getting a useful compilation going here.

At the end of the day, for most of us this is a fun hobby. If it’s “fun”, then a lot of times that feels like “low effort” because the motivation is there and it doesn’t feel like work. So that will add a little subjectivity to a list like this. Sometimes I see a procedure that is fairly simple but it seems like more effort to me, because it uses some basic equipment that I do not normally use. So we can limit ourselves in this way sometimes.




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[*] posted on 6-4-2021 at 13:35


And, of course, as experience increases, you will get better at handling chemistry. Chemistry is an art of experience and practice. Eventually, you'll be able to foresee many issues before you end up in a mess that can take a LOT of work to return to the point you started from. The more you do simple reactions, the better you are prepared for more challenging stuff, and you will begin to see very swift hints what's going on, and know what to look for and what to expect.

Doing same synthesis all over again makes you good at making that one compound. Gaining experience all over will make you good at making all kinds of compounds. And, also, what a hobbyist can learn from professional, industrial and manufacturing settings is process economics.
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Antiswat
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[*] posted on 8-4-2021 at 05:42


i have a few to add- alcohol oxidation using heated copper or silver wire to aldehydes, for instance formaldehyde or acetaldehyde- this was done by a chemist i talked to long ago using glass jars and copper wire, and an aquarium bubbler to give slow air supply, the acetaldehyde was mixed with ammonia to make it more easily to store forming an adduct of some sort

fermentations would definitely go on this list, ive thought of making butyric acid but i couldnt find out where to get the bacteria, so fermentations would depend on what you can easily get access to, nitrifying bacteria would also count as fermentation. identifying and isolating strains of bacteria i wouldnt say is something everyone can do

alkali metal formation using liquid medium reduction, you can use menthol and maybe even MgAl dust, i dont see why people dont run this reaction in 31 stainless steel so youre free from worrying about the glass getting etched up and eventually releasing liquid alkali metal and alkali hydroxide

there was a method of making sulfuric acid using SO2 and vanadium oxide catalyst, but you needed dry air for this, the idea was that it created SO3 and that SO3 was pumped into H2O to give H2SO4, but the threads on it never seemed to give much off others than anticipation

i recall something about an "uncle festers" electrolytic reduction cell, from vague memory it relied on putting a current through glucose which at one electrode would form single hydrogen that would then serve as a powerful reducing agent, and i recall also something about analine being possible to produce from similar electrolytic method- sadly chloroform cant be made using continous electrolysis as it would form some toxic chemical, COCl2 was it? they say it smells like wet hay and can kill you with just low ppm exposure for an hour

thermodecompositions could also be very cool in this regard, except theyre oftenly difficult to run- i remember one guy who made a 100L PP/HD/LDPE decomposition chamber, electronic heating that was insulated in a 200L barrel leading to a crude distillation apparatus
he would acquire 0.8L of "diesel" from 1kg of plastic, if the product was too thick he would just run it through another time and it would become less viscous, now this is certainly not a pure chemical product but very useful- working at a scrap yard its 100% that this is out there in the industry, we almost pay people to come pick up the valuable plastic types, one company bought 20 tonne truck load for maybe 200 euro or around that. now if you could turn that mix into some pure chemicals, but i dont even have a guess of what chemicals PP or PE could break down into, that could be quite something.

just in reply to chloroform, if you can buy some trichloroacetic acid online you can run destructive distillation on it with NaOH and get quite great yields, its also possible to make NaClO from trichloroisocyanuric acid and NaOH, this might be ""bleaching powder"" but i assumed it to be CaClO

i just like these low effort processes, because it gives me an objective number that i can look back at and see that i did this and that much, like a nice stack of freshly cast aluminium, all squared and lined up, i think home chemists can generally be put into 2 categories- producers and consumers, im very much a collector myself and ive managed to buy mercury, P2O5, guanidine carbonate and other gems

it was also found that you can make regular vodka taste like expensive whiskey by dumping the vodka with some pieces of wood into a high frequency cleaning machine- can this machine maybe alter chemicals or make chemicals more reactive? pulsing a specific frequency into a solution to cause some quantum like effect

in the view of home chemistry, we generally like to stay at atmospheric pressure and below 600*C, im sure you would weld up a thick metal pipe to resist easily 1000 bar, but at the time that goes wrong you wouldnt even wanna be in that same room if you were dressed in a blast suit




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
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Fyndium
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[*] posted on 8-4-2021 at 09:35


Pressures up to 10bar are readily achievable if one is willing to see some effort on equipment construction. But if one has only duct tape and some glassware, stay ntp.
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[*] posted on 8-4-2021 at 11:54


Quote: Originally posted by Antiswat  
fermentations would definitely go on this list, ive thought of making butyric acid but i couldnt find out where to get the bacteria, so fermentations would depend on what you can easily get access to, nitrifying bacteria would also count as fermentation. identifying and isolating strains of bacteria i wouldnt say is something everyone can do

This is a very interesting notion, and on biology forums I have read threads about this. Selecting and growing bacteria is a field of research in its own right. Industry started to make use of that when all regular syntheses had low yield or were too laborious. But again, I don't rule it out as impossible in an amateur setting, and it's not principally difficult.

Another very elegant route of synthesis is the use of enzymes. Their use does require closely controlled conditions in particular regarding temperature and concentration, which makes it merely a specialism by design and less suitable for amateur chemists.

But as remarked earlier, it's also a matter of how much you're willing to invest and what you consider difficult. A few years back, there has been a lot of discussion about opening hard calcined (rare earth) oxides, but I found that the majority of them can be opened by prolonged boiling in concentrated H2SO4. Water comes over dropwise, but it's not complicated, it just takes time. The only complicating factor is that the remaining unreacted oxide is usually so fine that it needs to be centrifuged or it will stay in suspension.
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Antiswat
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[*] posted on 9-4-2021 at 03:30


calcined oxides? that sounds like it could use some vibrations. i dont quite get it. the problem is that the material is very hard or that it doesnt wanna dissolve easily? turning it into dust would make it react faster, and i imagine that one could turn platinum metal bar into platinum powder to get it to dissolve same day, dissolving platinum can take many days.

i bet these hard calcined materials could be turned into finer particles with a demolition charge underwater, might not take a whole lot, then again aluminium oxide is super hard metal oxide. what exact metal oxides are they talking about?




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
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[*] posted on 11-4-2021 at 15:08


Cr2O3, Nd2O3, CeO2, Fe2O3, ...
Due to their crystal structure they are very hard to dissolve, check here, here, and here.
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[*] posted on 18-4-2021 at 17:32


Every trial that doesn’t go as planned and is deemed safe enough to be shelved for the time being.....
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Antiswat
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[*] posted on 20-4-2021 at 05:48


long ago i mixed some ethylene glycol with urea and heated it, it was supposed to give ethyl amine, very minor odor. i dumped it into a vial and stashed it for years, storing it with a bunch of other vials i found out that it does produce ethyl amine over long time, i had to throughly wash every other vial in there, just washing them on the outside as they all had different contents didnt rid the smell, i have no guesses on concentration of ethyl amine



~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
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Antiswat
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[*] posted on 13-6-2021 at 02:41


i have an addition, chlorine gas can be formed slowly using potassium dichromate and HCl, it forms chlorochromate
if a flask with this mix was positioned above another reaction flask so that the formed chlorine gas would fall into the second flask, with maybe some organic compound it should over time react to chlorinate that organic compound if its possible at room temperature, the gain from this would be having no chlorine gas escaping and no need for sophisticated chlorine gas removal equipment or a fan to extract the chlorine fumes




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
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[*] posted on 13-6-2021 at 07:00


I think the amount of cleaning up the mess is another matter making some reactions nicer than some others that give a huge mess. Often the reaction is not the source of the mess, but the separating and purification steps. Sometimes it is less work in total making an extra step if the other method saves you from a lot of cleaning.

Easy product identification is a huge deal for a hobbyist. For example, an a professional organic lab things get so much easier when you routinely run for example NMR and IR on every product. A bench top NMR would be so great at home lab but unfortunately they are not too affordable. Methods to analyze small amounts of products also enables you to make small scale experiments.

So, you're left with easy to recognize products that can be separated without making a huge mess. Add in requirement for relatively safe materials and reactions that work with wide (or at least well known and easily controllable) tolerances. Avoid high (and too low) temperature and pressure. Then it sounds like a simple hobby chemist favorite candidate.
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[*] posted on 15-6-2021 at 13:42


@Antiswat How do you produce Nitrate from Urea?

[Edited on 15-6-2021 by Chemgineer]
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Antiswat
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[*] posted on 18-6-2021 at 10:16


nitrate from urea, using bacteria, using hay as substrate or maybe air pump to oxidize the solution and give the bacteria the needed oxygen to create nitrate



~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
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[*] posted on 18-6-2021 at 10:34


Quote: Originally posted by Bezaleel  
Quote: Originally posted by Antiswat  
fermentations would definitely go on this list, ive thought of making butyric acid but i couldnt find out where to get the bacteria, so fermentations would depend on what you can easily get access to, nitrifying bacteria would also count as fermentation. identifying and isolating strains of bacteria i wouldnt say is something everyone can do

This is a very interesting notion, and on biology forums I have read threads about this. Selecting and growing bacteria is a field of research in its own right. Industry started to make use of that when all regular syntheses had low yield or were too laborious. But again, I don't rule it out as impossible in an amateur setting, and it's not principally difficult.

Well, there are hobbyists out there obtaining lysergic acid via fermentation, so its definitely doable in an amateur setting, given enough dedication :P
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[*] posted on 18-6-2021 at 11:14


https://www.youtube.com/watch?v=vJfc6dxrllI
This guy makes an PVC membran for electrolysis you can make sulfuric acid with it in great quantitis ore other stuff.
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[*] posted on 18-6-2021 at 11:30


Quote: Originally posted by Alkoholvergiftung  
https://www.youtube.com/watch?v=vJfc6dxrllI
This guy makes an PVC membran for electrolysis you can make sulfuric acid with it in great quantitis ore other stuff.


*this guy is a member here.
https://www.sciencemadness.org/whisper/member.php?action=vie...




My new youtube channel, primary focus will be on industrial chemistry: https://www.youtube.com/channel/UCQNj8r14-dyi4mlyenLwnaw/vid...
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[*] posted on 18-6-2021 at 12:04


We really have a lot of, what was it called, I heard that term recently...?
It was "niche internet micro celebrities", yes! :D
I like that term, because we have a whole lot of them, which are only known to a very small audience too :o
Like, drop a name like Nicodem, or Organikum, everyone here will know who it is, but outside? Nobody at all! :P
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[*] posted on 19-6-2021 at 11:23


I think mysteriusbhoice has the right idea. Sulfuric acid is a precursor to many restricted chemicals, and you will always have access to metal sulfates. And modern DC PSUs are cheap and effective. With a rugged, low cost DIY membrane we're pretty close to the perfect setup.



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