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Author: Subject: Old process for synthetising chemicals
plante1999
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Old process for synthetising chemicals

I will start with the making of NH3 from urine , the process is simple, dry the urine and dry distill the dry urine to disolve the ammonia in water.

(NH2)2CO -) NH3 + HOCN

If you have other process , like reffining iron from ore and other please share it! C, Carbon , S8, Sulfur , CH3OH, Methanol are chemicals that are easy to synthetised/found in the wild.

I am looking for the process for refining galena, PbS, to get lead metal.

Thanks!!!!

[Edited on 16-12-2011 by plante1999]

[Edited on 16-12-2011 by plante1999]

[Edited on 16-12-2011 by plante1999]

cyanureeves
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try using horns. just stuff them in an old empty spray paint can and make a cork out of a tree branch, drill a hole in the center and push a copper tube in it. this is how i made my first ammonia.i then went on to use dried wood instead to make methanol but only got a few drops.i tried fermenting urine one time but it just stunk my tool shed too bad.
JibbyDee
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Can you actually get significant amounts of NH3 like this? Very interesting, keep us updated on this. I'm very interested in outdoor/survival chemistry myself too. I'm going to try making KOH from wood ash one of these days.
Neil
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Ho I'd love to see you make iron via a bloomery - it's hard as heck!
You need to mix up clay and form it into a bloomery, once you've done that it needs to be dried and heated till it is red inside and then feed ore and charcoal until it's clogged. hopefully the clog is an iron bloom.

http://iron.wlu.edu/
Magpie
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I have done some smelting:

*Sn from cassiterite using H2. Tried using C but no success.
*Zn by reduction of ZnO using C at high heat
*P from NaPO3 using Al at high heat
*Au from quartz ore using fire assay method. In this method PbO is reduced to Pb using any carbonaceous material. I used wheat flour.

If you have any questions about these experiments let me know.

I think the smelting of iron or copper ores would be quite a challenge due to the high heat required.

[Edited on 16-12-2011 by Magpie]

The single most important condition for a successful synthesis is good mixing - Nicodem
bbartlog
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 Quote: I will start with the making of NH3 from urine , the process is simple, dry the urine

Well, let's start with that part. How are you going to dry the urine (to urea I suppose) without decomposing it in the process? And if you dry distill what's left, how much other stuff do you think you will get? I have boiled down urine and recommend against that way of doing it - foul smelling mess, basically, and premature decomposition.
Anyway, I suggest hydrolyzing the urea in the urine (without trying to dry it) either by adding base or just letting it stand. Then you can force the NH3 out of solution by heat or more base. I once made some dilute ammonia solution (only 3%, sadly) by putting stale urine and agricultural lime in a 5 gallon bucket, then putting a beaker of water in with it (above the urine) and closing the lid. Using the same materials with some setup that allows for efficient removal/transfer of the ammonia, rather than vapor pressure equilibration, would allow for better results.
plante1999
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 Quote: Originally posted by Magpie I have done some smelting: *Sn from cassiterite using H2. Tried using C but no success. *Au from quartz ore using fire assay method. In this method PbO is reduced to Pb using any carbonaceous material. I used wheat flour. If you have any questions about these experiments let me know. I think the smelting of iron or copper ores would be quite a challenge due to the high heat required. [Edited on 16-12-2011 by Magpie]

This is the style of foundry that I use to make metals from oxide.

Cassiterite is supposed to be reduced by CO so is supose there was a probleme with the C burning to make CO. I will try it if I find cassiterite.

I suppose that sawdust + PbO will make Pb...

I aready smelted copper oxide to copper in a bloomery style foundry fired with hard wood. But I maked a sponge of copper.

[Edited on 16-12-2011 by plante1999]

[Edited on 16-12-2011 by plante1999]

[Edited on 16-12-2011 by plante1999]

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Even better method od producing ammonia from urea is using sodium hydroxide - more ammonia is released.

CH4N2O + 2 NaOH ----> Na2CO3 + 2 NH3

blogfast25
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Ammonia: any old ammonium salt, dry distilled with NaOH will give good quality NH3. (NH4)2SO4 is available at many garden centres. NPK fertilisers usually contain ammonium too. The N content of urine is really quite low.

Tin from cassiterite, with carbon? Requires at least 900 - 1000 C. I did it in a corned beef tin on a charcoal fired furnace.

plante1999
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Did you have picture of the reduction of Cassiterite?

C , Carbon can be made from pyrolisis of wood. I have Already done it.

CH3OH can be made by distilling two time wood, for the first distillation it make oil and at the second distillation CH3OH with some other ligth hydrocarbon will distil off .

[Edited on 17-12-2011 by plante1999]

Neil
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Your picture is close to an iron bloomery.

A bloomery has no charcoal grate as nothing would survive. The air blast (tuyer) pipe shoots directly into the charcoal. The furnace doesn't have a closed bottom, instead it has a tap arch which is lower then the opening of the tuyer.

As the smelt goes on, the tap arch is opened and extra slag is drained whenever the air blast is blocked. The temperatures in the furnace are relatively low for air/charcoal - you only want about 1200­°C IIRC.

Key things seem to be the preheating of the furnace and making sure the ore is well roasted and broken up thoroughly.

blogfast25
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 Quote: Originally posted by plante1999 Did you have picture of the reduction of Cassiterite?

Unfortunateky not. It would have been worth taking one though: when the reaction starts the SnO2/C mixture starts behaving like a fluid bed; 'bubbles' of CO2 start rising up through the fine powder. Quite a sight!

White Yeti
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I've tried getting a fire hot enough to melt iron for quite some time, the issue is really to get lots of air into the mix. My friend recommended building and using a huge box bellow to supply air, especially if your furnace is far from any sources of electricity.

My furnace is a work in progress, I'm getting it to be only 800C. I wish I could get it to be hot enough to melt glass, so that I could blow my own glassware.

"Ja, Kalzium, das ist alles!" -Otto Loewi
blogfast25
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 Quote: Originally posted by White Yeti I've tried getting a fire hot enough to melt iron for quite some time, the issue is really to get lots of air into the mix. My friend recommended building and using a huge box bellow to supply air, especially if your furnace is far from any sources of electricity. My furnace is a work in progress, I'm getting it to be only 800C. I wish I could get it to be hot enough to melt glass, so that I could blow my own glassware.

Search for 'charcoal paint can furnace': there are some very simple designs around that will melt mild steel in a jiffy. The key is indeed lots of charcoal and huge amounts of air, I supply air with an inverted old 'bag type' hoover. Mine's falls just short of meting appreciable amounts of copper.

For instance:

http://developing-your-web-presence.blogspot.com/2007/05/cof...

plante1999
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A copper melting furnace is pretty easy to make.... I already make many furnace for melting metal ... Electric , hard wood , Propane gas , C carbon , personnaly I prefer to use hardwood. It heat about as hot as C , carbon but smell realy better.

[Edited on 17-12-2011 by plante1999]

[Edited on 17-12-2011 by plante1999]

Vogelzang
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 Quote: Originally posted by cyanureeves try using horns. just stuff them in an old empty spray paint can and make a cork out of a tree branch, drill a hole in the center and push a copper tube in it. this is how i made my first ammonia.i then went on to use dried wood instead to make methanol but only got a few drops.i tried fermenting urine one time but it just stunk my tool shed too bad.

I remember using an outhouse on one of my relatives' farms a long time ago. It didn't stink, probably in part because air could freely circulate in it. Also, you shouldn't use toilet paper in an outhouse, because its screws it up. They usually use corn cobs. Outhouses take care of themselves from what I've heard. I've got to remember to clean my toilet, BTW.

[Edited on 17-12-2011 by Vogelzang]
Neil
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With charcoal focus on your charcoals surface area and you'll get well over 800°C even with a piddly air blast
MagicJigPipe
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"I'm going to try making KOH from wood ash one of these days."

I have successfully made K2CO3 from wood ash before. It works great and seems to be relatively pure. I'm not sure how you would go about getting KOH, though.

"There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think, free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer
neptunium
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i have this book from 1876 where a lot of chemicals are prepare the old fashion way...
galena is wash with water then it discribe 2 methods 1 reduction and 2 oxidation
1 heatint the galena with iron in the oven
2 heating the mineral with air blowing on it to oxidized the PbS in sulfates and oxide.
when the color is just right they closed the oven and heat it up higher.
the remaining sulfite react with the oxide and sulfate . according to

4PbO+2PbS = S2O4+6Pb and 2PbO,S2O6+2PbS=2S2O4+4Pb

the book goes on to discribe what to do if the original ore contain silver, arsenic, zinc etc..
I like this 135 years old book i have others but this is the oldest
cyanureeves
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i read that in the olden days potassium hydroxide was made by first making the potash then limestone was heated to brittleness in a fire pit then added to the potash.i believe caustic lime is still made that way in old mexico for skinning maiz before turning it into corn flour.they add it to pumpkin also to make a certain candy.
hissingnoise
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 Quote: I have successfully made K2CO3 from wood ash before. It works great and seems to be relatively pure. I'm not sure how you would go about getting KOH, though.

You could precipitate carbonate from the solution as CaCO<sub>3</sub> by addition of quicklime.

plante1999
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Does someone have already made Calcium hydroxide from calcium carbonate mineral? I want to make calcium oxide from the carbonate by heating than dump the product in water to make calcium hydroxide. I dont yet know what fuel I will use.
What set-up should I use?

More detail:

This is the type of rock that I found, I disolved some in HCl and then I presipitate the sulphate, This is not the best test ever but It was the best I could do for calcium at this time.

[Edited on 19-5-2012 by plante1999]

[Edited on 19-5-2012 by plante1999]

plante1999
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Sorry for the double post.

I tried heating one piece of this mineral. I place the piece on a SS sheet and I heated on it with a propane torch to red heat. Suddenly the mineral made a lot of very bright white light, from what I read calcium oxide make a really intense white glow upon heating so I lets the mineral cool. I don't think my mineral have been heated to 2400 degree Celsius like Wikipedia said, at maximum I Think I got 1300 degree Celsius, so I think Wikipedia need sources for the 2400 degree Celsius, the ''source'' they use did not talk about the required temperature at all. Then I dumped it in distill water, the mineral make a hisss sound and the piece broke in many piece and most of them dissolved. Finally the solution was filtered and tested with universal ph indicator showing more then 10 on ph scale.

It was quite easy to perform this synthesis, I'm planing to make more of it to get my desired product 100g of Calcium hydroxide made from completely by natural occurring material (including charcoal fuel).

Does calcium oxide dissolve in methanol to make calcium methoxide? If yes what is the solubility of calcium oxide in methanol?

CaO + 2 CH3OH -) Ca(OCH3)2 + H2O

Thanks!!!

[Edited on 19-5-2012 by plante1999]

[Edited on 19-5-2012 by plante1999]

barley81
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CaO is used to dry alcohols including methanol. Its solubility in methanol is likely to be very, very small.

http://delloyd.50megs.com/moreinfo/drying.html
plante1999
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Today I raffined my process for making calcium hydroxide...(picture and better explanation will be added tomorrow).

Background information:
Where I live I cannot get sodium hydroxide/ammonia/calcium hydroxide in fact the only hydroxide that is sold is drano which is a hard to separate chloride/nitrate/hydroxide of sodium and aluminium. This obligated my for a long time to change part of synthesis to use carbonates in places of the hydroxides, in some reaction the hydroxide could not be substituted by carbonate. I finnaly decided to make my own hydroxide, and the most easy to make was calcium hydroxide and its synthesis use realy easy to find reagent here. A typical lime kiln was made with brick, the fuel was coal/charcoal and the calcium carbonate was in form of limestone(the name is a little obvious). the air supply was not compressed as modern variant, the kiln was filled with alternated layer of coal/limestone. As this technologie was old and quite simple I desided to give it a go.

Limy the lime kiln

First I made a hardwood charcoal furnace from normal sized plain brick a hairdryer and a 1.5inch steel tube.
The hardwood charcoal was in 3x3x2inch pieces size. I named it limy since it will be used mostly to make calcium oxide.

I make a patern with the bricks which lets one half brick of space for the combustion chamber by 4 brick heigh. The kiln was placed on a 3/8inch steel plate.

Total cost for this part:0$CAN It cost me nothing since all these things where liing around in my garage. The calcium carbonate source: I originatly wanted to use limestone that I found arround my house but I found that they where highly contamined with iron/sulphur. From wath I read in the old time that some time seashells is used if limestone was nnot avaible so I bougth seashells at the dollarstore, I was not sure if it was ''natural'' seashell so I added one seashell in HCl and it dissolved completly levving a colorless solution, I dumped half of this solution in sodium carbonate solution and the other part in sodium sulphate solution these two solution becomed cloudy. It's not the best test for calcium but it worked. The fuel: I used to fire things with wood since it is free here , one 15 minutes walk in the forest and I could get 50Kg of wood. But I found that wood in this type of furnace is not the best fuel since it is very smelly, the wood seem to char by only burning the carbon. Since this try I took my 4kg bag of hardwood charcoal and tested it, it maked almost no odor and sligthly more heat than wood, it seam to be the best fuel for this purpose. Firing it: I made 1 layer of charcoal on the bottom, on it I made a layer of seashells and A last layer of charcoal. Here methanol is 4$CAN for one gallon. I poured 50ml of methanol in the combustion chamber, I poured most of it on the botom of the furnace and ligthed it, after a few minutes I started the hairdrier at maximum speed. the reaction(the buring phase) took ten minutes and then I lets it cool for 30minutes(the brick where red hot after the reaction).

Recolting/processing/drying:

Then there was white piece of shells on the bottom of the furnace , there was some charcoal dust on it but I tougth that it will not be a probleme. The shells(which are suposed to be calcium oxide now) where placed in distill water at R.T, I took 10minutes for the reaction to start but whent the reaction started the water start boiling and there was a very vigourus reaction ocuring, . Then the calcium hydroxide paste was poured in a stainless steel mug and heated with limy to redness for 10minutes. The powder was passed in a S.S mesh and the powder was keeped and named ''crude Ca(OH)2''. The shells pieces that where on the mesh where keeped for a future run.
Yield for 3 run is 3 pound of crude calcium hydroxide.

Total cost for the project/$per pound of crude hydroxide: 10$/1\$ per pound of crude calcium hydroxide

Testing:

The crude product where tested with HCl solution to see if there was carbonate in the hydroxide, only a very small amount of gas where produced( approximation, Maximum 7% calcium carbonate) then the crude product was added to ammonium nitrate solution and a very strong ammonia odor was observed, Succes!!

Description of the crude product: Pure white powder with few small black particles which I suppose are carbon.

CaCO3 -850degree Celsius-) CaO + CO2

CaO + H2O -) Ca(OH)2

Like I said the post will be updated tommorow.
Thanks!!!

[Edited on 21-5-2012 by plante1999]

[Edited on 21-5-2012 by plante1999]

[Edited on 21-5-2012 by plante1999]

[Edited on 21-5-2012 by plante1999]