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SM2
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Quote: Originally posted by plante1999  | 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] |
Yes, white P was also made from plain old urine as well, if I am not mistaken. It took hundreds of gallons just to get the tiniest amount.
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plante1999
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| Quote: Originally posted by plante1999 | 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] |
I'm working on a improved version of this text. I will add picture, more text and better explanation. Should I make a PDF version for the
prepublication thread? Does someone have actually the same problem as me to find hydroxides?
Thanks!!!
I never asked for this.
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plante1999
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Calcium hydroxide production
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. It is know that when calcium carbonate is heated to 850 degree
Celsius it decompose to carbon dioxide and calcium oxide(1), This theory have been use since very old time for quicklime production. Mixing the
calcium oxide with water would produce calcium hydroxide(2) which have been use as a cement since early man civilization. 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
try it on a reduced scale.
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.
:Limy the lime kiln
:The hairdryer
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.
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 seashells
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.
:''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.''
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$CAN for one gallon. I
poured 50ml of methanol in the combustion chamber, I poured most of it on the botom of the furnace and ligthed it, after a few minutes I started the
hairdrier at maximum speed. the reaction(the buring phase) took ten minutes and then I lets it cool for 30minutes(the brick where red hot after the
reaction).
:The charcoal
:The first layer of charcoal
:The layer of seashells
:The last layer of charcoal
:''The burning phase''
Recolting/processing/drying:
Then there was white piece of shells on the bottom of the furnace , there was some charcoal dust on it but I tougth that it will not be a probleme.
The shells(which are suposed to be calcium oxide now) where placed in distill water at R.T, I took 10minutes for the reaction to start but whent the
reaction started the water start boiling and there was a very vigourus reaction ocuring, . Then the calcium hydroxide paste was poured in a stainless
steel mug and heated with limy to redness for 10minutes. The powder was passed in a S.S mesh and the powder was keeped and named ''crude Ca(OH)2''.
The shells pieces that where on the mesh where keeped for a future run. I do recommend to use my process for crude purification but other process to
purify the hydroxide could be used in place of it.
Yield for 3 run is 3 pound of crude calcium hydroxide.
: Temperature raising when the calcium oxide react with water and the newly formed calcium hydroxide paste.
Total cost for the project/$ 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.
:''Pure white powder with few small black particles which I suppose are carbon.''
Side point:
I'm planning to make a PDF version of this for the prepublication thread, I would really like to have help. I you can help my please use the U2U
system.
Quote 1:
CaCO3 -850degree Celsius-) CaO + CO2
Quote 2;
CaO + H2O -) Ca(OH)2
Sources:
Wikipedia
-calcium hydroxide
-calcium oxide
-lime kiln
My own test
[Edited on 21-5-2012 by plante1999]
[Edited on 21-5-2012 by plante1999]
I never asked for this.
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plante1999
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PDF was made and is in the prepublication thread. If someone want to help me it will be greatly appreciated.
I never asked for this.
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Adas
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What a beautiful piece of work! And you have nice forests there :O
Rest In Pieces!
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simba
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What about distilling formic acid from ants?
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Adas
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This would also yield too many side-products. But it is possible.
Rest In Pieces!
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barley81
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Apparently distillation of ants was used to make formic acid back in the day. Here is the thread on this topic.
http://www.sciencemadness.org/talk/viewthread.php?tid=19129
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plante1999
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As you may know I made a better version f the calcium hydroxide post in the prepublication thread, be sure to read it and please leave a comment. I'm
actually working on a process to make a inorganic acid from ''raw'' material much like my calcium hydroxide production. I'm planning to make sulphuric
acid or phosphoric acid but I could make other acid, I would like to know which acid I should make to help/interest SM users.
thanks!!!
I never asked for this.
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Adas
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you can make H3PO4 - get some P-containing mineral and heat it with coal, and lead the exhaust gasses through water.
Rest In Pieces!
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plante1999
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| Quote: Originally posted by Adas | | you can make H3PO4 - get some P-containing mineral and heat it with coal, and lead the exhaust gasses through water. |
I already know the process I will use for sulphuric acid/phosphoric but I just want to know which acid I should make to interest SM user. I know
that some acid are harder to make with raw material but I want to do process that no one on SM did before me, with raw material and that SM user would
like to know how to make with raw material. For the base made with raw material, I made calcium hydroxide (I'm currently making the part 2, using
crude calcium hydroxide to make sodium/potassium hydroxide). If someone want that I make conc. nitric with raw material, I will do it(take note that
nitric acid need nitrate which is not really raw, but if I need to I will make nitrate from raw material.
thanks!!!
[Edited on 27-5-2012 by plante1999]
[Edited on 27-5-2012 by plante1999]
I never asked for this.
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Adas
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You can find nitrates in shit of animals, but I see no way you can make nitric acid from it (with no use of H2SO4). You can also try oxidation of NH3
made by decomposing urea, but urine is very smelly source of urea. Good luck, anyways.
Rest In Pieces!
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SM2
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This reminds me of Dicks, or any of the publications by Kurt Saxon. It is very true, almost any chemical can be made from fire, earth, and water.
But knowledge and sophisticated equipment is also, often, a requisite. In a bit of an irony, it would seem we are going back to some of the older
processes. With new recombinant DNA technology, some commodities can basically be made through the fermentation of bio-mass. Oh, how much I would
give just to have a small plate of some of these bacteria. The justification is the lower carbon fingerprint, as well as reduced costs, as the
bio-mass is ideally free.
I have little doubt in my mind that nutrients containing the proper mix of amino acids, and the some specific engineered bacteria, could form
morphine, LSD, THC...get the picture.
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ElectroWin
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the method used in Edwardian period for making wrought iron, was shared on a TV episode of Edwardian farm.
The ore is heated to yellow hot with a coke-oven, and then struck with a sledge hammer on an anvil to agglomerate the pieces. You get your product
through a sequence of reheating and folding. some discussion of this process is at http://brassgoggles.co.uk/forum/index.php?topic=35966.0
and a youtube video
http://www.youtube.com/watch?v=uSgk73-W0kY
[Edited on 2012-10-04 by ElectroWin]
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elementcollector1
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Very nice process for that Ca(OH)2!
Do the shells really stay solid while decomposing to the oxide? One would think CO2 would be released, causing them to split open, or violently crack,
or some such.
Where I live, I do have access to almost all of the major acids and bases, so I'm not very motivated to make Ca(OH)2 other than if I want potassium
hydroxide (which is one of the few bases that is not available locally. I did order some reagent grade, though...).
Still, great job! I have to go find some bricks! 
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
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hyfalcon
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If you have pickling lime at the store you have Ca(OH)2.
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shannon dove
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Please try to make phosphoric acid from bones the natural way. My idea was to make phosphorus first then make the acid from that. Everyone in the
phosphorus thread keeps using aluminum to reduce phosphates. Reduced aluminum is not natural, and is harder to make than the phosphorus. I have been
researching ways to make it old style, but it is beyond my ability. Any ideas would be appreciated.
What about natural made battery, then divided cell electrolysis using charcoal electrodes, would the positive side become phosphoric acid? Using bone
ash dissolved in vinegar for electrolyte. Or starting with salt water, and when positive side becomes acidic, add bone ash.
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ElectroWin
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if i recall correctly, recovering phosphorus from bone ash usually goes through H2SO4, as
Ca3(PO4)2 + 3 H2SO4 (aq) --> 3 CaSO4 (s) + 2 H3PO4 (aq),
the phosphoric acid is then filtered, the liquid pyrolyzed and P4O10 volatized and collected.
since this depends on availability of H2SO4, maybe do the old process for making H2SO4?
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Adas
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| Quote: Originally posted by ElectroWin | if i recall correctly, recovering phosphorus from bone ash usually goes through H2SO4, as
Ca3(PO4)2 + 3 H2SO4 (aq) --> 3 CaSO4 (s) + 2 H3PO4 (aq),
the phosphoric acid is then filtered, the liquid pyrolyzed and P4O10 volatized and collected.
since this depends on availability of H2SO4, maybe do the old process for making H2SO4?
|
Are you sure that H3PO4 can be pyrolyzed to P4O10? Never heard of that.
Rest In Pieces!
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ElectroWin
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i have not done this, myself. but, from what i read,
as you heat H3PO4, it drives off water, polymerizing to metaphosphoric acid, (HPO3)n. eventually, between 300 - 500C, phosphorus pentoxide is
volatised as the dimer, P4O10.
"Improvements in filter technology is leading to the 'wet phosphoric acid process' taking over from the thermal process, obviating the need to produce
white phosphorus as a starting material.[7] The dehydration of phosphoric acid to give phosphorus pentoxide is not practicable; on heating,
metaphosphoric acid will decompose before it loses water." -- http://en.wikipedia.org/wiki/Phosphorus_pentoxide
although this appears to contradict me, read between the lines, with me, here...
the metaphosphoric acid decomposes, but into what?
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tetrahedron
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freom http://en.wikipedia.org/wiki/Phosphoric_acid:
| Quote: | | Metaphosphoric acid is a singly anhydrous version of orthophosphoic acid and is sometimes used as a water- or moisture-absorbing reagent. Further
dehydrating is very difficult, and can be accomplished only by means of an extremely strong desiccant (and not by heating alone). It produces
phosphoric anhydride, which has an empirical formula P2O5, although an actual molecule has a chemical formula of P4O10. Phosphoric anhydride is a
solid, which is very strongly moisture-absorbing and is used as a desiccant. |
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Magpie
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old lime kilns
Here's pictures of 1800's era lime kilns that I recently saw while on vacation. The brightened photo shows one of the five kilns on site. The other
furnace I presume is for making charcoal. Maybe someone on this forum knows more about this equipment style.
 
The single most important condition for a successful synthesis is good mixing - Nicodem
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Boffis
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Going back to the OP recovery of ammonia from urine. This was actually a commercial process in Glasgow (Scotland) in the late 18th and early 19th
century. They collected to urine and took it to a factory where it was mixed with lime (slaked?) and distilled. This process was eventually overtaken
by the recovery of ammonia from coal distillate liquor. Although the yield looks small on paper given the vast amounts of coal distilled in Britain in
the 19th century production from this source exceeded demand and much of it was dumped into rivers!
Other old processes that have been reported elsewhere on this site are numerous, I reported uric acid from bird guano, there is a potash-from-wood ash
thread and others. Other processes include the recovery of ferrocyanide and ultimately cyanide from coal gas scrubber waste (so-called blue billy
where I come from) or from animal waste. Since blue billy is a complex mixture of iron oxides, sulphides cyanides etc I think you could use prussian
blue as a suragate in the coal process if you want to experiment with this and for the calcined animal (protein rich) waste route try cyanuric acid or
urea; I tried the former its much less smelly than calcining hoof and horne and using the residue!!
There are many more such processes if you're interested check out an early version of the book Spon's Workshop Receipts
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idrbur
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I have tried to make methanol from wood but i end up with only alot of tar.
These days i am trying to make furfural from corn cobs.
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Boffis
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If you want to make furfural try using a bought pentose such a xylose or ribose which are now readily available and fairly cheap. Alternatively you
can make arabinose from OTC sodium gluconate and dilute H2O2 or from glucosamine and hypochlorite. Another good source material is the gum that oozes
from old cherry and almond trees. These materials all give much better yields.
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