Sciencemadness Discussion Board - Old process for synthetising chemicals

Old process for synthetising chemicals

plante1999 - 15-12-2011 at 16:05

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 - 15-12-2011 at 17:09

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 - 15-12-2011 at 18:15

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 - 15-12-2011 at 18:34

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 - 15-12-2011 at 19:00

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]

bbartlog - 15-12-2011 at 19:28

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 - 16-12-2011 at 05:00

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]

Adas - 16-12-2011 at 07:09

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

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

[Edited on 16-12-2011 by Adas]

blogfast25 - 16-12-2011 at 07:44

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 - 16-12-2011 at 18:15

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 - 16-12-2011 at 19:13

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 - 17-12-2011 at 05:39

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 - 17-12-2011 at 07:13

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.

blogfast25 - 17-12-2011 at 08:46

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 - 17-12-2011 at 09:59

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 - 17-12-2011 at 10:11

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 - 17-12-2011 at 19:04

With charcoal focus on your charcoals surface area and you'll get well over 800°C even with a piddly air blast

MagicJigPipe - 17-12-2011 at 20:57

"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.

neptunium - 18-12-2011 at 08:43

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 - 18-12-2011 at 14:05

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 - 18-12-2011 at 15:12

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 - 19-5-2012 at 05:44

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 - 19-5-2012 at 10:04

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 - 19-5-2012 at 10:09

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 - 20-5-2012 at 19:07

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]

SM2 - 21-5-2012 at 05:38

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.

plante1999 - 21-5-2012 at 05:52

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!!!

plante1999 - 21-5-2012 at 13:41

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]

plante1999 - 21-5-2012 at 17:54

PDF was made and is in the prepublication thread. If someone want to help me it will be greatly appreciated.

Adas - 22-5-2012 at 08:45

What a beautiful piece of work! And you have nice forests there :O

simba - 23-5-2012 at 11:03

What about distilling formic acid from ants?

Adas - 23-5-2012 at 11:37

Quote: Originally posted by simba

What about distilling formic acid from ants?

This would also yield too many side-products. But it is possible.

barley81 - 23-5-2012 at 11:46

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

plante1999 - 26-5-2012 at 10:46

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!!!

Adas - 26-5-2012 at 11:15

you can make H3PO4 - get some P-containing mineral and heat it with coal, and lead the exhaust gasses through water.

plante1999 - 27-5-2012 at 02:03

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]

Adas - 27-5-2012 at 07:00

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.

SM2 - 12-7-2012 at 06:54

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.

ElectroWin - 4-10-2012 at 10:21

Quote: Originally posted by plante1999

If you have other process , like refining iron from ore and other please share it!

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]

elementcollector1 - 4-10-2012 at 11:17

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!

hyfalcon - 4-10-2012 at 15:28

If you have pickling lime at the store you have Ca(OH)2.

shannon dove - 4-10-2012 at 18:48

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.

ElectroWin - 17-10-2012 at 14:56

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?

Adas - 18-10-2012 at 05:59

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.

ElectroWin - 18-10-2012 at 09:55

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?

tetrahedron - 18-10-2012 at 11:06

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.

old lime kilns

Magpie - 17-7-2015 at 18:42

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.

Boffis - 18-7-2015 at 06:26

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

idrbur - 19-7-2015 at 02:19

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.

Boffis - 19-7-2015 at 07:30

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.