Sciencemadness Discussion Board

Lab scale industrial processes

plante1999 - 7-10-2012 at 09:41

Lab scale industrial processes 2012
volume 1

Its the first volume of a series of many short books containing about 5 industrial process adapted for lab work. All the procedure have been made by me and tested by me. At the time 3 other volumes have all procedures done but the writing is not completed. Eventually compilation will be made to have one bigger Book containing few volumes. If it is possible I would like to use only one thread to upload all the volumes so, for the next volumes I will probably request moderator help to make changes to this post.

The volume 1 contain:

Sodium carbonate
• Leblanc process
• Solvay process
Calcium hydroxide
Mercury
Carbon

The volume 2 contain:

Sulphuric acid
•Lead chamber process
•Contact process
Refractory ceramics
•Fused silica
•Carbon
Nitrogen


Please note that the number of download is irrelevant since frequently I correct mistakes and change the download resetting to Zero the number of download.

Attachment: Lab scale industrial processes Volume 1.pdf (163kB)
This file has been downloaded 3090 times


Attachment: Lab scale industrial processes Volume 2.pdf (151kB)
This file has been downloaded 2032 times

[Edited on 24-10-2012 by plante1999]

Vargouille - 7-10-2012 at 10:22

Regarding the mercury, I was under the impression that simply heating cinnabar will liberate elemental mercury and sulfur, from an anecdote in Periodic Tales: A Cultural History of the Elements. Also, regarding the charcoal, is there a specific reason that sugar-based charcoal must be ground before storage, or is it just because it melts before pyrolysis to carbon occurs?

Good piece, though, grammatical errors aside. Can't wait for the next installments.

plante1999 - 7-10-2012 at 14:06

The sugar will melt and pyrolise at the same time making a column of porous carbon, much like bread so It can't be used in another format than powder.

I would like to know if you could help me to correct grammar?

Thanks for the comment!

[Edited on 7-10-2012 by plante1999]

madcedar - 7-10-2012 at 14:32

Great stuff Plante1999. I'm really looking forward to the next editions. :)

Vargouille - 7-10-2012 at 16:22

Much like a black snake reaction, I suppose. That actually makes sense, now that I think about it. The steam evolved makes pockets in the carbon, making it rise.

I'll send a U2U about the grammar, so as not to clutter up the thread too badly.

Hexavalent - 10-10-2012 at 07:29

Very, very nice, Plante - excellent work.

I really like your writing style and original ideas.

If you need any help at all with grammar, U2U me at any time and I'll be very happy to help.

Regards,
Hex

ElectroWin - 10-10-2012 at 14:54

This is good news, as it is often hard to get reagents, on a budget. thanks

Hexavalent - 23-10-2012 at 07:17

Incredible, plante: you continually amaze me with your ingenuity, sheer knowledge of chemistry and fascinating ideas. A great publication, I really enjoyed reading it. Well done!

I understand that English is not your first language (your English is much better than my French!:)), but here are a few things you may want to consider looking at regarding the wording - I've written your original statement first and then my suggestion below. They're all in chronological order of how they appear in the book (volume 2).

“pyrolysis of sulphate salt”
the pyrolysis of sulphate salts

“at the time.”
at a time

“all reagent”
all reagents

“it make nitrogen”
it makes nitrogen

“Nitrosyl sulphuric acid hydrolyse”
Nitrosyl sulphuric acid hydrolyses

“sulphur dioxide oxydation.”
sulphur dioxide oxidation

“to 300 degree Celsius”
to 300 degrees Celsius

“two holes stopper”
two-hole stopper OR two-holed stopper

“the stopper have”
the stopper has

“The third holes”
The third hole

“The bottle have a two holes stopper”
The bottle has a two-hole stopper

“60 degree Celsius”
60 degrees Celsius

“will have burner”
will have burned

“and sulphuric acid fume is emitted”
and sulphuric acid fumes are emitted

“for most application”
for most applications

“some contact process sulphuric acid plant where made”
some contact process-based sulphuric acid plants were constructed

“and platinum catalyst slowly eroded”
and the platinum catalyst slowly eroded

“that vanadium pentoxide based catalyst”
that a vanadium pentoxide-based catalyst OR that vanadium pentoxide-based catalysts

“(equation 20)”
Do you mean equation 2?

“and glass tube”
and glass tubing

“three 250 ml flask”
three 250 ml flasks

“heated till white fumes”
heated until white fumes

“sulphur dioxide oxidation is exotermic”
sulphur dioxide oxidation is exothermic

“all the sulphur have burned”
all the sulphur has burnt

“and make acid droplet”
and make acid mists/fine droplets

“most lab preparation”
most lab preparations

“In laboratory, time to time”
In the laboratory, from time to time

“have only little shrinkage during cooling”
exhibits little shrinkage during cooling

“for basic Ph condition”
for basic pH conditions

“require to be partially melted which require a lot of heating.”
but requires being partially melted which requires a lot of heating

“it make insoluble”
it makes insoluble

“Kielsegur help”
Kielsegur helps


“looks like floor”
looks like flour

“until It look like a castable paste”
until it resembles a catsable paste

“casted in is shape, casting can be done in wax impregned wood”
casted in its shape; casting can be done with wax impregnated wood

“cure in”
cures in

“two day”
two days

“to use inert atmosphere for them”
to use them in an inert atmosphere

“it pyrolise to carbon”
it pyrolises to carbon

“require liquid air to distill the nitrogen of the air”
is by the (fractional) distillation of liquid air

“regenerate the copper”
regenerates the copper

“copper powder makes roughly one 850 ml”

copper powder purifies sufficient air to yield roughly 850 ml of pure nitrogen gas


“some other gas”

some other gases/other gases


“most application”

most applications


[Edited on 23-10-2012 by Hexavalent]

ElectroWin - 23-10-2012 at 11:04

How odd,
i went to your web site, http://HClO3Chem.TK to try to download the second volume; but instead of a pdf, i got a pop up to http://adf.ly/CUaId which turned out to be porn spam. this happened when i clicked to the link http://89c8a785.linkbucks.com/
which was supposedly about the chlorates

[Edited on 2012-10-23 by ElectroWin]

Vargouille - 23-10-2012 at 12:49

Yes, it was quite odd. It's almost like it's an infinite loop specifically designed to get a lot of link usage and get money...

I noticed this for both the calcium hydroxide ".pdf" and the chlorate ".pdf". Only the Lab-Scale Industrial Processes (Volume 1) was safe. How odd.

plante1999 - 23-10-2012 at 12:57

Quote: Originally posted by ElectroWin  
How odd,
i went to your web site, http://HClO3Chem.TK to try to download the second volume; but instead of a pdf, i got a pop up to http://adf.ly/CUaId which turned out to be porn spam. this happened when i clicked to the link http://89c8a785.linkbucks.com/
which was supposedly about the chlorates

[Edited on 2012-10-23 by ElectroWin]


Sorry, I just have fixed that. The link intermitted didnt do what they where supposed to do and I just stopped using them. All links should work good now.

Thanks for your Help Hexavalent!

[Edited on 23-10-2012 by plante1999]

Bezaleel - 5-11-2012 at 08:40

Hi Plante1999,

On page 7 of volume 2 you mention the following equation:

2CaOH + 2SiO2 → 2CaSiO3 + H2O

This equation is not balanced, as the left hand side contains 6 oxygen atoms, whereas the right hand side contains 7.


You state in your first post that you have yourself tested all of these processes. When you made your refractory object in this process, you did you manage it to cool down slowly?

plante1999 - 5-11-2012 at 09:13

I made a mistake, I will correct it soon, thank you. Its
Ca(OH)2 + SiO2 -) CaSiO3 + H2O

Yes I did cooled it slowly to prevent stress in the material.

I'm currently working on the volume 3.

Hexavalent - 5-11-2012 at 09:16

Quote: Originally posted by Bezaleel  


This equation is not balanced, as the left hand side contains 6 oxygen atoms, whereas the right hand side contains 7.



The problem is with the formula, not the balancing; the formula of calcium (II) hydroxide is Ca(OH)2, meaning the overall equation is;

Ca(OH)2 + SiO2 → CaSiO3 + H2O

I know this because I had to learn it for my exam last year:)

Bezaleel - 6-11-2012 at 04:19

Ehm, yes, so I had only one eye open ;)

But, plante1999, how did you make it cool down slowly? If you wrap it in a blanket, you'll end up with a home fire.

[Edited on 6-11-2012 by Bezaleel]

plante1999 - 6-11-2012 at 04:44

I have a aluminium melting furnace with vermiculite/fire cement insulation. I simply put the hot piece in the preheated furnace and then turned off the propane. The piece cooled slowly. I guess porous alumina firebrick are suitable too.

plante1999 - 10-11-2012 at 10:41

Some user asked me if I could make few bigger volumes instead of many tiny one. I think it was a good idea, so the next volume should take a very long time to make but it should contain most of the processes in the list. Yield should be included too and maybe some pictures. Some of these processes aren't tested but I'm trying them at the moment, especially the last process.

Hop you like the content and if you have any questions please ask.

Attachment: compound list.pdf (114kB)
This file has been downloaded 1191 times

[Edited on 11-11-2012 by plante1999]

ElectroWin - 13-11-2012 at 14:30

one of these mentions using xylenes; can i substitute mineral spirits?

plante1999 - 14-11-2012 at 13:59

I'm not sure but toluene should work too. It might worth trying it using mineral spirits tough.

Bezaleel - 16-11-2012 at 07:25

Have you already started working on hydrogen through electrolysis? I've been working on that for a few months now, and am now stuck in the process of making an electr(on)ically controlled needle valve.

[Edited on 16-11-2012 by Bezaleel]

plante1999 - 16-11-2012 at 07:45

Yes I did, but I found the reaction to need engineering skills since separating the hydrogen form the oxygen make a pressure differential that push electrolyte in the cathode compartment. I personally preferred the carbon reaction with water. A one way valve for the cathode should fix the problem.

ElectroWin - 17-11-2012 at 11:33

a semi-permeable membrane to separate the half-cells might do?

[Edited on 2012-11-17 by ElectroWin]

lolcat - 27-11-2012 at 20:55

In volume 1, when burning the cinnabar to obtain mercury, what piece of glassware can be used for this? A link or picture would be nice. Also, it says to distill the mercury in a steel retort. What is the reason for this? Can it not be normal glassware?

[Edited on 28-11-2012 by lolcat]

Vargouille - 28-11-2012 at 02:09

There is a picture in the section for burning cinnabar. The piece is called a "combustion tube". I haven't managed to find one cheaply from quartz, which is necessary to withstand the relatively high temperatures that the mercury boils at (356.7C), and to withstand the approximately 10C or 20C overshoot that will get all of the mercury out of the combustion tube. This, incidentally, is why normal glassware should not be used, as this is well out of the normal operating conditions of the glassware. It can be done, if you have particularly high-quality glassware, but I wouldn't want to do it to my own stock. While distilling the mercury, take care not to go over 615C, because arsenic will begin to sublime.

plante1999 - 28-11-2012 at 04:38

I have used a borosilicate combustion tube with success. I recommend alcohol heating. The cinnabar, when heated in an air flow will catch fire, this fire contain a lot of mercury fumes and produce heat. Using a steel retort is optional. Iron retort cannot break by mercury bumping, however glass can.

lolcat - 6-12-2012 at 16:25

I am a bit confused about the combustion tube. Is there a flame in direct contact with the material being combusted, like is there a hole in the combustion tube? Or does the flame just heat up the glass? Which doesn't really make sense, because then how would it combust.

plante1999, do you remember where you bought your borosillicate combustion tube? I found one at, http://www.perkinelmer.com/Catalog/Product/ID/N2411300 , but it seems rather expensive.

Also, in your Bibliography, you mention Ullmann, F. Ullmann’s Encyclopedia of industrial chemistry, 5th ed.; John Wiley & Sons, 1999, I was curious as to how you had access to this source.

[Edited on 7-12-2012 by lolcat]

Vargouille - 7-12-2012 at 02:15

The flame just heats up the glass. It combusts because there is an external air stream done up with glass tubing. But it is an interesting point, because I had brought up earlier that I wasn't sure if combustion was necessary, as I recalled an anecdote where mercury was freed from cinnabar simply by heating, leading sulfur in the vessel.

plante1999 - 7-12-2012 at 03:46

The cinnabar need external heating to combust in air, without air it will only sublime.

For the tube I simply bought a 18mm by 150 borosilicate test tube and I cut the bottom to get a really cheap tube.

Well, I have "some" book in the PDF format...

Vargouille - 7-12-2012 at 11:26

The cinnabar will sublime? As far as I am aware, cinnabar does not sublime to any considerable extent, only convert to the black mercury sulfide at around 344C, which melts at 850C. At least, that's what the CRC says, and it does not mention any sublimation. Incidentally, this casts aspersions on my recollection that cinnabar forms mercury and sulfur when heated in absence of air. Perhaps I'm losing my memory prematurely.

lolcat - 7-12-2012 at 12:16

plante1999 - If you have any pdf's from Ullmanns Encyclopedia of Industrial Chemistry that cover the extraction of mercury from cinnabar, I would be very grateful if you could post it, I would like to read up some more on the whole process.

Lambda-Eyde - 7-12-2012 at 14:24

Quote: Originally posted by lolcat  
plante1999 - If you have any pdf's from Ullmanns Encyclopedia of Industrial Chemistry that cover the extraction of mercury from cinnabar, I would be very grateful if you could post it, I would like to read up some more on the whole process.

Here is the chapter on mercury from Ullmann's, extracted from the whole book kindly provided by solo in the References section.

Attachment: Mercury - Ullmanns Encyclopedia of Industrial Chemistry p. 781-812.pdf (262kB)
This file has been downloaded 2317 times

lolcat - 7-12-2012 at 15:42

Oh! thanks, I didn't know that Ullmanns Encyclopedia was in the resource section, I guess I will need to ask for permission to that forum.
A few questions on plante1999's diagram.
What is the reason for the air pump going through an empty glass bottle before entering the combustion chamber. My only thought is that this might prevent unwanted back flow into the pump itself.
Why is the glass bottle that is directly connected to the combustion chamber in an HCL ice bath, I understand why it is in an ice bath, but why a hydrochloric acid ice bath?
Could a Liebig condenser be attached directly to the combustion tube, and cold water run through the condenser, instead of the glass bottle acting as the condenser? The mercury would still fall into a glass flask and glass tubing would carry away the SO2 to the next bottle.

plante1999 - 7-12-2012 at 17:28

You got it wrigth for the first bottle. The ice/HCl bath cool down to minus 30 degree celcius instead of 0 for normal ice bath, you can use CaCl2 too. A liebig condenser would be hard to clean up, the dirty mercury contain mercury ashs. Mercury ashes is cinnabar dust with 60% + elemental mercury in it. This ash would restrict the mercury flow. This ash can be distilled to get the mercury out of it.

What cinnabar will you use?

If you have any questions, please ask.

[Edited on 8-12-2012 by plante1999]

lolcat - 7-12-2012 at 17:48

http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&item=20033...

That makes sense as why not to use the liebig condenser.
2 questions concerning the HCL/ice bath. Will the ice/HCl bath actually go below zero, to minus 30 degrees as you say?

And why would you want it that cold if that is the case? Sulfur dioxide condenses at -10 degrees and mercury condenses at 356 degrees. So wouldn't there be a fear of the SO2 condensing as well?

plante1999 - 7-12-2012 at 18:02

I didn't saw sulphur dioxide problem, because the gas are extremely hot. Because gas are extremely hot, extremely low cooling is needed to get room temp. in the chamber.

That's good cinnabar.

lolcat - 7-12-2012 at 20:58

Attached is a rough draft of the procedure I will follow, pretty much an adaptation of your plate1999's work. The Erlenmeyer Flasks in the picture are 125 mL each. Its not in the picture, but I think I might place the last glass tube into a beaker of water, to see if any SO2 is leaving the sodium carbonate beaker. Any comments will be appreciated.

Attachment: Mercury from Cinnabar1.pdf (372kB)
This file has been downloaded 809 times

plante1999 - 8-12-2012 at 14:14

It should go alright. But for heating, like I said, you may need something stronger. Time to time I used a propane torch to get to the wright temperature. You may see blue flame in the tube if you heat enough.

Good luck.

plante1999 - 15-1-2013 at 19:32

Look at what I just found:

http://ebookbrowse.com/lab-scale-industrial-process-for-chem...

And I didn't put it there, it seams my pdf are shared without any reference to my website! I'm glad I put a link on the top of the first page!

Any thoughts on this?

Vargouille - 16-1-2013 at 01:28

Well, link's broken, so it's not a problem.

On topic, it is an odd thing to happen. From what I gather, someone who saw your pdf linked it to e-Book Browse. I can't really think of an innocuous reason to do so, considering that the downloads on your site are free.

plante1999 - 17-1-2013 at 04:57

Yea, thats what I wanted to show, there is many link to my PDF on other page than my website.
I guess there is sort of reward for people who put PDF...

plante1999 - 17-1-2013 at 04:57

Yea, thats what I wanted to show, there is many link to my PDF on other page than my website.
I guess there is sort of reward for people who put PDF...