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plante1999
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[*] posted on 7-10-2012 at 09:41
Lab scale industrial processes


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 2898 times


Attachment: Lab scale industrial processes Volume 2.pdf (151kB)
This file has been downloaded 1864 times

[Edited on 24-10-2012 by plante1999]




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Vargouille
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[*] posted on 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.
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plante1999
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[*] posted on 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]




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[*] posted on 7-10-2012 at 14:32


Great stuff Plante1999. I'm really looking forward to the next editions. :)
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[*] posted on 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.
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Hexavalent
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[*] posted on 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




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[*] posted on 10-10-2012 at 14:54


This is good news, as it is often hard to get reagents, on a budget. thanks
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Hexavalent
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[*] posted on 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]




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[*] posted on 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]
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[*] posted on 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.
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plante1999
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[*] posted on 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]




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[*] posted on 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?
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plante1999
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[*] posted on 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.




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Hexavalent
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[*] posted on 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:)




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[*] posted on 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]
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plante1999
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[*] posted on 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.



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plante1999
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[*] posted on 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 1073 times

[Edited on 11-11-2012 by plante1999]




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[*] posted on 13-11-2012 at 14:30


one of these mentions using xylenes; can i substitute mineral spirits?
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plante1999
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[*] posted on 14-11-2012 at 13:59


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



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[*] posted on 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]
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[*] posted on 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.



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[*] posted on 17-11-2012 at 11:33


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

[Edited on 2012-11-17 by ElectroWin]
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[*] posted on 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]
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[*] posted on 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.
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[*] posted on 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.



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