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Author: Subject: Thy famous tubes - a scrapyard approach
Organikum
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shocked.gif posted on 12-3-2004 at 09:59
Thy famous tubes - a scrapyard approach


I n this thread I will document an approach to build a multipurpose furnace tube by the most simple means without any hard to get parts or catalysts. The tube shall be used in oxidations/dehydrogenations, like toluene to benzaldehyde/benzoic acid, ethylalcohol to acetaldehyde/acetic acid and more. It is by no means sure that it will work well also I am sure it WILL actually work more or less. The approach aims for simplicity and selectivity, say purity of product, the actual yield per pass is not important here. Unreacted substrate will be refed and if higher throughput is wanted the tube can simply be made bigger or preferable multiple tubes may be used.

Here a first picture of the rawmaterials which I plan to use.



I will post pictures of every single step of building this - this tells more than 1000+ words I believe, but one point may be disclosed in advance:
It is a "boilerless" design I will try to implement here for safety and simplicity.
:D

here we go




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[*] posted on 12-3-2004 at 10:17
Hey!


I'm doing basically the same thing, only difference is that my burner will only be burning sulfur.

My approach is basically the same, apart from material choices.

And dare I suggest an addition to your general purpose burner? Well, I'll do it anyway: Add an air dessicator somewhere in the air pump feed path. I'd suggest a CaCl2 column. It's not really general purpose if you feed the odd water molecule from time to time... :)

You can see some of my ideas at
http://species8472.dyndns.org/so3/so3.html

Edit: I should really submit some pictures of my scrapyard-contents-built copper melting capable propane burner..... it really kicks. In lack of a picture, it's basically a Reil burner with an adjustable air feed blower. Melted a distillation borosilicate vessel by accident once....
:o

Edit2: Whoooooaaaahhh!!! My weblog just started vomiting access lines like a maniac!


[Edited on 2004-3-12 by axehandle]

[Edited on 2004-3-12 by axehandle]




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[*] posted on 12-3-2004 at 10:47


Quote:

I'm doing basically the same thing


Oh!
Really?




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[*] posted on 12-3-2004 at 11:39


Yes, really. Well, not <i>exactly</i> the same, but still... it's a strange coincidence, no?

It's funny how people who think somewhat alike often take on the same thing at the same time... like trying to call another at the same time, deciding to build something, etcetera....




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[*] posted on 12-3-2004 at 11:53


OK, let's see... What is the blue stuff? Why do you need steel wool?
What is the orange gadget?

Humm... I understand the tube will be made of copper and you will insert the glass tube inside of it as needed, is that right?

You wouldn´t, by any chance, be in need of a thermostat, would you?

Have I ever told you about the wonders of dentist´s phosphate cement?

axehandle, I gess I found a new victim.
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[*] posted on 12-3-2004 at 11:56


Tacho, are you planning on shoving 30 thermostats down Organikum's throat as well? :)

To be honest, I don't feel like a victim, you have been a great help to me, especially with the molten salt thermostat. <b>Very</b> impressive and innovative work. Needless to say, I'll use it.

Edit: Btw, copper isn't inert enough. Organikum, I suggest you use osmium-plated iridium instead. Much easier.

[Edited on 2004-3-12 by axehandle]




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[*] posted on 12-3-2004 at 12:53


ehem....

if you two look into some of my older posts you may find that tubes are not really new to me.......
:P
Quote:

It's funny how people who think somewhat alike often take on the same thing at the same time... like trying to call another at the same time, deciding to build something, etcetera....

Eh, thus honors me, but I just need some benzaldehyde, thats all....
;)

[Edited on 12-3-2004 by Organikum]




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[*] posted on 12-3-2004 at 13:10


No, there is no glasstube to be inserted into the coppertube, why should this be done?

The orange thingie is a hairdryer, 350W, somehow oldfashioned.....
Also there is a dimmer for comtrolling the temperature, some coppersulfate, a toaster (400W) with nice ceramictubes for heating which make isolation between the coppertube and the heatingpart neglectable and some steelwool which is bound to serve as preheating and condensation enhancer - it will be pushed in the relevant parts of the tube....


FYI



:P:P:P:P

[Edited on 12-3-2004 by Organikum]




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[*] posted on 12-3-2004 at 16:38


Hot steel wool is not known for it's inert nature.
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[*] posted on 13-3-2004 at 01:57


unionised wrote:
Quote:

Hot steel wool is not known for it's inert nature.
Btw. you didnt bother reading my first post where I descriped for what purpose I am building this tube furnace, did you?



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[*] posted on 13-3-2004 at 02:23


Thanks axehandle. I just tested it and it is still OK.

Organikum,

I attached a drawing of two possibilities. Maybe I got it all wrong. Using the search engine here is a pain, because everytime you go back, the page has expired and you have to do it again. Searching all your posts is not an option.

Take a look and tell me which, if any, are you planning to built.

Tubeoptions.jpg - 12kB
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[*] posted on 13-3-2004 at 07:58


Organikum,
So far as I can tell from this thread (and you don't seem to have included a reference to any others) your first post starts with the words "In this thread" and ends with "here we go.
It doesn't mention steel wool in between those phrases.
It does talk about oxidation and I presume that you will be using air as the oxidant (again, it isn't specified).
Steel wool is not known for tolerating "hot air".
Please let me know what it is that I haven't read.
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[*] posted on 13-3-2004 at 10:55


The (stainless btw.) steelwool is for preworming toluene or ethylalcohol at about 100°C to 150°C, I doubt this will hurt in any way. This is a tube for ORGANIC oxidations, the steelwool is not in the reactor itself (and if it will with coated by copper/copperoxide).

But I made an quick experiment and heated the wool for 30minutes with my hot-air pistol which is rated at 500°C. Nothing happened. So I guess that steelwool can stand hot air very well.




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[*] posted on 13-3-2004 at 11:57
My experience


Hello,

Wow,that resembles the makings of a furnace i once built.



When opperating my furnace for the uses mentioned previous,I toyed with various catalyst composition and substrates,-
My first attempt being that of simply attatching a copper tube filled with copper scrub pads to the top af a flask and heating the tube until red hot with a stove element, then passing vapour through this,resulting in fruity aromas in the vapour trap and that was about all.

I found that in low-tech applications a nice catalyst was produced by simply steaming(in a kitchen steamer) some copper scrub pads over vinegar,and then reducing the
acetate coating on the pads, in a fashion not so dissimular to the method you suggested in the acetaldehyde thread,e.g
heat and hold,heat an hold to +-450c.

The beauty of a furnace of this design,is that one can controll the heat,making for
better catalyst production and selectivity.


A better catalyst was produced by steeping activated filter carbon into a hot Cu acetate sollution and then heating until dry,but not at a high enough temp or over a long enough duration to reduce the acetate to oxides.
I would then fill my tube with this carbon support and then top the tube up with more acetate sollution.
Id slowly crank the heat tube to its highest temp,along the way holding the temp every 100deg or so for 3-4 hours at a time.
Let it cool,Invert the tube and then repeat a time or two more.
I dont remember the precise details,
but I got the idea from a patent I found which decribed the entire process,including furnace design/dimensions etc.
Unfortunately,I never atempted to activate the catalyst by passing H2 over the catalyst.

I also tried using bought copper oxides without any of the activation steps,without nearly as much success as the home-preped catalyst.
I think much to do with that was the inhibited flow rate of the vapour stream,
due to being careless and simply coating,or dusting some ground scoria with the oxide and using that as is.
Basically clogged the tube.




I am interested to see how you work such a device without a boiler.
I assume you will include an air-port,pre tube?
I found this seemed to help the process quite substantially if a LIGHT stream of air was introduced.

Sorry Org Ill stop shitting in ya thread now.
Carry on.
Look forward to your picture essay.


Thats a funky toaster btw.

[Edited on 13-3-2004 by ballzofsteel]

[Edited on 13-3-2004 by ballzofsteel]
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[*] posted on 13-3-2004 at 12:19


Very interesting project...
Eagerly awaiting reports of progress.
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[*] posted on 13-3-2004 at 13:54


Thanks Ballz, was helpful what you wrote. The copper-acetate patent is known to me, it is US2002/0143213A1, if I am right....
As told, I am sfter the most simple way now...not sure how it will work though.

The tube will work like a carburator, the fan blows air in, a small nozzle/tube inserts toluene/EtOH and some heated steelwool makes sure all is well mixed and in gasphase when it hits the hot catalyst.

Pictures will be made furtheron to show the howto. First run is tomorrow night so everything works well. :D

Here we go.




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[*] posted on 13-3-2004 at 16:16
OT


Quote:

Eh, thus honors me, but I just need some benzaldehyde, thats all....

No, it honours me.




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shocked.gif posted on 14-3-2004 at 07:39


This resembles my ideas best:



Courtesy Polverone.

Somebody traveled through time, stole my ideas and wrote an article in the past. Its always the same....
;)




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[*] posted on 14-3-2004 at 16:41


Just on the off chance that someone is interested I made a tube furnace too.
I got a foot of half inch brass tube, filled it with granular copper oxide, wrapped it with filter paper (Whatman's GF/A) and then wound on nichrome wire (about 4.2 ohm/ metre). I put a thermocouple against this and then more layers of the same paper. I then wrapped it with glass cloth and finally put it in a pyrex tube.
I connected the nicrome to a 50 V transformer (100W IIRC) that was controlled with a phase angle controller.
I turned up the voltage until the meter connected to the thermocouple said 300C.
I had hoped to use it to oxidise ammonia to nitrogen. Unfortunately (from my point of view) it gave a mixture of NO and NO2.
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[*] posted on 15-3-2004 at 02:47


Quote:

I had hoped to use it to oxidise ammonia to nitrogen. Unfortunately (from my point of view) it gave a mixture of NO and NO2.

Which could be very useful for using the lead chamber process for H2SO4 production, without using xNO3!

Edit: Or for making 68% nitric acid...


[Edited on 2004-3-15 by axehandle]




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[*] posted on 15-3-2004 at 07:13


unionised, you have to heat the tube to a red glow for the HN3 to nitrogen oxidation, this is best done by an propane burner.

There must be a thread somewhere here on nitrogen production (as inert gas) under my name.

ADDON:
Hey! I think its great that more members are going to play with the hot tubes! They are nifty devices and sooo useful in many ways - collecting and sharing our experiences will bring us a big step foreward in whatever direction we want to go!

[Edited on 15-3-2004 by Organikum]

-----------------------------------------

Note to other members: This might be one of Orgies evil plans to grab world domination. Be careful and use your tinfoil hat!

[Edited on 15-3-2004 by vulture]




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[*] posted on 15-3-2004 at 14:12


And for fuck's sake, don't BUY a propane burner. You can build one from scrap plumbing and some brass rod for next to nothing. If anyone's interested, I'll document my monster burner on my homepage. That was an RFC.



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[*] posted on 15-3-2004 at 14:29


Quote:

If anyone's interested, I'll document my monster burner

Interested.
I.
Am.

:D
Dont think I havent seen it Vulture.......




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[*] posted on 15-3-2004 at 14:34


Very well. I'll begin now. There will shortly be a section on my homepage titled "Monster Propane Burner". :)



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[*] posted on 15-3-2004 at 15:18
Done.


http://species8472.dyndns.org/burner/burner.html

Edit: If anyone wants to see the flame of burning hell, I could, with some longer network cable to the Axis camera server, take pictures. Suffice to say, it's <b>VERY</b> hot...

Edit2: And it <b>gobbles</b> propane too fast for my economy. I'll have to buy a 0.6mm drill....

[Edited on 2004-3-15 by axehandle]

[Edited on 2004-3-15 by axehandle]




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