Sciencemadness Discussion Board
Not logged in [Login - Register]
Go To Bottom

Printable Version  
 Pages:  1  ..  54    56
Author: Subject: Preparation of elemental phosphorus
Magpie
lab constructor
*****




Posts: 5812
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 11-10-2017 at 04:23


I like your design, but would make a few changes:
1. Change carbon to aluminum.
2. Monitor all condensers for temperature and control to the optimums.
3. Incorporate cyclone separators where needed to separate gasses from the liquid Phosphorus.






The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
metalresearcher
National Hazard
****




Posts: 486
Registered: 7-9-2010
Member Is Offline

Mood: Reactive

[*] posted on 11-10-2017 at 09:20


This would be a rather compled design. It needs indeed strict temperature control in the condenser. But what is actually the problem that CO and P4 arrive together in the condenser? They don't react with each other and can easily be separated by condensing the P4, as CO remains a gas.



DJT is for the USA and the world as ClF3 is for humans.
View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5812
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 11-10-2017 at 10:27


My suggestions are for producing clean P at high yield, not for convenience of the operator.

Use of carbon vs aluminum will greatly increase gas formation, and decrease the necessary retort temperature. My experiences with aluminum and SiO2 produced a nasty voluminous slag that contaminates the P.

Use of a centrifuge for gas-liquid separation would be wonderful but indeed too complicated. A cyclone might work just as well and be far simpler.

[Edited on 12-10-2017 by Magpie]




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
Assured Fish
Hazard to Others
***




Posts: 193
Registered: 31-8-2015
Location: Noo Z Land
Member Is Offline

Mood: Misanthropic

[*] posted on 11-10-2017 at 21:54


@metalresearcher i think the problem is that the combined pressure of the gasses being produced and the high temp make condensing the P4 a quite challenging, a liebig type condenser may not be enough to condense all the P4 and a large amount may possibly be lost out the top (hence my idea of using a stopchock).

Unfortunately I have no idea just how quickly the reaction proceeds beyond what BluePlanet1 described, what he described seems quite intense.

A possible simple solution, if the condenser is not enough would be to pack the condenser with a material with high surface area such as glass wool.

@Magpie i do like the cyclone idea but im a tad confused as to its operation.
Is the spinner supposed to rotate solely by the pressure of the gases being pushed through or would it have to be electrically driven.
View user's profile View All Posts By User
j_sum1
Super Moderator
*******




Posts: 3788
Registered: 4-10-2014
Location: Oz
Member Is Offline

Mood: Maintaining a semblance of equilibrium

[*] posted on 11-10-2017 at 22:32


A cyclone has no moving parts. It spins the gas into a vortex. Denser material is flung out to the edge and funnels to the bottom. Light gas leaves at the centre top so that gas flow is maintained.

2013042051046249.jpg - 32kB
View user's profile View All Posts By User
Assured Fish
Hazard to Others
***




Posts: 193
Registered: 31-8-2015
Location: Noo Z Land
Member Is Offline

Mood: Misanthropic

[*] posted on 13-10-2017 at 11:42


The cyclone separator would appear to be a lot easier to engineer than i had originally thought.
One problem though: from what ive read on them cyclone separators are only capable of separating particulates or liquid droplets from a gas flow, they cannot separate 2 gasses at all.

This means that we would still need to condense the P4.
A water jacket around the cyclone housing would be the minimum required to accomplish this. Achievable but it makes other methods look more appealing.
View user's profile View All Posts By User
clearly_not_atara
International Hazard
*****




Posts: 1010
Registered: 3-11-2013
Member Is Offline

Mood: No Mood

[*] posted on 13-10-2017 at 12:09


I'm really confused as to why the "just use a longer pipe and submerge it very deep in water" method is not being taken more seriously. Using water eg one meter deep should condense most of the phosphorus. It's not like you have any other condensates to worry about.
View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5812
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 14-10-2017 at 00:11


First the P4 must be condensed using a proper condenser. Then it will drop out the bottom of the cyclone into a water filled receiver. Gasses will leave the top port of the cyclone, hopefully relatively free from P4. Cyclone design will be important, as well as condenser design and temperature.



The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
wg48
International Hazard
*****




Posts: 631
Registered: 21-11-2015
Member Is Offline

Mood: No Mood

[*] posted on 14-10-2017 at 02:50


Quote: Originally posted by Magpie  
First the P4 must be condensed using a proper condenser. Then it will drop out the bottom of the cyclone into a water filled receiver. Gasses will leave the top port of the cyclone, hopefully relatively free from P4. Cyclone design will be important, as well as condenser design and temperature.


So is the problem believed to be that the phosphorus condenses to a fine mist or dust that does not easily settle?

Looking at the short exit pipes and large bubbles in the water I would think cooling is the main problem. One end of the exit pipe is at +1000C with the gaseous CO and P even higher and only about 200mm of air cooled pipe to get the temperature down to say 200C.

The large bubbles so near the surface probably don’t wash out the P or cool it very efficiently particularly given the flow of CO.


View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5812
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 14-10-2017 at 03:40


Yes, condenser design is important and less than optimum design was the cause of many of my troubles. Even though I generally used aluminum as reductant the gas/P/slag rush could be explosive. I used an air condenser made of 1/2" electrical conduit (EMT).

Gruson did excellent work with the help of his science teacher and some welding craftsmen. Here is a link to his work: https://www.sciencemadness.org/whisper/viewthread.php?tid=65...

Unfortunately his photos are no longer available.




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
e14
Harmless
*




Posts: 7
Registered: 23-10-2016
Member Is Offline

Mood: No Mood

[*] posted on 8-2-2018 at 03:27


Shouldn't this thread be erased? The DEA lists it. So, how easy is this stuff easy to make?
View user's profile View All Posts By User
Sulaiman
International Hazard
*****




Posts: 1776
Registered: 8-2-2015
Location: England
Member Is Online

Mood: No Mood

[*] posted on 8-2-2018 at 03:45


Compared to the risk of the experiment I would not worry about the DEA, unless you plan to go into production.



When doing chemistry, don't forget basic physics.
View user's profile View All Posts By User
wg48
International Hazard
*****




Posts: 631
Registered: 21-11-2015
Member Is Offline

Mood: No Mood

[*] posted on 8-2-2018 at 03:51


But don't do it on your front lawn or poison your neighbours .
View user's profile View All Posts By User
Assured Fish
Hazard to Others
***




Posts: 193
Registered: 31-8-2015
Location: Noo Z Land
Member Is Offline

Mood: Misanthropic

[*] posted on 8-2-2018 at 16:28



Quote:

Shouldn't this thread be erased? The DEA lists it. So, how easy is this stuff easy to make?


:o The DEA can go fuck themselves, phosphorous is an element and a fundamental one for life, why the hell would we restrict information because a bunch of degenrate apes want to misuse phosphorous for illegal or immoral purposes.

That aside, the items on that list are not illegal, we are technically allowed to make them, however the DEA or other government agencies from what i understand do also have the right to lay charges on us if we are caught with possession of those materials.

If you spend some more time lurking the older threads you will likely come across several threads discussing the preparation of scheduled compounds such as lysergic acid and anthranilic acid.
The forum cares little for the bickering stupidity of mortals.
View user's profile View All Posts By User
Bert
Super Administrator
*********




Posts: 2593
Registered: 12-3-2004
Member Is Offline

Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".

[*] posted on 8-2-2018 at 17:13


e14 is one of a number of low post, dormant accounts that reactivated recently, posting gibberish or, if intelligible, quite different from their earlier activity.



Rapopart’s Rules for critical commentary:

1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.

Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).

View user's profile View All Posts By User
Rogeryermaw
International Hazard
*****




Posts: 654
Registered: 18-8-2010
Member Is Offline

Mood: No Mood

[*] posted on 2-3-2018 at 10:12


derped. sorry

[Edited on 2-3-2018 by Rogeryermaw]
View user's profile View All Posts By User
Rogeryermaw
International Hazard
*****




Posts: 654
Registered: 18-8-2010
Member Is Offline

Mood: No Mood

[*] posted on 2-3-2018 at 10:18


mmmm phosphorus! deelish! man...this thread has moved quite a bit since i've been away.

Quote: Originally posted by clearly_not_atara  
I'm really confused as to why the "just use a longer pipe and submerge it very deep in water" method is not being taken more seriously. Using water eg one meter deep should condense most of the phosphorus. It's not like you have any other condensates to worry about.


it doesn't take much fluctuation in temperature to cause a suction. i would be afraid of a steam explosion blasting hot slag and gaseous phosphorus all over.
View user's profile View All Posts By User
zed
International Hazard
*****




Posts: 1556
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline

Mood: Semi-repentant Sith Lord

[*] posted on 2-3-2018 at 11:54


Easy to make? Hard to make?

Seemingly impossible for some of us to make Phosphorus, but not very difficult for Rogeryermaw.

Has a nice series of Youtube videos. https://www.youtube.com/watch?v=mibM4WUx74Q
View user's profile View All Posts By User
 Pages:  1  ..  54    56

  Go To Top