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Offline dudeman

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Sodium Sulfate synthesis...
« on: October 23, 2009, 03:55:26 PM »
I want to make this stuff so I get the ingredients. Although I doubt either are pure I mix them together and see the reaction stated on wikipedia... Clear fumes that turn white are emitted and the solution bubbles. The sulfuric acid is of 93% purity and the salt is meant for the pool so this is being done without pure reagents. The end produt still has small chunks of unreacted salt that wont seem to react even though there is a small layer of sulfuric acid that precipitates to the top of the solution. I mix this layer into the salt layer and the chunks dont seem to react.

My main question is this. I know that there is sodium sulfate in this mixture but it has sulfuric acid around it... How would I remove the sulfuric acid? Would I wash the mixture with a solvent such as chloroform or naptha? I don't want to procede without first knowing the right solution to add as I dont want to waste my good stuff... I have naptha that I can use if thats the right stuff... Oh and I also have acetone... Thanks for any help...

Dudeman


Edit...

Alright I decided to try soemthing and wasted some good stuff... Anyways I added water to the solution and swashed it around... This ended up crating more hydrochloric acid fumes which I think was the result of the water dissolving some of the salt from the chunks... in the end I have quite a bit of salf material still at the bottom of the jar. I poured through a coffee filter into a glass cup. this ended up not filtering anything and what I found was that the only chunks of anything I had was just salt... Because the only thing i had left after the addition of water was chunks of salt... I did this thinking that the sulfate would absorb the water not the other way around so I ended up just pouring it out... Next time I wont use water... That's the whole point of this stuff is to absorb the water out of other chemicals... Does anyone know what solvents would be used to remove the sodium sulfate from the sulfurica acid and salt solution if this is even the way to make it?
« Last Edit: October 23, 2009, 04:54:04 PM by dudeman »

Offline nj_bartel

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Re: Sodium Sulfate synthesis...
« Reply #1 on: October 23, 2009, 05:25:54 PM »
Please write down your procedure.  I am so confused as to what you did exactly.

Offline dudeman

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Re: Sodium Sulfate synthesis...
« Reply #2 on: October 23, 2009, 07:15:59 PM »
I took the sulfuric acid and added salt to it until it stopped reacting... Then I added water to find that the solid particals that I thought were sodium sulfate dissolved... so I poured it out... I tried again but this time I added naphtha and all that did was sit on top of the solution... I decided naphtha doesn't do anything so tried acetone. The acetone had an effect but I only added 50 ml so I didn't know for sure and poured the whole thing out because the naphtha was on top of it and I was frustrated because I was covered in hydrochloric acid from the reaction lol... I went inside and washed off... Potent gas this reaction gives off...

Edit:

I thought i was supposed to get a salt cake from this... But it doesn't make a salt cake... It just turns tan and foams up and then does nothing...

Offline nj_bartel

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Re: Sodium Sulfate synthesis...
« Reply #3 on: October 23, 2009, 07:27:38 PM »
If you boil the solution to get rid of the water, the HCl should come out of solution too, first.

Offline dudeman

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Re: Sodium Sulfate synthesis...
« Reply #4 on: October 23, 2009, 07:40:54 PM »
HCI is not in it... What happens is the Sulfuric acid reacts with the salt to make sodium sulfate and Hydrogen chloride which reacts with the water in the air to form HCI... So it is not the HCI that I am worried about it the the 7% contamination of the sulfuric acid + the excess sulfuric acid...

Also I am pretty sure sulfuric acid doesn't evaporate or boil off... according to a video I saw on you tube... So if anyone here knows of a way to extract the sodium sulfate out of the sulfuric acid that would be good... Also I know that it would be wise to distill the sulfuric acid drain cleaner I'm using but I don't want to bother with all that as I don't have a laboratory grade distillation kit... The only thing my distillation kit is good for is distilling ethanol as the tubing is made of copper... So distillation is out of the question unless you guys tell me that it's safe...

Offline dudeman

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Re: Sodium Sulfate synthesis...
« Reply #5 on: October 23, 2009, 10:15:10 PM »
Ok so... I almost died...  :-X

BUT I MADE SODIUM SULFATE!!!

All I did was put some sodium hydroxide in a cup and then poured an equal portion of sulfuric acid onto it... I did this right outside my back door... So what I noticed was that it wasn't doing anything so i swirld it around with my hand and swashed it all together... then I sat it down and stood up and then like 1 second later it started to fiz really hard so i jumped back and slammed the door just as it started to go nuts and splater s#*$ all over! I look out of my window and see that the sodium hydroxide had grown into the coral reef lookin thing that I beleive to be sodium sulfate... Makes sence right? SODIUM hydroxide + SULFURIC acid = SODIUM SULFATE + some insane amount of white gas fumes that I wass very lucky to dodge... Don't worry I had my safty glasses on...

So I took most of the coral reef out and then left the rest of the stuff at the bottom in there... I put the sodium sulfate into some tissue wrapping papper that I just got to make sure that it stays dry... I also put it in a plastic bad and stuff the bag with more paper for added dryness...  ;D

The stuff on the bottom had the consistancy of the coral reef but was just a tad harder and when i flipped over the cake there was what looked looked to be some embedded sulfuric acid...  so I just tossed it...  :P

Offline dudeman

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Re: Sodium Sulfate synthesis...
« Reply #6 on: October 23, 2009, 10:20:13 PM »
So im guessing that the only way to make this stuff from the salt I was using is to heat it up! like that rt guy said but yeah i dont think it was reacting... well it was but it wasn't... All I know is that the other way is better easier and way faster... It's like "poof" then you have this stuff... pretty cool...

Offline nj_bartel

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Re: Sodium Sulfate synthesis...
« Reply #7 on: October 23, 2009, 10:30:47 PM »
Please don't kill yourself.

Let's draw out the reactions.

H2SO4(aq) + NaCl -> NaHSo4(aq) + HCl(aq)

Sorry for the confusion - the first reaction produces sodium bisulfate, not sodium sulfate.  At any rate, assuming you react stoichiometrically, you'll be left with your sodium bisulfate and hcl in aqueous solution.


For the reaction you just did... Yes, you should have your sodium sulfate now.  Just a dangerous reaction the way you ran it.  Dilute H2SO4 mixed dropwise with dilute NaOH would be a better idea.

Offline dudeman

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Re: Sodium Sulfate synthesis...
« Reply #8 on: October 23, 2009, 10:45:54 PM »
Haha I liked it... made me feel all wizard like...  :D

Ok so what your saying is the reaction did not go strait to sodium sulfate it went from sodium bisulfate + hcl then this turned into the gas and sodium sulfate... Well to me it went poof and turned into coral reef but i get what your saying... I just went over the whole section of time in my head in slow motion and actually noticed what you were saying...

Edit:

and btw I think you should try it... it was so AWESOME I couldn't beleive it... after it stoped reacting the glass cracked from the heat... I wasn't even able to pick it up a minute later... So I picked it up with a towel and used a fork to break off the coral reef stuff into another cup... I must say this was the most kick ass thing I have ever done with chemicals...

Offline dudeman

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Re: Sodium Sulfate synthesis...
« Reply #9 on: October 24, 2009, 07:48:49 PM »
Hello everyone sorry to make a reply but I thought I might let you know about something that happened to the sodium sulfate I made... I put a few chunks into a little thing used for holding ketchup at resturants and pourd on some acetone... I was supprised that the crystals started turning blue... Not dark blue but just a slight blue hue... I'm not sure if this is the crystals becoming hydrated or if there was an impurity that reacts with acetone to form a blue molecule. Anyone know?

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