387 replies to this topic

[fishy1]

Your brown liquid electrolyte might have a bit of something useful in it, like naclo3/4. You can remove the precipitate by filtering.

Fugenhobel-I reckon you mean gouging rods.

P.S what's in that container labled KNO3? It looks horribly like urine.

[newtoolsmith]

Sure I will filter the electrolyte hot and then cool it down to get the Chlorate out. I think I wont wait for perc to form.

Urine?? Fishy1, what do you think about me?

It is dirty NaOH solution I used to prepare the GSLD anodes. The colour is given by "dissolved" carbon particles.

The KNO3 labeling was from prios use and should really be corrected. I normally label all containers very precise to avoid mistakes.

I added the NaOH container to catch Cl2 out of the exhaust.

The exhaust is guided deep into the NaOH solution and I hope, the Cl2 will react with the NaOH:

4NaOH + 2Cl2 -> 4NaCl + 2H2O +O2 or something like that.

I noticed that Cl2 is very nasty and hurts when breathed in. Dont ever do that!!


I think you are right fish1, gauging rod is the correct name for the carbon sticks I use. On frogfots homepage you can see them unplated:

frogfots chlorate synthesis

His homepage is interesting due to many nicedatails. Enjoy it!

MFG
newtoolsmith

Edited by newtoolsmith, 01 October 2006 - 10:07 AM.

[newtoolsmith]

Hi Friends,

the cell has run for 56 hours. The current decreased a bit and is 18,75 Ampere now.

Half the NaCl should be converted to NaClO3 now.

Its hard for me to wait another three days!

The cell is much to slow for me. I have many good characteristics but patience is not one of them.

Next days I will search for a micro wave transformator and give him a new secondary winding. It should be able to deliver 200A@4VAC and the following rectifier gives about 5,7VDC.

The 200A will require 1000cm? anode aerea.

We will see...

MfG
newtoolsmith

[leosedf]

newtoolsmith
You said this will give about 1kg NaClO3 which seems fine to me for 7 days since i cannot find it here.
A supplier here in Greece told me that he has to call the police if someone asks for it. (damn)

[fishy1]

Sure I will filter the electrolyte hot and then cool it down to get the Chlorate out. I think I wont wait for perc to form.

Urine?? Fishy1, what do you think about me?

It is dirty NaOH solution I used to prepare the GSLD anodes. The colour is given by "dissolved" carbon particles.

The KNO3 labeling was from prios use and should really be corrected. I normally label all containers very precise to avoid mistakes.

I added the NaOH container to catch Cl2 out of the exhaust.

The exhaust is guided deep into the NaOH solution and I hope, the Cl2 will react with the NaOH:

4NaOH + 2Cl2 -> 4NaCl + 2H2O +O2 or something like that.

I noticed that Cl2 is very nasty and hurts when breathed in. Dont ever do that!!
I think you are right fish1, gauging rod is the correct name for the carbon sticks I use. On frogfots homepage you can see them unplated:

frogfots chlorate synthesis

His homepage is interesting due to many nicedatails. Enjoy it!

MFG
newtoolsmith

Even better for you, the reaction of chlorine and naoh is

3 Cl2 + 6 NaOH ==> 5 NaCl + NaClO3 + 3 H2O

So you'll be making chlorates very inefficiently with that method, and some might be recoverable. At the very least, you could boil it down when it tests neutral (PH=7ish) and electrolyise it instead of just plain nacl solution so you'll get a helping hand and save some energy.

"Urine?? Fishy1, what do you think about me?"

You know what I think about you.

Edited by fishy1, 01 October 2006 - 08:31 PM.

[BrightStar]

newtoolsmith, I'm really impressed that you have made so much progress with the GSLD electrodes.

Can I just warn though that the chlorine gas from these cells is MUCH more harmful than one might think. I half gassed myself at the age of 11 electrolysing NaCl solution in a misguided attempt to fill a balloon with H2 / O2 mix at only 3A cell current, and will never forget it.

To quote the FDA, "In animal models of chlorine gas toxicity, immediate respiratory arrest occurs at 2000 ppm, with the lethal concentration for 50% of exposed animals in the range of 800-1000 ppm. Bronchial constriction occurs in the 200-ppm range with evidence of effects on ciliary activity at exposure levels as low as 18 ppm. With acute exposures of 50 ppm and subacute inhalation as low as 9.0 ppm, chemical pneumonitis and bronchiolitis obliterans have been noted. Mild focal irritation of the nose and trachea without lower respiratory effects occur at 2.0 ppm."

ie lethal effects in animals at 0.1% concentration, ranging to irritation at 0.0002% ...

Edited by BrightStar, 03 October 2006 - 10:37 AM.

[newtoolsmith]

@fishy1:

You know what I think about you.

Do I?

@Bright Star:

Of course the cell will have to run outside. Even running it inside the garage would be too dangerous.

As I told, I unfortunately breathed in some chlorine and had little pain for about half a day. The dose was very low but it was still enough to cause some damage.

So again for everyone who tries electrolysis: Be very careful.

MfG
newtoolsmith

[leosedf]

Anyone knows where i can find lead nitrate and copper(II)nitrate?

[newtoolsmith]

@leosedf:

I dont know where to buy lead- or coppernitrate. I made them by adding HNO3 to lead or copper. The acid has to be hot therefor!! Very nasty operation.

If you need small amounts I could give you some. Lets say 250g or so.

But, to tell you the truth, I am not very happy with that since leadnitrate is very, very toxic as all water soluble lead compounds are. Are you sure to handle it with enough care? The forum doesnt want to loose its members.

Anyway I am always happy to help someone.

MfG
newtoolsmith

[leosedf]

I am not ready to proceed with electrolysis yet, i am looking for info about the whole proccess, trying to find chemicals (nitrates, acids etc) and do a lot's of reading for this since it will be my first time doing this.
Are there any links describing the proccess to create those nitrates?
About safety: any special thing i need to take care? except off course gloves masks etc.?

Edited by leosedf, 02 October 2006 - 07:31 PM.

[newtoolsmith]

@leosedf:

I didnt find any links when I tried to make the nitrates.

For the lead nitrate I trieb to simply put some lead (sheets for roof sealing) into nitric acid. The result was, that a closed nitrate layer formed on the leads surface and no further reaction took place.

I did this using a PE canister and decided to put it into a water bath and heat it to approx 80?C. This worjed fine but gives a huge amount of N2O fumes.

DO THIS OPERATION OUTSIDE ONLY OR YOU WONT BE ABLE TO SEE THE FINISHED NITRATE ANYMORE!!!!!

The copper reacts with the nitric acid even at room temperature.

The reaction is described here: UK Rocketry & Pyro forums: lead nitrate

Gloves, eyeprotection and plastic clothes are a must.

Dont try to heat nitric acid in a stainless pot - I never did it and Im sure I wont!



Some words about my cell:

The current has decreased to 18 ampere now. Approximately 1800 amperehours have passed the cell. Assuning a efficiency of 91% all the NaCl will be converted to NaClO3 now. Surely this is not real. I ecpect a efficiency of only 55% and so only 72% of the NaCl are converted yet.

PS: I will open a new topic to discuss high current power supplies today.

MfG
newtoolsmith

[leosedf]

Ok thank you for the info.
I am thinking of using a PC power supply (40A at 5V).

[newtoolsmith]

Hi friends,

a new cell has been constructed.

The bucket holds 10 litres and already has a airtight lid.

The whole cathode assembly is made from 1.4571 stainless steel. The screws as well.

The sealing is made of two components silicone.

The cathode is 23cm long, 5mm thick and 5cm wide.

No anode has been prepared yet but it will come soon...

Have a look:





MfG
newtoolsmith

[leosedf]

Pretty nice job may i say!

You are many steps ahead of me, i am still trying to find anodes!

[pkhow]

Some advise for any one who wants readily available anodes for chlorate production and I have has reasonable success making per chlorates although it is hard on the material. The anode material used for Domestic swimming Pool chlorination MMO electrodes are designed to operate in very low saline so will give years of Production making chlorates. As most anodes will now operate as low as 2000~3000ppm(2~3grms per Litre) you will find that you can run them in weaker KCL solutions. If running on to perch take care not to run them buried in the precipitating material. This will cause loss of some of the MMO coating which is easy to filter as I looked on it as a running cost but was able to minimize this by removing the precipitate.
You shouls be able to make a cell capable of 20~30amps for well under $100 that will last for years making chlorate and with care a reasonable time in perch production.

Pkhow