The Bucket Cell - Start to Finish

[WSM]

I now need to cut the pieces apart and turn the pipe sections on the lathe to clean up the sealed end, with a slight, rounded chamfer on the sealed outer edge. After the ends are cleaned up, I plan to drill lots of tiny holes in the sealed pipe to form my filters.

 

I cut the excess, flat PVC stock away from the pipe nipple sections, and carefully turned them on the lathe to form the basic shape of my tank filters.

 

 

I also threaded one of the filter bodies into the bulkhead adaptor mounted in the bottom of the tank, for a visual of how it'll look when the filter holes are drilled in it and it's mounted.

 

 

This is about like I envisioned it, and should work well to keep the system working correctly.

 

WSM

Edited September 8, 2016 by WSM

[WSM]

I took one of the filter blanks and started to drill lots of holes in it in a random pattern. It ended up looking like this:

 

 

I originally planned to use a smaller drill, but the cordless drill I used wouldn't hold a drill bit smaller than 1/16" so I used a #51 drill bit (068") and we'll see how that works. It occurred to me later that I could've used a Dremel tool and used a #60 drill (0.040" or about 1 mm). I may do that with the next one.

 

This is what the filter looks like (hand tight; I should use a strap wrench and tighten it fully) in the bulkhead adaptor in the bucket tank:

 

 

I need to set up the external plumbing and try it out.

 

WSM

[WSM]

I've taken the rough bucket tank and plumbed it for a brine preparation vessel.

 

Top view

 

Bottom view

 

Inside top

 

Inside bottom

 

The idea is to draw the water through the salt in the bottom of the tank. The brine flows downward into the pump and is pumped up to the top of the tank and directed to move counter clockwise in the tank, to facilitate dissolving the salt with a high rate of water flow.

 

Now I need to fill the bucket tank with salt and distilled water, and see how well things mix with the new setup.

 

More later...

 

WSM

 

Edit: I also have a large brine tank made up; a duplicate of the one used in the sodium chlorate cell experiment. I planned to run the second large polypropylene brine tank (about 100 liter capacity) as part of a larger scale salt purification and drying system for making clean, dry salt as feedstock (and salt replenishment for the liquor) for my sodium chlorate system (to keep the chlorate levels high, while keeping contaminants low).

 

I may try it with the bucket tank first before going full-scale with the larger, secondary brine tank.

Edited September 18, 2016 by WSM

[MrB]

Drawing brine through the salt, and dumping it up top might be attractive since it, in theory at least, wont disturb the salt as much. But what about the solids that get sucked in to the pump-line? Those holes will either clog with to large particles, or let smaller particles in, creating wear on the pump, or even stalling it.Is there a problem related to fluidizing the setup, and have the salt suspended in the brine? If not, placing the pump return facing the bottom, and collecting clear brine up top for the pump-line might be easier to live with. More sensitive to fluctuating fluid levels, which isn't really a problem where i'm used to seeing this tech, as filter systems for aquariums. (Using sand, or bead media)

 

Since the media in a reactor of this kind is exposed to a slight grinding action, i think it would hit equilibrium faster as well, and save you time on producing the brine. Not sure if that actually will be a problem, running for chlorates takes longer then producing brine, but still...

 

Just thinking out loud, you probably already considered it. But i wanted to at least try and be helpful, since i enjoy reading about your progress so much.

Good luck.

B!

[WSM]

Drawing brine through the salt, and dumping it up top might be attractive since it, in theory at least, wont disturb the salt as much. But what about the solids that get sucked in to the pump-line? Those holes will either clog with to large particles, or let smaller particles in, creating wear on the pump, or even stalling it.Is there a problem related to fluidizing the setup, and have the salt suspended in the brine? If not, placing the pump return facing the bottom, and collecting clear brine up top for the pump-line might be easier to live with. More sensitive to fluctuating fluid levels, which isn't really a problem where i'm used to seeing this tech, as filter systems for aquariums. (Using sand, or bead media)

Since the media in a reactor of this kind is exposed to a slight grinding action, i think it would hit equilibrium faster as well, and save you time on producing the brine. Not sure if that actually will be a problem, running for chlorates takes longer then producing brine, but still...

Just thinking out loud, you probably already considered it. But i wanted to at least try and be helpful, since i enjoy reading about your progress so much.

Good luck.

B!

 

 

Thanks for your comments, MrB. The filter on the bottom of the bucket tank doesn't have openings that are actually on the bottom of the tank. I think the holes in the PVC filter I made start roughly 3/4" (19 mm) above the tank bottom.

 

The magnetically coupled, chemical handling pump I'm using has a fairly high flow rate and can handle the small salt crystals that may go through without much difficulty. It's proven itself in the brine tank of my sodium chlorate experiment, to dissolve the salt crystals faster than merely soaking the salt in still water, and I expect it'll be the same with the bucket tank.

 

I think part of the success while using this style of pump lies in the fact that it's not a positive displacement pump and the slippage in the volute makes it more forgiving in operation. The design of it also allows for easy disassembly for servicing and repair (plus replacement parts are readily available at a reasonable cost).

 

Part of the reason I place the pump near the bottom of the tank is that these pumps aren't self-priming, and need the head pressure to operate correctly; but once they start to pump, they do a great job moving the liquids.

 

I see the bucket tank as a useful tool for preparing many sorts of water based solutions, or as a reservoir for additions of necessary solutions to larger systems (or even a water tank for field operations).

 

Thanks again to OldMarine for the suggested setup/improvement on my idea. The irrigation valve box stand might also be useful for a modified bucket cell setup for a sodium chlorate cell.

 

WSM

Edited September 20, 2016 by WSM

[WSM]

Last night my wife and I were shopping for snacks to eat while watching a movie together. When we passed the water aisle, I noticed gallons of distilled water were on sale. She wondered what I was thinking, buying twelve gallons of distilled water.

 

I'm grateful that, even though she doesn't share my passion for scientific things, at least she's tolerant of my interests (and me of hers).

 

WSM

[OldMarine]

Would charcoal pre-filtered reverse osmosis water be pure enough for your purpose?

[MrB]

Since it's pretty much the way they make the "distilled water" you can buy in bulk, it should do fine. In reality they run a DI filter after the membrane to remove the last 0.000% of contaminants, mostly silicates.

It's a lot slower then just grabbing the next jug, but also a lot cheaper. Just get a TDS meeter, and keep track of the quality of the product.

Depending on water-pressure where one lives, use a booster-pump. Makes a HUGE difference.

B!

[WSM]

Would charcoal pre-filtered reverse osmosis water be pure enough for your purpose?

 

On the one hand, yes. I've used RO water for my KCl to KClO₃ runs without any problems. On the other hand, in a NaClO₃ system where one is more likely to recharge the depleted electrolyte and continue running it, even the lower amount of contaminants will eventually increase to where they're a problem (contaminating the final product).

 

So, in my opinion it's better to use distilled (or deionized) water for the sodium chlorate system. This is especially so where the sodium chlorate is used to produce perchlorates which are designated for making pyrotechnics grade potassium perchlorate, which we want in the purest form possible.

 

This is also why I'm attempting to purify the salt (NaCl) used, as well. I want to see if I can make a product as pure, or purer than is available commercially from industry. This is the reason for all the attention to detail; to do at least as good as industry, and better if we can.

 

I've obtained a small, stainless steel distiller; and instead of using tap water to fill it, I start with RO water. This is to keep the tank cleaner than tap water would leave it (and less cleanup is required later). In a different direction, if I get to it, a dedicated RO system with a special pre-filter (ion exchange type) [or is that post-filter?] will remove the remaining 5% of dissolved solids and yield DI (de-ionized) water for use in the system, with zero dissolved solids.

 

A lot of thought is going into this and I think the results will be worth the effort.

 

WSM

Edited September 26, 2016 by WSM

[OldMarine]

Before WallyWorld and other stores started offering water jug filling stations I owned several stand alone dispensing machines. I still have enough parts in storage to assemble a couple of complete units. These used a pump to assist the R/O process. De-ionizing was terribly expensive then so was not an option for my budget.

[WSM]

Since it's pretty much the way they make the "distilled water" you can buy in bulk, it should do fine. In reality they run a DI filter after the membrane to remove the last 0.000% of contaminants, mostly silicates.

It's a lot slower then just grabbing the next jug, but also a lot cheaper. Just get a TDS meeter, and keep track of the quality of the product.

Depending on water-pressure where one lives, use a booster-pump. Makes a HUGE difference.

B!

 

Yes, that's where my thoughts are headed. I have a couple TDS meters (I got the first several years ago) and they've opened my eyes to not only the quality of water going into my system, but also the wretched quality of my tap water here. We use RO water for cooking and drinking, and it's easy to taste the difference. The household RO system removes 95% of the dissolved solids from our tap water, leaving about 20-50 ppm of dissolved minerals in the drinking water (which tastes FAR better than what comes out of the tap ).

 

The distilled water I either buy or make has 0.0% dissolved solids, according to the reads of the TDS (total dissolved solids) meter. I agree and think the DI system would produce much more pure water and cost even less, in the long run.

 

WSM

 

Caution: don't drink distilled or deionized water. Water is naturally "hungry" for minerals, and if you drink pure water it'll strip the minerals from your body and cause harm. It's okay to cook with, but don't drink it. Our bodies need essential minerals, so salt with calcium and magnesium is good for consumption. Removing those minerals from the salt used in our electrochemical cells, is in an effort to improve the purity of our yield and produced materials.

[WSM]

Before WallyWorld and other stores started offering water jug filling stations I owned several stand alone dispensing machines. I still have enough parts in storage to assemble a couple of complete units. These used a pump to assist the R/O process. De-ionizing was terribly expensive then so was not an option for my budget.

 

It sounds like you've got a treasure trove of useful materials on hand. Excellent!

 

Let us know what you end up doing with them.

 

WSM

[MrB]

[or is that post-filter?]

 

Post. If you pre-filter, it will eat your media at a scary rate...

 

De-ionizing was terribly expensive then so was not an option for my budget.

 

eBay, DI media for preparing water for aquarium. It's quite cheap, and last a while.

 

Caution: don't drink distilled or deionized water. Water is naturally "hungry" for minerals, and if you drink pure water it'll strip the minerals from your body and cause harm. It's okay to cook with, but don't drink it. Our bodies need essential minerals, so salt with calcium and magnesium is good for consumption. Removing those minerals from the salt used in our electrochemical cells, is in an effort to improve the purity of our yield and produced materials.

 

Ask anyone who spent a bit of time on a US hangar ship, if they had serious salt deficiency. The same goes for submariners, and to some extent astronauts. (They all drink distilled water. However, astronauts actually may take salt supplements. I believe it's a part of the food today, but a couple of years ago it was a pill, taken once a day.) The reality is, that if your living on a mountaintop, (Naturaly low salinity in the local water) and have a very low salt intake from your daily foods, you might get a salt deficiency, but given a "normal" diet, you have enough salt in your daily food intake, that it wont matter. Drink away. That said, people die from competitions where you try to drink the most tap water. This is "normal" tap water, with normal salinity, and still it gets to the point where the salt level in your body gets to low, and the electrical properties of your tissue breaks down, to the point where the nerve impulses to make the heart beat, or to make the lungs take a breath, just doesn't reach the muscle tissue, and you die. The point being, don't drink excessive amounts of water at once, regardless of the salt content.

 

B!

[WSM]

Post. If you pre-filter, it will eat your media at a scary rate...

eBay, DI media for preparing water for aquarium. It's quite cheap, and last a while.

Ask anyone who spent a bit of time on a US hangar ship, if they had serious salt deficiency. The same goes for submariners, and to some extent astronauts. (They all drink distilled water. However, astronauts actually may take salt supplements. I believe it's a part of the food today, but a couple of years ago it was a pill, taken once a day.) The reality is, that if your living on a mountaintop, (Naturaly low salinity in the local water) and have a very low salt intake from your daily foods, you might get a salt deficiency, but given a "normal" diet, you have enough salt in your daily food intake, that it wont matter. Drink away. That said, people die from competitions where you try to drink the most tap water. This is "normal" tap water, with normal salinity, and still it gets to the point where the salt level in your body gets to low, and the electrical properties of your tissue breaks down, to the point where the nerve impulses to make the heart beat, or to make the lungs take a breath, just doesn't reach the muscle tissue, and you die. The point being, don't drink excessive amounts of water at once, regardless of the salt content.

B!

 

Post filter it is, then (thanks).

 

Okay, my caution about drinking distilled water may be overblown (rainwater is essentially distilled water, after all). Cooking with distilled water is okay because the minerals in the food are drawn into the water and it all becomes easier to assimilate.

 

It does appear that deionizing, post-filters are much more affordable these days; and a good option to add to an RO system for producing DI water. If you don't want to (or can't afford to) invest in such a system, buying (or making) distilled water is the next best option.

 

On the face of it, it seems silly to use pure water and add an impure salt to it; but it really does help in producing a more pure end-product (the less junk put in, the lower the level of contaminants in the resulting product, especially if the electrolyte is recycled).

 

WSM

Edited September 27, 2016 by WSM

[Arthur]

You'd be eating an odd diet if RO water caused you problems -but then people living remotely on ship or space ship do get an odd diet!

 

RO water can be better than DI water, but all depends on the way you keep the system running.

 

One patent I read said that accumulated debris was precipitated during the process of recycling the used liquors. Add some Barium salt and all the insoluble salts will slowly ppt out And other chems!

[WSM]

You'd be eating an odd diet if RO water caused you problems -but then people living remotely on ship or space ship do get an odd diet!

RO water can be better than DI water, but all depends on the way you keep the system running.

One patent I read said that accumulated debris was precipitated during the process of recycling the used liquors. Add some Barium salt and all the insoluble salts will slowly ppt out And other chems!

 

I'm used to the RO systems for home use (about 95% solids removal), are you referring to industrial setups? If my understanding is correct, DI water has zero dissolved solids, just as distilled water does.

 

I'm familiar with the technique of using BaCl₂ solution for removal of hexavalent chromium from cell liquor by filtration of the barium chromate precipitate. What other ions are removed by the process?

 

WSM

Edited September 29, 2016 by WSM

[WSM]

On the face of it, it seems silly to use pure water and add an impure salt to it; but it really does help in producing a more pure end-product (the less junk put in, the lower the level of contaminants in the resulting product, especially if the electrolyte is recycled).

 

If you use distilled or DI water in purification steps, you're not adding unknown contaminants from the water. There's enough unwanted material in the salt and we can remove it by chemical and physical means to end up with a brine, free of interfering ions, to use as the electrolyte in our cells.

 

At some point I intend to purify my KCl as well. I want to see if I can meet and exceed industry's level of purity for pyrotechnics grade oxidizers. We'll see what, if any, difference it makes...

 

WSM

[WSM]

Okay, I put three gallons of distilled water into the bucket tank and started the pump. Everything looks normal so I added 12 pounds (5.43 kilos) of salt water pool salt (NaCl) and one more gallon of distilled water for a total of four gallons, or more than 15 liters of brine (360 ml per liter). Surprisingly, it takes about three pounds per gallon to make my brine (American measures seldom come even close to matching S.I. measures).

 

I do see some small crystals flowing through the clear vinyl tubing, but it's no problem. I'll let the bucket tank circulate for a while and see how well it works (but, so far so good).

 

WSM

Edited September 30, 2016 by WSM

[WSM]

Okay, I put three gallons of distilled water into the bucket tank and started the pump. Everything looked normal so I added 12 pounds (5.43 kilos) of salt water pool salt (NaCl) and one more gallon of distilled water for a total of four gallons, or more than 15 liters of brine (360 g per liter). Surprisingly, it took about three pounds per gallon to make my brine (American measures seldom come even close to matching S.I. measures).

I do see some small crystals flowing through the clear vinyl tubing, but it's no problem. I'll let the bucket tank circulate for a while and see how well it works (but, so far so good).

WSM

 

For some reason, as the pumped fluids cycled through the bucket tank, foam collected on top of the brine in the tank. I'm not sure why unless there was either some residue left in the new bucket or, more likely, there's some unwanted contaminating material in the pool salt.

 

My initial thought is to scoop the scum off the surface of the brine and continue running the pump till the salt is completely dissolved. After that, I plan to purify the salt with sodium carbonate solution and possibly a little sodium hydroxide solution also, as industry does, to remove unwanted mineral contaminants by filtration. The next step is to neutralize the purified brine with hydrochloric acid, to remove any alkalinity in it (and create a little more NaCl in the bargain).

 

After I create the pure sodium chloride brine, the plan is to dry the pure salt for use in the next run of the sodium chlorate experiment. If the bucket tank system proves itself as a brine preparation component, I'll step up the salt purification process to a larger scale using my 100 liter tank system (number two).

 

I have a lot (maybe a couple hundred pounds) of impure sodium chloride water softener salt, which I can convert to pure salt and brine to use in my sodium chlorate experiments. I believe starting with high purity materials will assure a higher quality end product. We'll see...

 

WSM

Edited October 16, 2016 by WSM

[WSM]

For some reason, as the pumped fluids cycled through the bucket tank, foam collected on top of the brine in the tank. I'm not sure why unless there was either some residue left in the new bucket or, more likely, there's some unwanted contaminating material in the pool salt.

My initial thought is to scoop the scum off the surface of the brine and continue running the pump till the salt is completely dissolved. After that, I plan to purify the salt with sodium carbonate solution and possibly a little sodium hydroxide solution also, as industry does, to remove unwanted mineral contaminants by filtration. The next step is to neutralize the purified brine with hydrochloric acid, to remove any alkalinity in it (and create a little more NaCl in the bargain).

After I create the pure sodium chloride brine, the plan is to dry the pure salt for use in the next run of the sodium chlorate experiment. If the bucket tank system proves itself as a brine preparation component, I'll step up the salt purification process to a larger scale using my 100 liter tank system number two.

I have a lot (maybe a couple hundred pounds) of impure sodium chloride water softener salt, which I can convert to pure salt and brine to use in my sodium chlorate experiments. I believe starting with high purity materials will assure a higher quality end product. We'll see...

WSM

 

So I located my aquarium net and scooped the foam off the top of the brine in the bucket tank, and ran the circulating pump for 24 hours. There's no more foam and the salt is nearly all dissolved.

 

I can see some silt on the bottom of the tank, so I plan to decant the clear brine off and place it in a separate bucket where I'll treat it with sodium carbonate solution, wait for the precipitated salts to settle and then vacuum filter the brine. Next comes a pH test of the purified brine and final adjustment of the pH to neutral, if it's not already there.

 

The treated brine is likely to be alkaline and adding enough HCl to correct it to a pH of 7.0, will leave a pure sodium chloride solution for either running in a sodium chlorate cell (as a starting electrolyte) or drying it to a pure salt for adding to the depleted electrolyte from former runs, to replenish the chloride level without adding unwanted ions.

 

WSM

Edited October 19, 2016 by WSM

[WSM]

The treated brine is likely to be alkaline and adding enough HCl to correct it to a pH of 7.0, will leave a pure sodium chloride solution for either running in a sodium chlorate cell (as a starting electrolyte) or drying it to a pure salt for adding to the depleted electrolyte from former runs, to replenish the chloride level without adding unwanted ions.

With the high temperature sodium chlorate experiment I'm working on, once the brine is purified and neutral, that's the end of my preparations. I use the pure brine for the starting electrolyte and for chloride replenishment; eliminating the need to dry the salt for adding to my lower temperature sodium chlorate cell.

 

Also, (according to the patent) the sodium chlorate crystals are supposed to drop out at higher temperatures (45°C), eliminating the need for expensive refrigeration to harvest the product. I think my yield should be good (even better) at room temperature. We'll see...

 

I can see that the bucket tank will serve me well in this venture.

 

WSM

Edited December 6, 2016 by WSM

[WSM]

With the high temperature sodium chlorate experiment I'm working on, once the brine is purified and neutral, that's the end of my preparations. I use the pure brine for the starting electrolyte and for chloride replenishment; eliminating the need to dry the salt for adding to my lower temperature sodium chlorate cell.

Also, (according to the patent) the sodium chlorate crystals are supposed to drop out at higher temperatures (45°C), eliminating the need for expensive refrigeration to harvest the product. I think my yield should be good (even better) at room temperature. We'll see...

I can see that the bucket tank will serve me well in this venture.

WSM

 

This is especially true since the capacity of my bucket tank is roughly equal to the expected volume of the prototype high temperature NaClO₃ cell I'm building to test the viability of this type of cell described in US patent 3043757 (Circa 1962), but using a DSA anode and titanium cathodes, instead of the platinum plated titanium and stainless steel electrodes called out in the patent.

 

My thoughts are to use my high-end power supply and feed the cell using the constant current (CC) mode. As the cell runs at roughly the boiling point of the electrolyte, the liquor will automatically concentrate the product as the water is both consumed and evaporated.

 

According to the patent, when the electrolyte level reaches roughly 50% of the starting level, the concentration of the sodium chlorate should be between 750 and 800 g/l. After harvesting the crystals which drop out at room temperature, the "depleted" electrolyte is recharged with purified brine and continues to run.

 

This is a much simpler system to operate than the original one I did earlier this year, and if I arrange to recover the large amount of water vapor coming out of the vent (separating it from the gaseous H₂ byproduct of the process), I can recycle it to make fresh brine.

 

I'm looking forward to setting up and starting a test run of this system.

 

WSM

Edited December 10, 2016 by WSM

[MrB]

This is a much simpler system to operate than the original one, and if I arrange to recover the large amount of water vapor coming out of the vent (separating it from the gaseous H₂ byproduct of the process), I can recycle it to make fresh brine.

 

Is there a problem with simply running a vent through a glass condenser for cooling? If the temperature delta isn't great enough just having it hooked there passively, a (very) small aquarium pump, and a small radiator for PC water-cooling would make for a closed loop system that should keep it at ambient temperature 24/7, for years to come. A system for collecting the distilled water, and venting of the gas byproduct should be easy enough at that point.

Also, the water-cooling loop really should have some corrosion inhibitor in it. Pick one with a color you like, it will look... "mad scientist", in the glass condenser.

B!

[WSM]

Is there a problem with simply running a vent through a glass condenser for cooling? If the temperature delta isn't great enough just having it hooked there passively, a (very) small aquarium pump, and a small radiator for PC water-cooling would make for a closed loop system that should keep it at ambient temperature 24/7, for years to come. A system for collecting the distilled water, and venting of the gas byproduct should be easy enough at that point.

Also, the water-cooling loop really should have some corrosion inhibitor in it. Pick one with a color you like, it will look... "mad scientist", in the glass condenser.

B!

Thanks, MrB.

 

I was thinking along those lines also (but hadn't said anything about it here, yet). Actually, a bucket tank could work quite well as a water reservoir for a closed-loop water cooling system (as you described).

 

WSM

[Arthur]

Check whether any of the feed brine will need heating before you dump heat to anywhere wasteful. Brine at 80C needs heating when you make and store brine at 20 - 30C ambient.