Simple, cheap large scale chlorine generation

Author: Subject: Simple, cheap large scale chlorine generation Simple, cheap large scale chlorine generation


There are many ways to generate chlorine gas at home. Some use calcium hypochlorite and I have always found this to be exquisitely inconvenient for large scale generation because of the stirring (or should I say non-stirring?) issue/problem.

Chlorox gives chlorine when acidified. It's about 5% NaOCl. Swimming pool "shock" treatments are about 10% NaOCl.

My chlorine generator is a glass 5 gallon water cooler bottle. I think it was all of $10 or $11 dollars a few years back. Place a long cylindrical stir-bar in the bottom, place it on a sturdy magnetic stirrer and add 4 - 4 1/2 gallons of 5 - 10% NaOCl. The top is closed with a 2 hole rubber stopper. One hole has a provision for a 1 liter sep. funnel full of conc. HCL (the pool supply store is your friend) and the other is for Cl2 to exit.

Start dripping HCl into the stirred liquid. A few minutes pass while the generated Cl2 saturates the solution and it becomes green-yellow. When it becomes saturated, Cl2 begins to leave through the Cl2 exit tube. Refill the sep. funnel with HCl solution as necessary (before it runs out).

You can do the math to see how much Cl2 is possible. I didn't bother as I knew that I needed to simply keep the chlorine coming until the liquid refluxed at the right temperature. A rough statistic: I dichlorinated about 400 mL of xylenes with one generator containing 4 1/2 gal. 10% NaOCL.

After the reaction is done, feed the generator output outside while it finishes. The next day, (CAREFULLY) pour the solution into a large plastic bucket outside. Allow a day or two for Cl2 to escape and dispose of the residual brine solution down a drain.

The Cl2 can be dried using a conc. H2SO4 trap.



Nice generator, I didn't realize that you could get conc HCl from a pool store. Also what are you using chlorinated xylene for?

Where does he mention HCl from the pool store?

Quote: Originally posted by Dan Vizine  One hole has a provision for a 1 liter sep. funnel full of conc. HCL (the pool supply store is your friend) and the other is for Cl2 to exit.


Sorry, didn't notice that!

The pool store is the best supplier for conc. HCl at low cost. It isn't quite as concentrated as normal commercial reagent grade but quite close (within a few %). Also it's the the best place for 10% NaOCl and bulk NaHCO3.

(also, FYI, Lowe's is the local place to find NaOH (drain cleaner. RIP Red Devil Lye). Hardware stores and similar often stock conc. H2SO4 for about $11/liter (also as drain cleaner/opener)).

The bis(chloromethyl)benzenes were made a few years back on a contract basis for a customer I initially met on eBay. Actually, 1.4- bis(chloromethyl)benzene was the original request but I didn't have a convenient source for p-xylene so he settled for a mixture at reduced cost which he said he'd purify. I don't know the purpose (exactly) but the terminology he used made me think it was being used as a cross-linker or for some other similar, polymer-related work. This material has no known drug or explosive connection that I'm aware of, so I didn't need to pry into motives too much.



[Edited on 9-4- by Dan Vizine]

Electrolysis of NaCl in solution is the cheapest way to make it chlorine on the large scale.

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One problem is, that method is rather slow so you have to have a way of storing chlorine. Also, won't most of the chlorine produced dissolve in the hydroxide to produce hypochlorite? Although, I guess you could get around this by placing the cathode near the top of the solution and the anode at the bottom. Bert

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posted on 9-4- at 08:11

Quote: Originally posted by Zyklonb  Electrolysis of NaCl in solution is the cheapest way to make it chlorine on the large scale.

If one has a good sized DC power supply and the materials already? That's certainly possible. You have done this? If so, you should post your lab notes here, so others may learn. Of course, with the links or citation of other materials you learned from.

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

My questions-

Did you use a pressure equalizing addition funnel for the hydrochloride acid?



If using H2SO4 dryer inline, bubbled through the acid, or merely passed over?

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Quote: Originally posted by Bert   Quote: Originally posted by Zyklonb  Electrolysis of NaCl in solution is the cheapest way to make it chlorine on the large scale.

If one has a good sized DC power supply and the materials already? That's certainly possible. You have done this? If so, you should post your lab notes here, so others may learn. Of course, with the links or citation of other materials you learned from.

I did make some with this method, yes. But only as a byproduct of a sodium hydroxide producing cell. I did use some of the produced the chlorine, but most I simply scrubbed out. I didn't need large amounts of it at the time. I did not quantitatively test the purity, nor did I dehydrate it, as I had no real use for it at the time.
I believe I used this set-up. I still have everything put-together, so I could try it again, but this time, intentionally for the chlorine, and making NaOH as a byproduct. I can't remember what voltage or amperage I used, but I'm sure it was not the best. I will test thest some more later.

Bert

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posted on 9-4- at 09:01

Quote: Originally posted by Zyklonb  
I could try it again, but this time, intentionally for the chlorine, and making NaOH as a byproduct. I can't remember what voltage or amperage I used, but I'm sure it was not the best. I will test thest some more later.

Two thoughts: ALWAYS TAKE NOTES. It REALLY helps down the road-

And do you know enough electrochemistry to work out just how much electric power it takes to electrolyze a mol of Cl2? Would your long term interest be better served by learning some theory, or in an experiment...

See problem example #2 here:

You might need a bigger power supply?

Your parents might be surprised at the electric bill?

[Edited on 9-4- by Bert]

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 (-).

Hi Bert,

Your questions-

Did you use a pressure equalizing addition funnel for the hydrochloride acid?
No, I don't have one as large as a liter. I used a sep. funnel with a tiny strip of paper towel in the stopper hole, along side the stopper. The addition rate is slow (controlled by how fast my chlorination would consume it) so this minute leak lets enough air in. The HCl layer seals the chlorine inside. If left unattended, make sure there is always HCl in the funnel or chlorine escapes here rather than push through H2SO4 and chlorination mixture.


If using H2SO4 dryer inline, bubbled through the acid, or merely passed over?
Passed over it? I would never consider this adequate. It was bubbled through a column of acid about 4 - 5 inches deep (use suck-back trap).

[Edited on 9-4- by Dan Vizine]

Don't produce chlorine from electrolysis. It sucks to capture it, and it's so contaminated with oxygen as to be not worth it (Up to 10%, if the thread in PrePub is to be believed).

Personally, for producing chlorine, I prefer battery paste (MnO2) or bleach and HCl.

Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd

Yes, I have been taking notes for some time now, I often look back at my earlier work, and regret not taking notes.
I will spend some time working out the math, and getting a better understanding of electrochemistry. I currently do not know exactly how to find out, but the link you provided, was very helpful.

I definitely need a new power supply, At the moment, what I've been doing is hooking up small PSU's in parallel to achieve higher amps, and in series to achieve higher volts.
Correct me if I'm wrong, but it looks like I'll need a total of 5.29 volts for the whole reaction. Is this right?
I will start off with very low amps, (in the order of 5-10 amps) so I doubt the electric bill will be very dramatically increased.

Here is a path to Cl2 I have discussed previously and performed on many occasions, namely create a so called Bleach battery. This would qualify as cheap and simple if you has some spare chlorine bleach around, copper (new US pennies are pure Cu plate), vinegar and Aluminum foil. One can also produce some electricity as well.

Steps:

1. Whip up some Hypochlorous acid by mixing bleach (NaOCl) and vinegar (which contains Acetic acid HAc) in the volume ratio 1.4 parts of 5% vinegar to one part of 8.25% extra strength chlorine bleach.

2. To the HOCl add a piece of copper metal which will function as the cathode and an Aluminum source to act as the anode (finely cut up Al foil, for example, will also work).

3. Lastly, add a little (or perhaps more, see discussion below) salt to act as the electrolyte to get things started.

My take on the chemistry:

The creation of Hypochlorous acid:

NaOCl + HAc --> HOCl + NaAC

And, on the major electrochemical reactions:

6 H2O <--> 3 H3O+ + 3 OH-

At anode:

Al + 3OH- &#; Al(OH)3 + 3 e-

At the cathode (copper):

3 HOCl + 3 H3O+ + 3 e- &#; 3/2 Cl2(g) + 6 H2O

for an implied net reaction of:

3 HOCl + Al --> Al(OH)3 (s) + 3/2 Cl2 (g) Eo net = 3.93 V

This battery cell is theoretically capable of generating 3.93 volts.

Reference: see http://www.exo.net/~pauld/saltwater/ and http://sci-toys.com/scitoys/scitoys/echem/batteries/batterie... and also http://www.dtic.mil/dtic/tr/fulltext/u2/d.pdf

There are also many side reactions. One with respect to increased chlorine production of interest is that with an excess of chloride, a possible competing reaction to the cathode reaction which consumes Hypochlorous acid and hydronium ions, and can enhance the chlorine yield:

HOCl + H3O+ + Cl- &#; Cl2 (g) + 2 H2O

The general nature of chlorine generation is nearly nill at the beginning (an induction period) followed by a consistent Cl2 generation. This is actually favorable for 'large scale' as one is given time to close and adequately seal (or move) the Cl2 generator. This is a potential issue with the hypochlorite/HCl method which is rapid (IMHO, possibly inviting an accident on a large scale).

[Edited on 9-4- by AJKOER]

Quote: Originally posted by Zyklonb   At the moment, what I've been doing is hooking up small PSU's in parallel to achieve higher amps, and in series to achieve higher volts.
Correct me if I'm wrong, but it looks like I'll need a total of 5.29 volts for the whole reaction. Is this right?
I will start off with very low amps, (in the order of 5-10 amps) so I doubt the electric bill will be very dramatically increased.


I find PC tower type PSUs perfect for everything.
You get 5v at 30 Amps
12v at (about) 10 Amps and they're cheap and rugged.

I think the one use was found in a discarded PC tower case in a bin, but they are dirt cheap on ebay too.

You just need to short out one of the pins to ground to get it to run.
I will go get mine and see which pin it is.

Just checked my PC power supply.

The big connector has 20 pins, in two rows of 10.
if you look Into that connector, with the latch-clip at the top, then you need to short the pin that is 4th from the Left, top row, to the 5th from the left, top row. That makes it run. Un-short and it stops.
The pin on the left, bottom is the only square pin.

The outputs on the Other leads (4-pin connectors) are +5V @ 30 Amps on the red wires, and +12V @ 15 Amps on the yellow wires, with 0V on the black wires.

You can also find +3.3V @ 20 Amps on the 20-pin connector if you have a voltmeter.

That's my power supply salvaged from the bin.

Your mileage will probably vary (likely you'll get more Amps from yours)

Sodium hypochlorite generator is a device used to generate sodium hypochlorite solution, which is commonly used for the disinfection of swimming pools, drinking water and industrial wastewater. Sodium hypochlorite is a strong oxidizing agent with bactericidal, disinfectant and bleaching properties.

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The working principle of sodium hypochlorite generator is to produce sodium hypochlorite by electrolyzing salt water.

Specifically, a sodium hypochlorite generator usually consists of an electrolyzer in which an anode and a cathode are inserted. The electrolyzer is filled with brine, usually a sodium chloride (NaCl) solution.

When an electric current is turned on, an electrolytic reaction occurs between the anode and cathode. At the anode, chloride ions (Cl-) are oxidized to chlorine gas (Cl2), while at the cathode, water is reduced to produce hydrogen gas (H2) and hydroxide ions (OH-).

The chlorine gas produced reacts with water to form hypochlorous acid (HClO) and hydrochloric acid (HCl). Hypochlorous acid is the active ingredient of sodium hypochlorite, which has strong oxidizing and bactericidal disinfecting ability.

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In order to improve the efficiency of sodium hypochlorite generation, generators usually employ measures such as increasing the area of the electrolyzer, improving electrode materials, and optimizing the concentration and temperature of the electrolyte. In addition, the production and concentration of sodium hypochlorite can be regulated by controlling the current density, electrolysis time and flow of electrolyte.

The generated sodium hypochlorite solution can be transported to the water to be treated for disinfection, sterilization or oxidation through an appropriate piping system.

The operating principle of the sodium hypochlorite generator is based on an electrolytic chemical reaction which, through proper design and operation, can effectively produce sodium hypochlorite solution for water treatment and other related applications. It is important to note that when operating and using the sodium hypochlorite generator, it is important to follow safe operating procedures in order to prevent chlorine leakage and other safety issues. It is also necessary to select the appropriate generator model and operating conditions according to the specific water treatment needs and water quality characteristics.

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Advantages of sodium hypochlorite generator:

1. No need to use dangerous chemicals, such as chlorine, high safety.

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2. Sodium hypochlorite generator can produce high concentration of sodium hypochlorite solution with good disinfection effect.

3. Sodium hypochlorite generator also has the advantages of simple operation and easy maintenance.

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 When using the sodium hypochlorite generator, it is recommended that the equipment be regularly inspected, cleaned, replaced and other maintenance work to effectively extend its service life and improve operational efficiency.

The cleaning steps of sodium hypochlorite generator are as follows:

1. Turn off the generator and cut off the power supply;

2. Remove the electrode and membrane of the generator. 3;

3. soak the electrodes and membranes in clean water and gently brush them with a brush to remove the dirt on the surface;

4. Place the main body of the generator in clean water, add appropriate amount of cleaning agent and soak for 1-2 hours. 5;

5. Rinse the main body of the generator with clean water until it is clean;

6. install the electrode and membrane back into the generator, turn on the power and check whether the equipment is running normally.

When cleaning the sodium hypochlorite generator, you need to pay attention to safety, avoid the use of corrosive cleaning agents, and at the same time, strictly comply with the operating procedures of the equipment to avoid damage to the equipment.

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 The maintenance and repair of sodium hypochlorite generator should pay attention to the following issues:

1. Regularly check the equipment: regularly check the operating condition of the equipment, check whether the pressure, flow, temperature and other parameters of the equipment are normal, check whether the sealing of the equipment is good, if there is any abnormality, it should be dealt with in time.

2. Regular cleaning of the equipment: the sodium hypochlorite generator will produce some sediments and impurities during operation, which need to be cleaned regularly. When cleaning, you can remove the electrode and membrane, soak it in water, and gently brush it with a brush to remove the surface dirt. At the same time, you can also put the main body of the generator into clean water, add the appropriate amount of cleaning agent, soak for 1-2 hours, and then rinse with clean water.

3. Regular replacement of electrode and membrane: Electrode and membrane are one of the core components of sodium hypochlorite generator, which can affect the performance of the equipment and the quality of output. Generally speaking, the service life of electrode and membrane is 1-2 years, and they need to be replaced regularly.

4. Pay attention to safety: when maintaining and servicing the sodium hypochlorite generator, it is necessary to pay attention to safety, avoiding the use of corrosive cleaning agents, and at the same time, strictly observing the operating procedures of the equipment to avoid damage to the equipment.

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5. Pay attention to the environmental temperature and humidity: the operating environment temperature and humidity of the sodium hypochlorite generator will also affect the performance of the equipment and the quality of output. Generally speaking, the operating environment temperature of sodium hypochlorite generator should be controlled between 5-40&#; and the humidity should be controlled below 80%.

6. Regularly add electrolyte: Sodium hypochlorite generator needs to consume electrolyte during operation, which needs to be added regularly. When adding electrolyte, it should be operated according to the instruction manual of the equipment to avoid adding too much or too little.

The above are some of the problems that need to be paid attention to in the maintenance of sodium hypochlorite generator, it is recommended to carry out reasonable maintenance according to the actual situation of the equipment, in order to prolong the service life of the equipment and improve the operational efficiency.

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