Making potassium perchlorate could be done by electrolysis of sodium chloride through the chlorate, and finally the double decomposition with potassium chloride, but here I will show you an another way for making potassium chlorate using household bleach.
All you will need is household bleach, potassium chloride and a big container.
First, pour at least a liter of household bleach in the container.
Then boil it for at least 15 minutes.
Finally, add potassium chloride until there is no more potassium chlorate precipitating out of the solution.
Filter to gather the potassium chlorate and let it dry.
Here is what's going on. Household bleach is a solution of sodium hypochlorite (NaClO) and heating leads to decomposition in sodium chlorate (NaClO3) and sodium chloride (NaCl).
Now adding potassium chloride (KCl) leads to a double decomposition between NaClO3 and KCl giving potassium chlorate (KClO3) that is a lot less insoluble than NaClO3, thus precipitating out of the solution.
The KClO3 can be used as is after drying or can be put into an electrolysis cell to give potassium perchlorate (KClO4). The solubility of KClO3 and KClO4 are very low so that there will be no separation possible until the end of the electrolysis.
But there is a way around this, you can make a saturated solution of KClO3 and let run the electrolysis until all the KClO4 is precipitated, filter and let dry all the KClO4.
Do again the procedure until you have made the desired amount of KClO4.
This procedure is not suitable for ammonium perchlorate because ammonium chlorate is VERY DANGEROUS AND UNSTABLE SO NEVER PUT ammonium chloride into the boiled bleach.
Sunday, August 12, 2012
Monday, August 6, 2012
Curiosity touched down the Martian soil
What an amazing news : Curiosity, the rover the size of a 4x4 has finally touched down the martian soil at 5h31 GMT after 8 months traveling through space.
All went like scheduled and here is the first image sent by the rover :
To the bottom, we can distinguish the edge of the Gale crater where the rover landed this morning.
All went like scheduled and here is the first image sent by the rover :
Friday, July 27, 2012
How to make a lead dioxide electrode for perchlorate synthesis
Here is a way I use to make my lead dioxide electrode
Lead dioxide forms on pure lead in dilute sulfuric acid. It use the same electrolysis procedure as to make ammonium perchlorate, however parameters change.
To make it, plug a lead electrode (a tube or a plate can do the job) to the + of the generator at about +1.5 V. Use any of those materials as cathode (- of the generator): copper, stainless steel or any other materials able to conduct electricity.
The electrodes are immersed in dilute (30%) and flowing sulfuric acid. To make it flow, you can use a fitted with a little blade like a mixer. The speed should be like a little swirl touching the electrodes. This avoid pitting the electrodes.
The electro deposition is carried out with a constant current at about 100 A/m2 for about 30 minutes.
Once you have made your electrode, you should manipulate carefully because it is a bit brittle.
Lead dioxide forms on pure lead in dilute sulfuric acid. It use the same electrolysis procedure as to make ammonium perchlorate, however parameters change.
To make it, plug a lead electrode (a tube or a plate can do the job) to the + of the generator at about +1.5 V. Use any of those materials as cathode (- of the generator): copper, stainless steel or any other materials able to conduct electricity.
The electrodes are immersed in dilute (30%) and flowing sulfuric acid. To make it flow, you can use a fitted with a little blade like a mixer. The speed should be like a little swirl touching the electrodes. This avoid pitting the electrodes.
The electro deposition is carried out with a constant current at about 100 A/m2 for about 30 minutes.
Once you have made your electrode, you should manipulate carefully because it is a bit brittle.
Monday, July 23, 2012
Preparing the electrolyte for the process
Preparing fresh electrolyte
First, prepare a saturated solution of sodium chloride. Take about 40 grams for every 100 ml of solution and bring the solution to a boil. Then allow to cool to room temperature again. Some sodium chloride will crystallize as the solution cools. The solution is then filtered to obtain a clear saturated solution.
Optionally, 2 to 4 g/l of potassium dichromate, potassium chromate, sodium chromate or sodium dichromate may be added to improve efficiency. These compounds are suspected carcinogens, so if you choose to add any, know the hazards involved and act accordingly. If lead dioxide anodes are used, do not add potassium dichromate as it will only reduce efficiency. Instead, 2 to 4 g/l of sodium or potassium fluoride may be used. Although not carcinogenic, the fluorides are nasty compounds as well and should be handled properly.
Finally, the pH of the solution can be adjusted. A pH of around 6 is optimal, but anything between 5.5 and 6.5 is reasonable. The pH can be increased by addition of sodium hydroxide solution and it can be decreased by adding hydrochloric acid. Do not use too concentrated solutions for adjusting the pH. A concentration of 2% (w/v) for both solutions is convenient to work with.
Recycling old electrolyte
When electrolyte from a previous batch of perchlorate is available the following steps can be used to recycle the electrolyte.
If the electrolyte is not clear but has solid particles in it, filter to remove these and dissolve any impure chlorate from the purification and extraction steps.
After, re-saturate the solution with sodium chloride. The procedure mentioned above in step 1 of 'preparing a fresh electrolyte' may be used.
The chromate, dichromate or fluoride if added is still present so does not need to be replenished. The pH should be readjusted, like in step 3 for preparing a fresh solution above.
Or you can prepare a saturated solution of sodium chlorate if you have access to it. Take about 60 grams of sodium chlorate for every 100 ml of solution and bring the solution to a boil. Then allow to cool to room temperature again. Sodium chlorate will crystallize as the solution cools. The solution is then filtered to obtain a clear saturated solution.
First, prepare a saturated solution of sodium chloride. Take about 40 grams for every 100 ml of solution and bring the solution to a boil. Then allow to cool to room temperature again. Some sodium chloride will crystallize as the solution cools. The solution is then filtered to obtain a clear saturated solution.
Optionally, 2 to 4 g/l of potassium dichromate, potassium chromate, sodium chromate or sodium dichromate may be added to improve efficiency. These compounds are suspected carcinogens, so if you choose to add any, know the hazards involved and act accordingly. If lead dioxide anodes are used, do not add potassium dichromate as it will only reduce efficiency. Instead, 2 to 4 g/l of sodium or potassium fluoride may be used. Although not carcinogenic, the fluorides are nasty compounds as well and should be handled properly.
Finally, the pH of the solution can be adjusted. A pH of around 6 is optimal, but anything between 5.5 and 6.5 is reasonable. The pH can be increased by addition of sodium hydroxide solution and it can be decreased by adding hydrochloric acid. Do not use too concentrated solutions for adjusting the pH. A concentration of 2% (w/v) for both solutions is convenient to work with.
Recycling old electrolyte
When electrolyte from a previous batch of perchlorate is available the following steps can be used to recycle the electrolyte.
If the electrolyte is not clear but has solid particles in it, filter to remove these and dissolve any impure chlorate from the purification and extraction steps.
After, re-saturate the solution with sodium chloride. The procedure mentioned above in step 1 of 'preparing a fresh electrolyte' may be used.
The chromate, dichromate or fluoride if added is still present so does not need to be replenished. The pH should be readjusted, like in step 3 for preparing a fresh solution above.
Or you can prepare a saturated solution of sodium chlorate if you have access to it. Take about 60 grams of sodium chlorate for every 100 ml of solution and bring the solution to a boil. Then allow to cool to room temperature again. Sodium chlorate will crystallize as the solution cools. The solution is then filtered to obtain a clear saturated solution.
Friday, July 20, 2012
The electrode for making perchlorate
The range of suitable electrode materials is very limited. Especially the anode material is critical. The positive charge on the anode promotes oxidation and the evolving oxygen attacks many anode materials. Several anode materials have been considered over the years. Today's main options are listed below along with a short description.
Anode materials (plugged on the +)
Platinum: The obvious disadvantage of platinum is its high price. However, platinum anodes corrode only at a very slow rate and are suitable for perchlorate production. They therefore provide an almost ideal anode material. High efficiency can be reached with platinum and processing of the electrolyte is greatly simplified.
Lead dioxide: Lead dioxide provides an economical alternative to platinum. Lead dioxide anodes can be made at home. This takes some work and effort, but the anodes are cheap, fairly resistant to corrosion even at higher temperatures and are suitable for perchlorate production.
Cathode materials (plugged on the -)
Both stainless and mild steel find widespread use as cathode materials. Brass and copper may also be used. Each of these metals is protected to a certain extent by the negative charge present on the cathode as long as they are submerged and the current per surface area is high enough. Unsubmerged parts of the cathode corrode at a high rate however due to the action of evolving gasses and droplets of cell electrolyte
Anode materials (plugged on the +)
Platinum: The obvious disadvantage of platinum is its high price. However, platinum anodes corrode only at a very slow rate and are suitable for perchlorate production. They therefore provide an almost ideal anode material. High efficiency can be reached with platinum and processing of the electrolyte is greatly simplified.
Lead dioxide: Lead dioxide provides an economical alternative to platinum. Lead dioxide anodes can be made at home. This takes some work and effort, but the anodes are cheap, fairly resistant to corrosion even at higher temperatures and are suitable for perchlorate production.
Cathode materials (plugged on the -)
Both stainless and mild steel find widespread use as cathode materials. Brass and copper may also be used. Each of these metals is protected to a certain extent by the negative charge present on the cathode as long as they are submerged and the current per surface area is high enough. Unsubmerged parts of the cathode corrode at a high rate however due to the action of evolving gasses and droplets of cell electrolyte
Tuesday, July 17, 2012
How to make ammonium perchlorate : electrolysis
As I told you earlier, ammonium perchlorate (AP) is not available in all countries.
Here is a way to make it.
First, AP is made by electrolysis of a solution of sodium chloride (table salt or NaCl).
Electrolysis is made by plunging 2 electrodes (an anode and a cathode) in an electrically conductive solution called electrolyte and plugging these electrodes to a power supply.
The electrolysis of NaCl results in the production of chlorine (Cl) and soda (NaOH). After a number of complex chemical and electrochemical reactions occurs as the chlorine dissolve in the solution.
This will yield sodium chlorate (NaClO3) if you have choose to use sodium chloride in your electrolyte, you can use potassium chloride (KCl) and you will have potassium chlorate (KClO3).
But KClO3 solubility is very low compared to NaClO3 so that it will precipitate out of the solution.
Not good for making perchlorate as the chlorate needs to be in solution in order to be electrolyzed in perchlorate.
NEVER USE AMMONIUM CHLORIDE (NH4Cl) in the electrolyte because the resulting salt ammonium chlorate is very instable though very dangerous.
Now that the sodium chlorate is made, let run the electrolysis. The chlorate will be electrolyzed to the corresponding perchlorate.
Once the electrolysis done, there is sodium perchlorate in the electrolyte. To obtain ammonium or potassium perchlorate, we will use what is called a double decomposition.
Introduce, either ammonium or potassium chloride in the solution and the corresponding salt will precipitate out as their solubility is very low compared to sodium perchlorate. To finish, extract the perchlorate and let it dry in the sun.
This post was the process of making the perchlorate, further post will cover the details like the electrode's materials (very important) and recycling the solution.
Here is a way to make it.
First, AP is made by electrolysis of a solution of sodium chloride (table salt or NaCl).
Electrolysis is made by plunging 2 electrodes (an anode and a cathode) in an electrically conductive solution called electrolyte and plugging these electrodes to a power supply.
The electrolysis of NaCl results in the production of chlorine (Cl) and soda (NaOH). After a number of complex chemical and electrochemical reactions occurs as the chlorine dissolve in the solution.
This will yield sodium chlorate (NaClO3) if you have choose to use sodium chloride in your electrolyte, you can use potassium chloride (KCl) and you will have potassium chlorate (KClO3).
But KClO3 solubility is very low compared to NaClO3 so that it will precipitate out of the solution.
Not good for making perchlorate as the chlorate needs to be in solution in order to be electrolyzed in perchlorate.
NEVER USE AMMONIUM CHLORIDE (NH4Cl) in the electrolyte because the resulting salt ammonium chlorate is very instable though very dangerous.
Now that the sodium chlorate is made, let run the electrolysis. The chlorate will be electrolyzed to the corresponding perchlorate.
Once the electrolysis done, there is sodium perchlorate in the electrolyte. To obtain ammonium or potassium perchlorate, we will use what is called a double decomposition.
Introduce, either ammonium or potassium chloride in the solution and the corresponding salt will precipitate out as their solubility is very low compared to sodium perchlorate. To finish, extract the perchlorate and let it dry in the sun.
This post was the process of making the perchlorate, further post will cover the details like the electrode's materials (very important) and recycling the solution.
Friday, July 13, 2012
How to make nitrocellulose
Nitrocellulose, also known as gun-cotton, is like black powder but more powerful and smokeless.
It is a bit more delicate to make than the other propellant I wrote about but can still be made at home.
You will need concentrated sulfuric acid (preferably 95%), nitric acid (70%), cotton and sodium hydrogenocarbonate (baking soda).
Here is how to proceed :
Chill the acids below 0°C.
In a fume hood, mix equal parts nitric and sulfuric acid in a beaker.
Drop cotton balls into the acid. You can tamp them down using a glass stirring rod. Don't use metal.
Allow the nitration reaction to proceed for about 15 minutes (Schönbein's time was 2 minutes), then run cold tap water into the beaker to dilute the acid. Allow the water to run for a while.
Turn off the water and add a bit of sodium bicarbonate (baking soda) to the beaker. The sodium bicarbonate will bubble as it neutralizes the acid.
Using a glass rod or gloved finger, swirl around the cotton and add more sodium bicarbonate. You can rinse with more water. Continue adding sodium bicarbonate and washing the nitrated cotton until bubbling is no longer observed. Careful removal of the acid will greatly enhance the stability of the nitrocellulose.
Rinse the nitrated cellulose with tap water and allow it to dry in a cool location.
You can dissolve it in acetone to make nitrocellulose lacquer, extrude it (the shape of your engine for example) and let the acetone evaporate (preferably outside) and you will have nitrocellulose in the required shape.
But beware nitrocellulose is easily ignited, it will burst into flame if exposed to the heat of a burner or a match.
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