This document will describe some detailed processes and methods to obtain chlorine gas and bromine, perchloric acid, potassium chlorate and some perchlorates from different chemicals and sources.

1. Introduction

2. Chlorine Synthesis

3. Bromine Synthesis

4. Potassium Chlorate Synthesis

5. Perchloric Acid Synthesis

6. Potassium Perchlorate and Ammonium Perchlorate Synthesis

7. Oxygen Synthesis

1. Introduction

In this document described methods to obtain upper mentioned chemicals which have some interest for common chemistry and some syntheses to obtain energetic materials. Perchloric acid, chlorates and perchlorates are good oxidizing agents for some reactions and some easy methods will be described in this document to obtain some chlorates from perchloric acid. The synthesis of bromine and chlorine gas will be easy in small quantities for a home lab and some chemicals like chlorine or bromine can be obtained per electrolysis. The last chapter will give a description to produce pure oxygen in small qantities.

2. Chlorine Synthesis

The lower picture will show a simple way for the chlorine production from HCl and KMnO4 or MnO2. When hydrochloric acid is dropped to a oxidizer this will obtain chlorine in small quantities. The best method is when potassium permanganate is used for this.

2.1 Chlorine from hydrochloric acid and potassium permanganate.
2 KMnO4 + 16 HCl -> 2 KCl + 2 MnCl2 + 5 Cl2 + 8 H2O
The lower picture will show a stoppered beaker with a glas pipe and a dropper. Put 106 g of KMnO4 in a 2000 ml beaker and the beaker is sealed with the stoppered glass pipe and a 1000 ml dropper. Set the beaker to a cold water bad, put 700 ml 25 % HCl in the dropper and slowly the HCl is dropped to the KMnO4. The addition of the HCl will regulate the quantity of the chlorine production. This is suitable to bubble chlorine through solutions in a home lab. The produced chlorine is around 1,68 mol and when a large apparatus is available the qantities of the chemicals can be calculated from that.

2.2 Chlorine from hydrochloric acid and manganese(IV)oxide.
4 HCl + MnO2 -> MnCl2 + Cl2 + 2 H2O
Put 167 g of MnO2 in a 2000 ml beaker and the beaker is sealed with the stoppered glass pipe and a 1000 ml dropper. Set the beaker to a cold water bad, put 1000 ml 25 % HCl in the dropper and slowly the HCl is dropped to the MnO2. The produced chlorine is around 1,92 mol.

2.3 Chlorine from sodium chloride, manganese(IV)oxide and     sulfuric acid
2 NaCl + MnO2 + 2 H2SO4 -> Cl2 + MnSO4 + Na2SO4 + 2 H2O
Put 210 g NaCl, 156 g of MnO2 in a 2000 ml beaker and the beaker is sealed with the stoppered glass pipe and a 1000 ml dropper. Set the beaker to a cold water bad, put 200 ml 96 % H2SO4 in the dropper and slowly the H2SO4 is dropped to the MnO2. The produced chlorine is around 1,8 mol.

2.3 Chlorine from Sodium Chloride per Electrolysis
The lower picture will show a simple way for the chlorine synthesis with a homemade apparatus to obtain chlorine with a sodium chloride cell. The apparatur is useful for a easy process in a homelab instead the chlorine cell with molten sodium chloride and a advanced equipment.

You need:
1 - 24 volts car battery
1 big glass dish with cover
acid resistant clue (two components clue)
rubber glue from kitchen or bad supplier
2 acid resistant rubber rings
1 - 24 volt/100 watts car lamp
some 20 mm2 copper flex
2 - copper or graphite electrodes from MnO2 batteries, platin     electrodes are perfectly for longer time and don`t     decompose.
2 - metal stripes with screws
2 - glass pipes
sodium chloride
distilled water
96 % sulfuric acid
1 small homemade (0,3 to 0,5 mm) glued calcium layer

The size of the apparatus is dependent on what quantity of chlorine you want produce and what prefabricated components you can bye in a market or store. You can construct the apparatus how the picture it shows and this should not be complicated.

The calcium layer:
More a problem is to prepare the layer which should be waterproof but not insulated. The layer can be glued between two glass plates from a mixture of 5% bone glue/95 % water and very fine calium powder and should have a thickness of 0,3 to 0,5 mm.

3. Bromine Synthesis

The lower picture will show some methods for the bromine production in small quantities. This is suitable for to oAbtain bromine in a home lab and the process is similar than the chlorine synthesis. The best method for that is when potassium permanganate and hydrobromic acid is used for this. A other simple method is when concentrated sulfuric acid is dropped to a mix of potassium bromide and manganese(IV)oxide or hydrobromic acid to a manganese(IV)oxide.
2 KMnO4 + 16 HBr -> 2 KBr + 2 MnBr2 + 5 Br2 + 8 H2O
4 HBr + MnO2 -> MnBr2 + Br2 + 2 H2O
2 KBr + MnO2 + 2 H2SO4 -> Br2 + MnSO4 + K2SO4 + 2 H2O

3.1 Bromine from hydrobromic acid and potassium permanganate
Put 120 g of KMnO4 in a 2000 ml beaker and the beaker is sealed with a stoppered glass pipe and a 1000 ml dropper. Set the beaker to a cold water bad, put 700 ml 47 % HBr in the dropper and slowly the HBr is dropped to the KMnO4. The addition of the HCl will regulate the quantity of the bromine production. The produced bromine is around 1,9 mol and larger quantities can be calculated by weight from this.

3.2 Bromine from hydrobromic acid and manganese(IV)oxide.
Put 188 g of MnO2 in a 2000 ml beaker and the beaker is sealed with a stoppered glass pipe and a 1000 ml dropper. Set the beaker to a cold water bad, put 1000 ml 47% HBr in the dropper and slowly the HBr is dropped to the MnO2. The produced bromine is around 2,15 mol.

3.3 Bromine from potassium bromide, manganese(IV)oxide and     sulfuric acid
Put 429 g KBr, 156g of MnO2 in a 2000 ml beaker and the beaker is sealed with a stoppered glass pipe and a 1000 ml dropper. Set the beaker to a cold water bad, put 200 ml 96 % H2SO4 in the dropper and slowly the H2SO4 is dropped to the MnO2. The produced chlorine is around 1,8 mol.

4. Potassium Chlorate Synthesis

Potassium chlorate is a good oxidizer and useful for many synteses. Some possibilites are exist to obtain potassium perchlorate and the lower picture will give some informations to the syntheses. The follow methods are a easy way to obtain potassium chlorate and a short description to this will give detailed information to the syntheses.

4.1 Potassium Chlorate from Chlorine and Potassium Hydroxide     and Potassium Chloride
A good possibility to obtain potassium chlorate is when chlorine is bubbled through a molten solution of potassium hydroxide.
KOH + Cl2 + O2 -> KClO3 + HCl
Place 200 g KOH in to a heat resistant beaker and place the beaker to a hotplate. Seal the beaker with a heat resistant stopper and a necked glass pipe and connect the beaker to a simple pump and a chlorine gas bottle. Heat the potassium hydroxide to 358 °C and bubble a regular current chlorine gas and air through the beaker until the wight of the mixture is around 626 g. Weigh the beaker bevor used and sometimes during the synthesis. Atfer the reaction is complete, remove the glas pipe and the stopper from the beaker, the remainder of water and HCl is then vaporized and the obtained mass of potassium chlorate is grindet with a motar to a fine powder. A clay vessel can be used instead the glass beaker. To use oxygen is possible, for instance when the in chapter 7 described oxygen generator is connected to the necked glass pipe with the chlorin gas flask.

4.2 Potassium Chlorate from Chlorine, Calcium Hydroxide     and Potassium Chloride
A more than wasteful method to obtain potassium chlorate is the process with calcium hydroxide and potassium chloride. The yield of the process is more than low but the method is useful for a homelab.
6 Ca(OH)2 + 6 Cl2 = Ca(ClO3)2 + 5 CaCl2 + 6 H2O (+HCl)
Ca(ClO3)2 + 2 KCl = 2 KClO3 + CaCl2
Prepare a slurry of 100 g Ca(OH)2 powder and 45 ml water in a 1000 ml beaker. Seal the beaker with a stopper and a necked glass pipe. Set the beaker to a stirrer or a hotplate, connect the glass pipe to a chlorine gas flask, heat the slurry to around 90 °C and bubble a regular current of chlorine through the slurry until the wight of the mixture is 230 g. Wehn the reaction is complete, let cool and stir 33,6 g of KCl powder to the mixture, the mixture is stirred and heated for 30 minutes to 50 °C and then chilled to 5 °C. The obtained potassium chlorate is then filtered and careful dryed on a warm place. To remove some remainders or impurities dissolve the them in a small quantity of water, filter the solution and the water is then evaporated. The obtained mass is then grindet with a motar to a fine powder. A simple possibility to obtain potassium chlorate is when it prepared from pure calcium chlorate.

4.3 Potassium Chlorate from a homemade Chlorine Source
The lower picture will give some informations for the potassium chlorate synthesis from a homemade chlorine source with the in the chemicals which was used in chapter 2. The example will give the calculated amounts per ratio to the produced chlorine.
Method 1: 106 g KMnO4 and 700 ml 25 % HCl per 124,5 g Ca(OH)2, 56 ml H2O and 41,8 g KCl or 94,2 g KOH.
Method 2: 167 g MnO2 and 1000 ml 25 % HCl per 142,3 g Ca(OH)2, 64 ml H2O and 47,8 g KCl or 108 g KOH.
Method 3: 210 g NaCl, 156 g MnO2 and 200 ml 96 % H2SO4 per 136,7 g Ca(OH)2, 62 ml H2O and 45,9 g KCl or 70 g KOH.

4.4 Potassium Chlorate per regulated Electrolysis from Chlorine

The lower picture will show the the possibility to obtain potassium chlorate or some other chlorates per electrolysis similar to the chlorine cell in chapter 2.3 and the chapter 4.3 with the chlorate synthesis. The chlorine cell is easy connected with a glass pipe to the beaker with the KOH or Ca(OH)2 mixture and the current of the chlorine is regulated with a voltage regulator module.

You need additional:
1 - 10 ampere fuse
1 - 50 ampere voltage regulator module
1 regulated resistor

5. Perchloric Acid Synthesis from H2SO4 and Potassium Perchlorate

The perchloric acid synthesis from H2SO4 and potassium perchlorate is somewhat dangerous but it is possible when a the condenser is sealed with a glass tube filled with dichloromethane to protect the synthesis against oxygen from outside of the air. To fill the tube with H2SO4 chauses to much pressure in the equipment and it is not recommend. The equipment should not explode and it is saver to use 90% H2SO4 for the synthesis to obtain perchloric acid higher 72 %.
KClO4 + H2SO4 -> HClO4 + KHSO4
Place 200 ml 90% H2SO4 to a 2000 ml glass flask in a salt ice bad and 489 g of potassium perchlorate powder is careful stirred to the H2SO4. Seal the beaker with a stopper and let stand for one hour. Set the flask in a oil bad, connect the flask to a condenser with water cooling and the condenser to a 1000 ml distillation flask which is standing in a salt ice bad. Then seal the condenser with a glass tube filled with dichloromethane and heat the oil bad careful on a hotplate to 160 °C until some perchloric acid will come over. Control the temperature of the oil bad with a thermometer and rise the temperature above 200 C until no perchloric acid can distilled. Take care to rise the he temperature to much at begin if the distillation that the equipment not explode. The obtained perchloric acid should have at least 80 %. Store the perchlorc acid in acid flask in a refrigerator and protect the flask againts light. A vacuum equipment is required to obtain anhydrous perchloric acid with a surplus of 99% H2SO4.

6. Ammonium Perchlorate and Potassium Perchlorate Synthesis

The follow desciption will give some informations to obtain potassium perchlorate and ammonium perchlorate from anhydrous potassium chloride, ammonium chloride and perchloric acid.

6. 1. Ammonium Perchlorate Synthesis from Ammonium Chloride and       Perchloric Acid
2 HClO4 + 2 NH4Cl -> 2 NH4ClO4 + H2
Prepare a solution of 100 g ammonium chloride in 270 ml distilled water in a 1000 ml beaker. To a 1000 ml beaker add 320 ml of 70 % perchloric acid (410 ml of 60 % perchloric acid), the perchloric acid is careful dropped and stirred to the ammonium chloride solution and then the beaker is sealed with a heat resistant plastic foil. Put the beaker to a hotplate or in a oven, the mix is careful heated to 90 °C and then standing for one day at 90 °C. After this the solution is then chilled to room temperature and standing in a frige for 4 hours between 0 and 5 °C. The crystals of ammonium perchlorate are filtered out and dryed on a filter paper at a warm place or careful in small quantities in a oven below 60 °C. Ammonium perchlorate is sensitive against heat, flame and spark on the open air and will ignite spontaneous when it is handled not careful. It can explode when it is heated or above 200 °C or it is burned. The dryed ammonium perchlorate is transfered to a airtight glass flask when it should be stored for some time. The moisture of the flask should be remove by heating the flask for some time bevor the ammonium perchlorate is transfered and the flask is sealed.

6.2. Potassium Perchlorate from Potssium Chloride and Perchloric Acid
2 HClO4 + 2 KCl -> 2 KClO4 + H2
The potassium perchlorate synthesis is similar to the ammonium perchlorate synthesis but the quantities of the chemicals are different.
140 g potassium chloride in 405 ml distilled water per 324 ml of 70 % perchloric acid (414 ml of 60 % perchloric acid).
The potassium perchlorate can be dryes at higher temperatures than ammonium perchlorate and is more than stable. It is useful for many syntheses and a good oxidizing agent.
The syntheses of more perchlorates from other chlorides is possible when the quantities are calculated by weight, for example barium chloride and sivler chloride. This methods to obtain some perchlorates in dilute solution gives purer results and are not to dangerous.

6.3. Potassium Perchlorate from Potssium Carbonate and Perchloric Acid
2 HClO4 + K2CO3 -> 2 KClO4 + H2O + CO2
The method to obtain potassium perchlorate from perchloric acid and potassium carbonate will give a pure product wich contains no impurities or reaminders. Place 324 ml of 70 % perchloric acid (414 ml of 60 % perchloric acid) to a 1000 ml beaker in a salt-ice bad and careful 130 g of potassium carbonate powder is stirred in. Let heat the mixture to room temperature and stirr until no fumes will bubble of. Then seal the beaker with a plastic foil, let stand for one day and then the water is careful vaporized in a oven.

7. Oxygen Synthesis

A simple method to obtain pure oxygen is when potassium chlorate is heated above 400 °C. It will decompose complete between 500 and 550 °C into potassium chloride and pure oxygen.
2 KClO3 -> heat -> 2 KCl + 3 O2
This is possible at lower temperatures when no flask is available which will be restistant against this temperatures. A porcelain or clay flask is recommend for that. The lower picture will show a method with a simple beaker to obtain oxygen at 150 to 200 °C when the potassium chlorate is mixed with magnese(IV)oxide powder in a ratio 1:1. The obtained oxygen is then slight polluted with 3 % chlorin dioxide. Prepare a mix of 187 g of MnO2 powder and 245 g of KClO3 powder in a 1000 ml beaker and the beaker is then sealed with a stoppered glass pipe. Set the beaker to a stirrer and maintain the temperature with a thermometer between 150 and 200 °C. This method is suitable for some syntheses to bubble oxygen through solutions. A other simple method to obtain oxygen is when potassium permanganate is decomposed above 240 °C in a beaker.