- Joined
- Feb 3, 2023
- Messages
- 10
- Reaction score
- 5
- Points
- 3
Yesterday I have tried the method with the microwave and in fact the result is interesting.
In baker mixed 20g 5449-12-7 and 20mL of 85% orto-phosphoric acid.
I put in microwave oven (700W), and set the lowest power. 5 -7 seconds of heating and 10-15 seconds brake for mixing and cooling the mixture because the temperature was too high. In sum 1 minute of active heating.
After heating added 50mL of distilled water.
Than extracted with dietyl ether (3x20mL) and washed with brine (3x100mL).
Dried with magnesium sulphate and evaporated ether:
Obtained very good looking product but only 7g from 20g of powder.
I was try again and heat in microwave longer - 2 minutes but there was no difference - the same yield (I was afraid of overheating because too much heat in microwave result creating solid, transparent glass-like surface which is unable to remove from baker).
Is there any method to improve the yield in microwave? Because now it is still between 30-40%?
In baker mixed 20g 5449-12-7 and 20mL of 85% orto-phosphoric acid.
I put in microwave oven (700W), and set the lowest power. 5 -7 seconds of heating and 10-15 seconds brake for mixing and cooling the mixture because the temperature was too high. In sum 1 minute of active heating.
After heating added 50mL of distilled water.
Than extracted with dietyl ether (3x20mL) and washed with brine (3x100mL).
Dried with magnesium sulphate and evaporated ether:
Obtained very good looking product but only 7g from 20g of powder.
I was try again and heat in microwave longer - 2 minutes but there was no difference - the same yield (I was afraid of overheating because too much heat in microwave result creating solid, transparent glass-like surface which is unable to remove from baker).
Is there any method to improve the yield in microwave? Because now it is still between 30-40%?
- Joined
- Dec 23, 2022
- Messages
- 325
- Solutions
- 1
- Reaction score
- 149
- Points
- 43
Yesterday I have tried the method with the microwave and in fact the result is interesting.
In baker mixed 20g 5449-12-7 and 20mL of 85% orto-phosphoric acid.
I put in microwave oven (700W), and set the lowest power. 5 -7 seconds of heating and 10-15 seconds brake for mixing and cooling the mixture because the temperature was too high. In sum 1 minute of active heating.
After heating added 50mL of distilled water.
Than extracted with dietyl ether (3x20mL) and washed with brine (3x100mL).
Dried with magnesium sulphate and evaporated ether:
View attachment 11610
Obtained very good looking product but only 7g from 20g of powder.
I was try again and heat in microwave longer - 2 minutes but there was no difference - the same yield (I was afraid of overheating because too much heat in microwave result creating solid, transparent glass-like surface which is unable to remove from baker).
Is there any method to improve the yield in microwave? Because now it is still between 30-40%?
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41Dxflatlineare you confusing glycidate oil with p2p oil? =)
w2x3f5I don't know. There's only ever been 2 layers, a cloudy white bottom layer and a light yellow layer on top. There has never been any brown anything like in other photos. It's possible the p2p isn't p2p since I'm not familar with p2p and I've not tested it in any way. What is glycidate oil? Glycidic acid?
41Dxflatlinepictured above is melted glycidate acid (not salt)
w2x3f5I'm pretty sure he took that photo at room temperature.
41DxflatlineTo be precise, there is a mixture of p2p and glycidic acid, for this reason it does not crystallize at room temperature
I did this yesterday, got almost exactly the same result. One thing I did observe though is when I didn't mix it straight away it seemed more p2p was forming but upon mixing it didn't return to the surface. Some sort of emulsification with the lower layer or a misobservation on my part?
- Joined
- Dec 23, 2022
- Messages
- 325
- Solutions
- 1
- Reaction score
- 149
- Points
- 43
are you confusing glycidate oil with p2p oil? =)
I don't know. There's only ever been 2 layers, a cloudy white bottom layer and a light yellow layer on top. There has never been any brown anything like in other photos. It's possible the p2p isn't p2p since I'm not familar with p2p and I've not tested it in any way. What is glycidate oil? Glycidic acid?
- Joined
- Dec 23, 2022
- Messages
- 325
- Solutions
- 1
- Reaction score
- 149
- Points
- 43
pictured above is melted glycidate acid (not salt)
I'm pretty sure he took that photo at room temperature.