Add extra water to reaction
- Thread starter Jeroenq
- Start date
External cooling by water bath is applied to control temperature more precisely, as well the dosage of methylamine.
The thin layer is recommended dripped by drip funnel with condenser and equipmed thermometer. Reaction is exotermic so temperature should be rinsed carefully, its not the stable temperature in whole RM.
There is a option to receive "optimal" result. Methylamnie can be added all at once in good thin layer applied on the wall of the vessel and temperature controled by little slowing the grow.
There are internal condensers as well. It can be put inside the vessell in case of emergency, but its not the case probably.
If you will add all of methylamine you can start at 20 degrees and add about 500 ml within 1min. The temp should be about 30 but it can vary. After that you can wait 5min to make sureit wont actually boil in some places becasue its strong dose within that time but stating temp at 20 allows you to add it like that.
Then can be thin layer till its added till end, the water bath is kept at the same temperature as mixture at about 30c, it should slow heating a bit, after its all poured its setuped at 36c.
The thin layer is recommended dripped by drip funnel with condenser and equipmed thermometer. Reaction is exotermic so temperature should be rinsed carefully, its not the stable temperature in whole RM.
There is a option to receive "optimal" result. Methylamnie can be added all at once in good thin layer applied on the wall of the vessel and temperature controled by little slowing the grow.
There are internal condensers as well. It can be put inside the vessell in case of emergency, but its not the case probably.
If you will add all of methylamine you can start at 20 degrees and add about 500 ml within 1min. The temp should be about 30 but it can vary. After that you can wait 5min to make sureit wont actually boil in some places becasue its strong dose within that time but stating temp at 20 allows you to add it like that.
Then can be thin layer till its added till end, the water bath is kept at the same temperature as mixture at about 30c, it should slow heating a bit, after its all poured its setuped at 36c.
i do the same in hdpe plastic barrels, i`m strongly recommend not exceed +35c, the lower the temp on amination - the less byproducts you have, but as you cant slowly aad MA, only options -
1) use more dcm (i use 4.5l if lab temp more than +20c)
2) add ice in the process (same as you ask basically)
3) barrel in more big barrel with outer water cooling, i use this 127 in 227l barrel + water from dip well (sorry, i dont know english word - artesian long hole about 100m down to the ground, water always +4-+8c)
1) use more dcm (i use 4.5l if lab temp more than +20c)
2) add ice in the process (same as you ask basically)
3) barrel in more big barrel with outer water cooling, i use this 127 in 227l barrel + water from dip well (sorry, i dont know english word - artesian long hole about 100m down to the ground, water always +4-+8c)