WinterDust

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That's what I thought.

Could you describe that to me? That's the big question mark I still got. As my lab equipment is already ordered and I'll be ready to start soon, I would like to solve this issue before
KokosDreamsHere is a simple blueprint of my setup, recommendation is to also connect the waterbath to a separate cooling container in the fridge that holds larger amount of water 25-30L.

This system is fully automatic and you don't need to worry about overheating, and the temperature is consistent. Works perfectly, easily keeps the condenser at 10c during my whole reaction.
 

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KokosDreams

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This system is fully automatic and you don't need to worry about overheating, and the temperature is consistent. Works perfectly, easily keeps the condenser at 10c during my whole reaction.
eyelowThank you so much dude :)

The last puzzle piece is here finally, I got the aquarium pump already but only wondered about how to actually set it up perfectly.

recommendation is to also connect the waterbath to a separate cooling container in the fridge that holds larger amount of water 25-30L.

How should the waterbath be connected to a seperate cooling container and for what sake? Does there needs to be a flow/exchange of cool and not-cool water from the main waterbath to the waterbath second container placed in the fridge?
 

Mystery_chemistry

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Thank you so much dude :)

The last puzzle piece is here finally, I got the aquarium pump already but only wondered about how to actually set it up perfectly.



How should the waterbath be connected to a seperate cooling container and for what sake? Does there needs to be a flow/exchange of cool and not-cool water from the main waterbath to the waterbath second container placed in the fridge?
KokosDreamsrecommend a wine warmer. there are different capacities. select the correct size of the flask. you pour water, you add ice, e.g. 1: 1 (water: ice) during the first stage, it cools everything nicely. after adding all p2np the ice is gone. you turn on the heating. you set the heater temperature and you continue to fly from the robot
NqD1zwa64x
 

KokosDreams

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recommend a wine warmer. there are different capacities. select the correct size of the flask. you pour water, you add ice, e.g. 1: 1 (water: ice) during the first stage, it cools everything nicely. after adding all p2np the ice is gone. you turn on the heating. you set the heater temperature and you continue to fly from the robot View attachment 7726
Mystery_chemistryInteresting, would you prefer this over a laboratory heating mantle?
It's actually genius as it combines first cooling, then heating!!!

@G.Patton What's your take on this idea?
 

Mystery_chemistry

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Interesting, would you prefer this over a laboratory heating mantle?
It's actually genius as it combines first cooling, then heating!!!

@G.Patton What's your take on this idea?
KokosDreamsin my opinion, this solution is the simplest and the equipment so constructed does not attract attention when completing all the necessary things for this reaction
 

KokosDreams

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in my opinion, this solution is the simplest and the equipment so constructed does not attract attention when completing all the necessary things for this reaction
Mystery_chemistryI am amazed by your recommendation.

So your advise would be to place the 5-Neck RBF inside of the wine warmer and adjust all tools (condenser, drip funnel, loader, etc.) with clamps + a regular stand?
 

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I am amazed by your recommendation.

So your advise would be to place the 5-Neck RBF inside of the wine warmer and adjust all tools (condenser, drip funnel, loader, etc.) with clamps + a regular stand?
KokosDreamsThere are exactly such heaters that even a 20l flask can fit. In my opinion, it is better to set up, for example, two such sets and process 1 kg of p2np at a time than to do it in one stainless steel tank.
 

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There are exactly such heaters that even a 20l flask can fit. In my opinion, it is better to set up, for example, two such sets and process 1 kg of p2np at a time than to do it in one stainless steel tank.
Mystery_chemistryYou're right!

This method could replace a big fridge, pumps aswell as a heating mantle just with this one thing, which is actually nice!

Did you executed this with 20L RBFs already?
 

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You're right!

This method could replace a big fridge, pumps aswell as a heating mantle just with this one thing, which is actually nice!

Did you executed this with 20L RBFs already?
KokosDreamspersonally not, but the person whom I advised to assemble the equipment was made of such unusual things on the buttstock 10 i
 

Mystery_chemistry

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You're right!

This method could replace a big fridge, pumps aswell as a heating mantle just with this one thing, which is actually nice!

Did you executed this with 20L RBFs already?
KokosDreamspersonally not, but the person whom I advised to assemble the equipment was made of such unusual things on the buttstock 10 i
 

KokosDreams

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personally not, but the person whom I advised to assemble the equipment was made of such unusual things on the buttstock 10 i
Mystery_chemistryInteresting :) I will wait on the feedback of @G.Patton on this to see if it's a good idea to replace a heating mantle + cooling system with this
Thanks a lot dude!
 

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Interesting :) I will wait on the feedback of @G.Patton on this to see if it's a good idea to replace a heating mantle + cooling system with this
Thanks a lot dude!
KokosDreamsit is known that laboratory equipment is much better than building your own design from generally available things .. plus there is certainly one in this solution that we do not pay attention to ourselves because these things individually have nothing to do with the equipment for such works.
 

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recommend a wine warmer. there are different capacities. select the correct size of the flask. you pour water, you add ice, e.g. 1: 1 (water: ice) during the first stage, it cools everything nicely. after adding all p2np the ice is gone. you turn on the heating. you set the heater temperature and you continue to fly from the robot View attachment 7726
Mystery_chemistry
Very easy and smart idea!
This is one of the best things that i saw in this thread! Big UP!
 

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it is known that laboratory equipment is much better than building your own design from generally available things .. plus there is certainly one in this solution that we do not pay attention to ourselves because these things individually have nothing to do with the equipment for such works.
Mystery_chemistryDefinitely :) I will surely try this out and will give a feedback once I tried it, which might take a while
 

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it is known that laboratory equipment is much better than building your own design from generally available things .. plus there is certainly one in this solution that we do not pay attention to ourselves because these things individually have nothing to do with the equipment for such works.
Mystery_chemistryCheck this out (below), this is from a lab where they convert APAAN to BMK. I always wondered what the kettles are, that they use.
It's pretty obvious now, it must be wine cookers.

So those things definitely do have a use in labs already, your suggestions puts it kinda on the next level as they will be used for cooling and heating, which is amazing.
Now the challenge will be to find a suitable one for a 20L RBF.

Original post: http://bbzzzsvqcrqtki6umym6itiixfhn...aan-a-phenylacetoacetonitrile-large-scale.57/

NmECsTPOoZ
4medYRXxIg
Rbv1Rmc87w
 

Prima4mmc

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Hi. After adding NaBH4 to a 2:1 IPA:H2O mixture, I start adding P2NP in batches to keep it below 60 degrees. When I finished adding each batch of P2NP, the color discolored nicely from yellow to white.

Towards the end of adding P2NP when the temperature stops rising on its own the liquid continues to bomb, and a thick very sticky white ooze begins to form.... so this is where I see the number one problem.

Next, when I want to add CuCl2, even one drop, immediately the mixture discolors black, as if it is oxidized / burned through... what is caused by this?
 

WinterDust

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Hi. After adding NaBH4 to a 2:1 IPA:H2O mixture, I start adding P2NP in batches to keep it below 60 degrees. When I finished adding each batch of P2NP, the color discolored nicely from yellow to white.

Towards the end of adding P2NP when the temperature stops rising on its own the liquid continues to bomb, and a thick very sticky white ooze begins to form.... so this is where I see the number one problem.

Next, when I want to add CuCl2, even one drop, immediately the mixture discolors black, as if it is oxidized / burned through... what is caused by this?
Prima4mmc

So where is the "problem" presented?

Your reaction is correct.

The reaction will turn black during this process, once the CuCl2 is mixed in.

It's time to heat the reaction to 80c and keep it there for 30-40minutes.

During this reaction part, the black discoloriation will disapear and apear in 3 different stages.

Last stage when you know it's ready you will have 2 layers.

Black bottom thick layer and a bright transparent top layer, when this happens keep mixing for another 10min, then add the NaoH 25% and mix for 5 minutes slowly.

Let it cool then start crystalization process.
 

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it is known that laboratory equipment is much better than building your own design from generally available things .. plus there is certainly one in this solution that we do not pay attention to ourselves because these things individually have nothing to do with the equipment for such works.
Mystery_chemistryI just had a short conversation with G.Patton, he approved this idea.

You saved me good money, thanks a lot :) I will put up a summary once I have used all that succesfully
 

Mystery_chemistry

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Check this out (below), this is from a lab where they convert APAAN to BMK. I always wondered what the kettles are, that they use.
It's pretty obvious now, it must be wine cookers.

So those things definitely do have a use in labs already, your suggestions puts it kinda on the next level as they will be used for cooling and heating, which is amazing.
Now the challenge will be to find a suitable one for a 20L RBF.

Original post: http://bbzzzsvqcrqtki6umym6itiixfhn...aan-a-phenylacetoacetonitrile-large-scale.57/

View attachment 7729 View attachment 7730 View attachment 7731
KokosDreamsI saw such a 33l on the net. the specification shows that the 20 l flask should fit ...
 

h20

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where can I buy 1 kg

CuCl2 in europe​

 
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