Recently, i carried out a copolymerisation reaction about 2-acrylamido-2-methylpropane sulfonic acid (AMPS) and itaconic acid. When i dried the reaction solvent in vacuum condition at 60 ℃ after 12 h, i found that the product became hard and cross-linked. Why is it not powdery solid? What method should i use if i want to obtain the powdered solid? The above experiment is to synthesize a scale inhibitor. Thanks in advance for your help!
I would suggest trying precipitate polymer by adding solvent which is not compatible with polymer to original reaction solvent.
If you get solids this way then you can filter it and dry
Igors Sivacovs Thank for you suggest, and i read the same method like as your said. They used a mixture of methanol and acetone to precipitate the synthesised polymer, so I would like to ask you if neither the autopolymers of itaconic acid or acrylic acid are soluble in this mixture. I'm not good at judging the solubility of unknowns.
Jiaqi Chen
What is the original reaction solvent that you are using?
Igors Sivacovs The reaction is carried out in deionized water, and the final product is soluble in water
Jiaqi Chen If your polymer is so polar that it is soluble in water then in theory you should lower polarity of solvent mixture. It may be difficult in your case.
I would start with methanol and, if nothing falls out, add some drops of hexane or toluene.
Btw, what is the pH of your system?
Igors Sivacovs I want to freeze-dry to get a solid product. I tried methanol, and it does not work. I'm not sure if I'm using too little methanol, that is my first time to use the alcohol precipitation. Is it possible to separate the organic components by column chromatography to get the organic components? If it is possible I plan to freeze-dry directly after column chromatography.
To elaborate, I used itaconic acid and AMPS as raw materials for the copolymerization reaction, the reaction solution was water and the initiator was ammonium persulfate.
Jiaqi Chen I have zero experience with column chromatography, so I won't be able to comment.
But freeze-drying is definitely an option. I forgot to mention it last time.
There is also one "dumb" approach — poor the reaction solution in petri dish, plate or tray and left it dry in an ambient condition.
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