Hello guys, I'm doing production chloroacetone. However, I had only 16% yield. Do you know what I can do to improve this performance using the methodology below?
250 ml acetone are placed in a flask and cooled in a waterbath to about 5°C. 3 ml H2SO4 and 3 ml HCl (30% suffices) are added.
50 g TCCA (trichloroisocyanuric acid) are crushed and dissolved in 150 g hot acetone. After all TCCA is dissolved or at least broken down to a very fine powder the mixture is cooled to about 5°C.
Some crushed ice is prepared.
The TCCA in acetone is added in portions over two hours to the acetone/HCl/H2SO4. The mixture turns greenish after every addition - chlorine. The next addition has to wait until the greenish color has disappeared and the mixture has cooled down again. Patience! Crushed ice is added to the waterbath as needed, the temperature should always stay below 10°C. Stirring or swirling with every addition is advised.
Just waiting 15 minutes after each addition of TCCA works fine.
Let sit for 4 hours and the cyanuric acid will settle. Decant the liquid, filter and add 50 g chalk, preferable in chunks, or pieces of broken marble.
The cyanuric acid is extracted twice with 100 ml hot acetone. The filtered extracts are joined with the first decanted acetone/chloroacetone mixture with the chalk.
Let settle, decant and filter and distill using a column. To the distillation flask some 10 g marble or chalk are added.