Method for preparing 1,1,3-trichloroacetone
A technology of dichloroacetone and acetone, which is applied in the field of preparation of 1,1,3-trichloroacetone, can solve the problems of low yield and long reaction cycle, and achieve the effect of high yield
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[0031] The method for preparing 1,1,3-trichloroacetone provided by the invention has the following specific advantages:
[0032] 1. Compared with the existing catalytic chlorination process using chlorine gas as the chlorination reagent, the present invention uses trichloroisocyanuric acid with lower activity as the reaction raw material, which has high available chlorine content, stable chemical properties, and is easy to transport, store and feed , there is no need to make special design for the operation workshop to use chlorine gas;
[0033] 2. The trichloroisocyanuric acid of the present invention can react rapidly at a relatively high temperature and simultaneously increase the yield of 1,1,3-trichloroacetone.
[0034] The present invention will be described in detail below by way of examples.
[0035] In the following examples, unless otherwise specified, all raw materials used were commercially available.
[0036] The following gas chromatographic analysis conditions...
Embodiment 1
[0042] Add 500 g of dichloroacetone mixture (made by reacting acetone (4.0 mol) and chlorine gas (8.0 mol) at 10° C. for 2 h in a 2500 mL three-necked flask, wherein the GC content of 1,1-dichloroacetone is 70.8% by weight, 1, 3-Dichloroacetone (GC content: 12.3% by weight), 25g of methanesulfonic acid, heating and controlling the internal temperature of the reaction solution to be 115-120°C, adding 100g of trichloroisocyanuric acid to the flask within 10min, and keeping the temperature for 30min after the addition; Then add 50g of trichloroisocyanuric acid to the flask, keep stirring for 30min after adding within 5min; then add 25g of trichloroisocyanuric acid into the flask, keep stirring for 30min after adding within 5min; then add 12.5 g trichloroisocyanuric acid, keep stirring for 30 minutes after adding within 5 minutes, stop the reaction. The 1,1,3-trichloroacetone GC content was 55% by weight. Remove the heat from the reaction, cool down to 45°C naturally, filter with...
Embodiment 2
[0045] Add 500 g of dichloroacetone mixture (made by reacting acetone (4.0 mol) and chlorine gas (7.0 mol) at 5° C. for 2.5 h into a 2500 mL three-necked flask, wherein the GC content of 1,1-dichloroacetone is 67.2% by weight, 1 , 3-dichloroacetone GC content 11.2% by weight), 25g of p-toluenesulfonic acid, heating and controlling the internal temperature of the reaction solution to be 125~130°C, adding 46.8g of trichloroisocyanuric acid to the flask within 30min, after adding Insulate for 10 minutes; then add 46.8g trichloroisocyanuric acid to the flask, keep stirring for 5 minutes after adding within 30 minutes; then add 46.8g trichloroisocyanuric acid to the flask, keep stirring for 5 minutes after adding within 30 minutes; then Add 46.8g of trichloroisocyanuric acid to the flask, and keep stirring for 5 minutes after adding within 30 minutes to stop the reaction. The 1,1,3-trichloroacetone GC content was 54% by weight. Remove the heat from the reaction, cool down naturall...
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