2,4-Dichlorobenzoyl peroxide synthesis

Yield:133-14-2 85.83%

Reaction Conditions:

with sodium peroxide;sodium dodecyl-sulfate in chloroform at 5 - 10; for 4 h;

Steps:

1.3-1.9; 2.3-2.9; 3.3-3.9

3) Add 0.85g of sodium lauryl sulfate to the intermediate liquid A prepared in step 2), and obtain intermediate liquid B after mixing evenly. 4) Fully dissolve 211.58 g of 2,4-dichlorobenzoyl chloride with a mass fraction of 99% into 846.30 g of chloroform, and mix them evenly to obtain a uniform and stable 20% mass fraction of 2,4-dichlorobenzoyl chloride in chloroform solution was obtained; 5) Under the conditions of cooling and increasing the stirring speed, to the intermediate liquid B obtained in step 3), dropwise the mixture of 2,4-dichlorobenzoyl chloride and organic solvent obtained in step 4). Mixing solution, obtain intermediate liquid C after completion;The dropwise addition was completed within 2h, the reaction temperature was 5°C to 10°C, and the reaction time was 2h; 6) Add 150g of water to the intermediate liquid C prepared in step 5), then stir for 10min successively, carry out liquid separation with a separatory funnel, and the upper layer obtained after the separation is completed is an aqueous solution and the lower layer is an organic liquid; 7) adding the organic liquid obtained in step 6) into the second reaction kettle at low temperature and containing 500 g of methanol, and using an ice machine to carry out quenching operation to the liquid in the second reaction kettle and continue stirring at low temperature, obtain intermediate after completion. liquid D; In step 7), the liquid in the second reaction kettle is carried out quenching operation until the temperature of the liquid in the second reaction kettle is reduced to -15°C ;At -15°C, stirring was continued for 25min; 8) filter the intermediate liquid D prepared in step 7), obtain filter residue and filtrate after filtering;9) drying the filter residue obtained in step 8) at low temperature, and obtaining powdered bis(2,4-dichlorobenzoyl) after drying;In step 9), the temperature of low-temperature drying is 50°C.After detection and measurement, the amount of bis(2,4-dichlorobenzoyl) peroxide prepared in Example 1 was 163.08 g, the yield was 85.83%, the appearance was white powder, the purity was 99.78wt%, and the particle size was less than or equal to 100 μm .

References:

CN113735754,2021,A Location in patent:Paragraph 0067-0068; 0074-0087; 0093-0106; 0112-0123