Industrial production method of alkylbenzene sulfonyl chloride
A technique for the production of alkylbenzenesulfonyl chloride and its production method, which is applied in the fields of sulfonic acid preparation and organic chemistry, and can solve problems such as difficult separation of materials and waste acid, poor safety of production equipment, lack of competitiveness in production, etc., and achieve good intrinsic safety , production cost reduction, and the effect of reducing the amount of hazardous chemicals
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[0024] Example 1
[0025] The benzene (liquid paraffin) solution with a flow rate of 39kg / h and a concentration of 20% is cooled by a metering pump and the pre-cooled liquid sulfur trioxide (liquid paraffin) solution with a flow rate of 16kg / h and a concentration of 50% is injected simultaneously with stirring. In the continuous sulfonation pipeline reactor with a 500ml four-necked flask with a thermometer, a thermometer and a feeding port, the reaction is controlled at a temperature of 50-60°C. The reacted liquid and chlorosulfonic acid with a flow rate of 11.6kg / h enter the continuous chlorination pipeline reactor, and the reaction temperature is controlled at 60-70°C. After the reaction, it enters the continuous desolvation system, and after the solvent is removed, it enters the crystallization system for separation. The benzenesulfonyl chloride product was 16.4kg / h, the product purity was 97%, and the yield was 90.1%.
Example Embodiment
[0026] Example 2
[0027] Add 920kg of toluene and 500kg of chloroform into a 3000L reactor equipped with a stirrer, thermometer and feeding port, start stirring, and add 1600kg of liquid sulfur trioxide / chloroform solution dropwise at a temperature of 60~70°C (where the concentration of sulfur trioxide is 50%) ), keep it for 1 hour after dropping, then add 1160kg of chlorosulfonic acid at 60~70℃, and keep it at 70~80℃ for 1 hour after dropping. Cooled to 20°C, washed with a small amount of water, separated into layers, and dissolved in the solvent layer to obtain 1860 kg of methylbenzenesulfonyl chloride product with a purity of 95% and a yield of 92.8%.
Example Embodiment
[0028] Example 3
[0029] Add 10 grams of liquid paraffin to a 500ml four-necked flask with a stirrer, thermometer and feeding port, start stirring, and then add 0.1 mol of benzene and 0.05 mol of liquid sulfur trioxide (containing 10 grams of liquid paraffin) at the same time. The reaction temperature is -20~0℃, after dripping, the temperature is kept for 2 hours, then 0.35 mol chlorosulfonic acid is added at -20℃, and the temperature is raised to 60~70℃ for 2 hours after dripping. Cooled to 20°C, washed with a small amount of water, separated into layers, and dissolved in the solvent layer to obtain 16.4 g of benzenesulfonyl chloride product with a purity of 97% and a yield of 90.1%.
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