A kind of synthetic method of environment-friendly type p-(β-hydroxyethyl sulfone sulfate) aniline
A technology of hydroxyethyl sulfone and synthesis method, applied in chemical instruments and methods, preparation of sulfonic acid, preparation of organic compounds, etc., can solve the problems of high cost, difficulty in meeting national standards, etc., and achieves changing sulfonation activity and reducing production. , the effect of reducing costs
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Embodiment 1
[0025] After adding 2500kg of chlorosulfonic acid into the sulfonation reaction pot, cool down to below 30 degrees, add 300kg of sulfur trioxide, stir and react for 2 hours, when the temperature is below 25 degrees, start feeding 1100kg of acetanilide, and keep the temperature below 30 degrees during the feeding process , feed intake finishes, insulation reaction 2 hours, reaction finishes, logical dry air is blown off redundant sulfur trioxide in the system, enters in the reactor containing hydrogen chloride, carries out chlorosulfonic acid synthesis, obtains reclaiming chlorosulfonic acid 280kg (for next a sulfonation reaction). Then the material for removing sulfur trioxide is heated up to about 45 degrees, and 1000 kg of thionyl chloride is added dropwise, and the temperature is kept at about 45 degrees during the dropping process. After the feeding is completed, the heat preservation reaction is carried out for 4 hours, and the content of p-chloroacetanilide is measured by...
Embodiment 2
[0027] After adding 2500kg of chlorosulfonic acid into the sulfonation reaction pot, cool down to below 30 degrees, add 500kg of oleum (the mass percentage of sulfur trioxide is 40%), stir and react for 2 hours, when the temperature is below 25 degrees, start to throw acetyl Aniline 1100kg, the feeding process keeps the temperature below 30 degrees, the feeding is completed, and the heat preservation reaction is carried out for 2 hours, then the redundant sulfur trioxide in the system is blown out by logical dry air, enters in the reactor containing hydrogen chloride, and synthesizes chlorosulfonic acid to obtain Reclaim 150kg of chlorosulfonic acid (for the next sulfonation reaction). Then the temperature of the material stripped of sulfur trioxide is raised to about 45 degrees, and 1000 kg of thionyl chloride is added dropwise, and the temperature is kept at about 45 degrees during the dropping process. The result was 220 ppm / kg. Then further add 820kg of sodium sulfite for...
Embodiment 3
[0029] After adding 2500kg chlorosulfonic acid in the sulfonation reactor, cool down to below 30 degrees, add 500kg fuming sulfuric acid (the mass percentage of sulfur trioxide is 25%) and 100kg phosphorus pentoxide, stir and react for 4 hours, reduce the temperature to Below 25 degrees, start to feed 1100kg of acetanilide, keep the temperature below 30 degrees during the feeding process, after feeding, keep warm for 2 hours, then blow dry air to blow out the excess sulfur trioxide in the system, and enter the reactor containing hydrogen chloride. Carry out chlorosulfonic acid synthesis, obtain and reclaim chlorosulfonic acid 200kg (for next sulfonation reaction). Then the temperature of the material stripped of sulfur trioxide is raised to about 45 degrees, and 1000 kg of thionyl chloride is added dropwise, and the temperature is kept at about 45 degrees during the dropping process. The result was 180 ppm / kg. Then further add 830kg of sodium sulfite for reduction, then add 6...
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