Method for preparing CLT acid (6-chloro-3-aminotoluene-4-sulfoacid) by utilizing o-chlorotoluene direct nitrification method
A direct technology of o-chlorotoluene, applied in the field of manufacturing 6-chloro-3-aminotoluene-4-sulfonic acid, can solve the problem of high equipment requirements
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[0010] Nitrification project: add 27.29g (0.424mol) 98% nitric acid, 6g acidic zeolite beta to the reaction bottle, stir and control the temperature at 10°C, add 49.76g (0.4728mol) 97% acetic anhydride dropwise, and continue the reaction for half a year Hours, 51.19g (0.400mol) 99% o-chlorotoluene was added dropwise within 1 hour at 20-25°C, reacted at 25°C for 30 minutes after dropping, and then heated to 40°C for 5 hours. Filtrate while hot, wash the filter cake with acetic acid for 2-3 times until the filtrate is basically colorless, combine the filtrate and lotion and distill under reduced pressure of 0.05MPa until the top of the fractionation column drops from about 110°C to below 90°C and stop, and the distillation of acetic acid is complete , Obtain 68g (0.396mol) of nitration liquid, and the nitration yield is 99%.
[0011] Reduction and separation project: Add 78.84g of cast iron powder and 200ml of water into the reaction bottle, put 19g of 36% concentrated hydrochlo...
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