I. Ammonolysis reaction: 1-amino-4-(ethylamino)anthraquinone-2-sulfonic acid by ethylaminylation of bromine (1-amino-4-bromoanthraquinone-2-sulfonic acid)
Batch A-1: In a 500ml autoclave, 24g of bromine, 3g of soda ash, 0.15g of copper acetate monohydrate, 170g of water, 15g of 70% ethylamine solution were put into the autoclave in order, and stirred for 20 minutes at room temperature, then the temperature was slowly increased to 95-98, the internal pressure was 0.5-0.6MPa, and the heat preservation was kept for 5 hours, and then the reactants were taken out of the autoclave at lower temperature, and the solids were separated from the liquids, and the solid amine was obtained with wet weight of 14.4g, and HPLC purity was 97%, and HPLC purity was 97%. HPLC purity of 97.76%; ammonia solution mother liquor 193.2g, of which amide HPLC purity of 91.17%, separated out 90g ammonia solution mother liquor set to the next batch, 90 evaporated out of the remaining mother liquor in the ethylamine added to the 90g of new water for the next batch.
II. Cyanidation reaction and graded washing: cyanidation of 1-amino-4-(ethylamino)anthraquinone-2-sulfonic acid and graded washing of the filter cake
Batch B-1: 1000ml flask was put into 350g of new water, 10g of sodium cyanide in turn, stirred for 20min, then put into A-1 batch of solid amine compounds and the remaining A-1 batch of ammonia masterbatch, slowly warmed up to 95~98, reflux holding 7h, sampling and measuring HPLC, the peak of the raw material disappeared, and the purity of the main peak was 85.34%, pumping and filtration while it was still hot, the motherbatch was collected as 483g, and washed to 6000ml of 90 hot water, and the cake was graded washing. 6000ml 90 hot water wash to neutral, collect the washing water as the next batch of the first washing water. The product was dried to 12.73g with 78.05% yield.
