Yield: 87.3%

Reaction Conditions:

Stage #1:chlorobenzene with potassium hydrosulfide;18-crown-6 ether in dimethyl sulfoxide at 110 - 120; for 16 h;Large scale;
Stage #2:1,8-dinitroanthraquinone in dimethyl sulfoxide at 40 - 50;Large scale;Solvent;Reagent/catalyst;

Steps:

6
This embodiment provides a method for producing Solvent Yellow 163 dye, which is basically the same as that in Embodiment 1, and the difference is:The amount of potassium hydrogen sulfide added in step (a) is 750 kg;Finally, 860 kg of finished Solvent Yellow 163 is dried, pulverized and packaged;The yield was 87.3%, the content was 98.8%; (a) Add 1600 kg of dimethyl sulfoxide (manual metering) to a 3000 L enamel reactor, and put 300 kg of chlorobenzene.500 kg of potassium hydrogen sulfide, and then add 6 kg of auxiliary 18-crown-6, and put it into the lid to stir;Open the condenser inlet and outlet water and use the jacket steam to raise the temperature and heat up to 110~120 °C in 1 hour (the temperature change in this temperature range is on the product quality)Has little effect),And maintaining the reaction at this temperature for 15 hours (the reaction equation is as shown in Figure 1 above, at which time the HPLC detection reaches the end point);(b) opening the jacket cooling water to cool the product of step (a) to 40 to 50 ° C, and adding 350 kg of 1,8-dinitroanthraquinone to the reaction vessel to carry out the reaction until the end of the reaction;(c) further cooling the product of step (b) to 20 ° C for suction filtration to obtain a filter cake and a filtrate;(d) The filter cake is washed with 400 kg of dimethyl sulfoxide, and the filtrate and the bubble are collected, and the solvent is recovered by distillation (containing dimethyl sulfoxide, water);The filter cake is then washed with 80~90 °C hot water to neutrality, dried, pulverized and packaged to obtain 856 kg of solvent yellow 163 finished product;The yield is 85.9%, and the content is 99.0%;

References:

Anhui Qing Keruijie New Materials Co., Ltd.;Zhou Lixia;Yang Qingshui;Tao Yimin;Liu Yong CN108624079, 2018, A Location in patent:Paragraph 0016-0025; 0027; 0028