Disperse Blue 14 synthesis
- Product Name:Disperse Blue 14
- CAS Number:2475-44-7
- Molecular formula:C16H14N2O2
- Molecular Weight:266.29
Yield:2475-44-7 95.1%
Reaction Conditions:
with 1-methyl-1H-imidazole;tetrafluoroboric acid;bromobutyric acid in methanol at 50 - 55;Large scale;Temperature;
Steps:
1-5 Example 1:
This embodiment provides a method for producing low-pollution diarylamino anthraquinone solvent blue 78 dye. The reaction mechanism is shown in Figure 1, and the process flow is shown in Figure 2, which includes the following steps:(a) Add 800 kg of methanol and 800 kg of N-methylimidazole to the reaction vessel, then slowly add 1200 kg of 4-bromobutyric acid dropwise under stirring and cooling, and slowly dropwise add 50% sodium hydroxide solution under stirring and cooling at 50°C To pH>9, add 50 kg of fluoroboric acid, stir for 5 hours to dissolve and then remove methanol under reduced pressure to obtain the first mixture;(b) Raising the temperature of the above-mentioned first mixture to 50°C,Put in 1,4-dihydroxyanthraquinone 1,200 kg,1,4-Dihydroxyanthraquinone leuco body 300 kg, monomethylamine 580 kg,Stir evenly and then continue to heat up to 55°C and react to the end point; use HPLC to determine the end point of the reaction; then lower the temperature to 35°C and open the bottom valve to discharge the material into the filter tank, drain the mother liquor to obtain a filter cake and filtrate;(c) Wash the filter cake with 500 kg of hot water, collect the washing liquid and the filtrate, and distill to recover the solvent; then wash the filter cake with hot water at 90-100°C until it is neutral, then dry, crush, and package 1582 kg of the finished product of Solvent Blue 78 was obtained; the yield was 95.1%. △C 2.714 is slightly brighter, and the pressure is 0.23.
References:
CN112661658, 2021, A Location in patent:Paragraph 0024-0040
17648-03-2
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$21.00/5g
2475-44-7
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$9.00/1g
