Method of preparing monoazo dye having stable crystal form
A technology of monoazo dyes and crystal forms, which is applied in the direction of azo dyes, organic dyes, chemical instruments and methods, etc. It can solve the problems of poor thermal stability of dyes at high temperature, instability, long sanding time, etc., and achieve good high temperature Thermal stability and dispersibility, effect of crystal form stabilization
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Embodiment 1
[0025] In a four-neck flask equipped with a stirrer and reflux condensation, add 60g of 2-amino-4-acetamidoanisole, 60g of sodium carbonate and 200g of methyl chloroacetate, and heat to 115°C for 6h under stirring; Cool to 30°C, add 300g of water and stir for 0.5h, then stand to separate layers; take the organic phase of the lower layer and distill to remove excess methyl chloroacetate, then add 200g of glacial acetic acid to the residue to obtain about 300g of coupling liquid with structural formula [II].
[0026]
[0027] Add 26.2g of 2,4-dinitro-6-bromoaniline and 38g of 98% sulfuric acid in a three-necked flask with a stirrer, stir and dissolve, then add 35g of nitrosyl sulfuric acid to react to obtain a diazonium salt solution ; The diazonium salt is gradually dropped into the coupling solution 100g containing the structural formula [II] and the mixture of ice and water and the coupling reaction obtains when X 1 = Br, X 2 = NO 2 、X 3 =OCH 3 、X 4 =COCH 3 , R 1 = ...
Embodiment 2
[0031] First, according to Example 1, except that 2-amino-4-acetamidoanisole is replaced by 60 g of m-acetamidoaniline, about 310 g of coupling solution of structural formula [IV] can be obtained.
[0032]
[0033] Then get 20.7g of 2,6-dichloro-4 nitroaniline diazotization according to the commonly known technology, then join the coupling solution containing structural formula [IV] 90g and the mixture of ice and water for proper coupling reaction. 1 =X 2 = Cl, X 3 = H, X 4 =COCH 3 , R 1 = R 2 =CH 3 , R 3 =H is an α-crystal dye with the structural formula [V]; add the α-crystal dye to 200 g of ethylene glycol, heat to 100° C. and keep it for 2.5 hours to obtain a β-crystal dye.
[0034] Take the α crystal form and β crystal form dyes in this example to test the melting point and X-ray diffraction respectively. The results are shown in Attached Table 1 and Attached Table 1. image 3 And attached Figure 4 .
[0035]
Embodiment 3
[0037] Get the o-cyano-p-nitroaniline of 16.3g, join after the diazotization according to common well-known technology and be the coupling liquid 90g that contains structural formula [IV] and the mixture of ice and water and obtain when X 1 = CN, X 2 =X 3 = H, X 4 =COCH 3 , R 1 = R 2 =CH 3 , R 3 When =H, the structural formula is the α-crystal dye of [VI]; this α-crystal dye is mixed with a solution containing 40g of 85A dispersant from U.S. WESTVACO Company; the temperature is raised to 95° C. and kept for 6 hours, and the crystal transformation is completed, and the process is continued at 80- Grind at 85°C until the dispersibility is qualified to obtain β crystal dye.
[0038]
[0039] Take the α crystal form and β crystal form dyes in this example to test the melting point and X-ray diffraction respectively. The results are shown in Attached Table 1 and Attached Table 1. Figure 5 , attached Figure 6 .
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