A method for continuously preparing azo dye in micro-reactors
A micro-reactor, azo dye technology, applied in the direction of azo dyes, monoazo dyes, chemical instruments and methods, etc., can solve the problem that the diazotization reaction temperature is difficult to control, the yield of diazonium salts is not high, and the reaction cycle To avoid decomposition and other side reactions, shorten the residence time, and shorten the reaction period
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[0030] Example 1: The specific steps for the continuous preparation of azo dye product 1# are as follows (such as figure 1 with figure 2 ):
[0031] (1) At room temperature (25°C), take 0.930g of aniline in a 100mL beaker, add 15mL DMF (N,N-dimethylformamide), 2.5mL concentrated hydrochloric acid (37%), 32.5mL deionized water, Stir evenly to obtain material liquid A;
[0032] (2) Take 0.731 g of sodium nitrite solid in a 100 mL beaker, add 15 mL of DMF (N,N-dimethylformamide), 35 mL of deionized water, and stir until the sodium nitrite solid is completely dissolved to obtain feed solution B;
[0033] (3) At room temperature (25°C), take 2.54g of coupling component 1-(4-sulfophenyl)-3-methyl-5-pyrazolone in a beaker, add 60mL water, 30mLDMF( N,N-dimethylformamide), shake it well, add sodium hydroxide solution to adjust the pH of the coupling component to 9.95-10.05, stir until the coupling component is completely dissolved, and prepare liquid C;
[0034] (4) The micro-reactor used i...
Example Embodiment
[0037] Example 2: The specific steps for the continuous preparation of azo dye product 2-12# are as follows (such as figure 1 with figure 2 ):
[0038] Use p-methoxyaniline, o-chloroaniline, p-nitroaniline, m-nitroaniline, o-nitroaniline, 1-naphthylamine, p-nitrile aniline, N,N-dimethylaniline, p-aminobenzenesulfonic acid , Anthranilic acid, 1-amino-4-naphthalenesulfonic acid instead of the diazonium component aniline in Example 1, and the coupling component 1-(4-sulfophenyl)-3-methyl-5 -Pyrazolinone is used for continuous synthesis of azo dyes, and other conditions are the same as in Example 1, to obtain azo dyes of structure 2-12# (see Table 1 for the structural formula).
Example Embodiment
[0039] Example 3: The specific steps for the continuous preparation of azo dye product 13# are as follows (such as figure 1 with figure 2 ):
[0040] (1) At room temperature (25℃), take 0.930kg of aniline into a 100L container, add 15LDMF (N,N-dimethylformamide), 2.5L concentrated hydrochloric acid (37%), 32.5L deionized water, and stir Evenly, material liquid A is prepared;
[0041] (2) Take 0.731kg of sodium nitrite solid in a 100L container, add 15LDMF (N,N-dimethylformamide), 35L of deionized water, and stir until the sodium nitrite solid is completely dissolved to obtain feed liquid B;
[0042] (3) Take 3.68kg of coupling component H acid monosodium salt at room temperature (25℃), add 60L of water, 30LDMF (N,N-dimethylformamide) and shake well, add sodium hydroxide solution Adjust the pH of the coupling component to 9.95-10.05, and stir until the coupling component is completely dissolved to obtain feed liquid C;
[0043] (4) The micro-reactor used in this example is composed ...
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