A kind of active methylene type azo-type reactive dye and preparation method thereof
A technology of active methylene-based azo type and methylene-based azo type, applied in reactive dyes, azo dyes, organic dyes, etc., can solve the problems of low dye uptake rate and low color fastness, etc. Achieve the effects of reducing the amount of dye, increasing the depth of dyeing, and increasing the dyeing rate
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Embodiment 1-6
[0070] This embodiment provides different structural A preparation method comprising the steps of:
[0071] 1) Mix compound III and thionyl chloride at a molar ratio of 1:1, heat up to 120-130°C under stirring conditions, and react for 12-14 hours to obtain compound IV; when compound III reacts with thionyl chloride, it will Hydrogen chloride and sulfur dioxide gas are generated, and the gas is pumped into the alkali-containing tank by a vacuum pump for treatment; the compound IV obtained by the reaction is dried for subsequent reactions;
[0072] 2) Add compound IV obtained in step 1) into a reaction vessel, add an aqueous solution of sodium fluoride into the reaction vessel, heat up to 70-80°C under stirring conditions, and react for 1-6h (reaction time can be monitored by TLC) control), to obtain compound V; wherein, the addition of sodium fluoride is 1.5-3 equivalents of compound IV, which can be adjusted according to the reaction yield in actual operation;
[0073] 3) ...
Embodiment 7-13
[0080] Embodiment 7-13 provides the preparation method method of dyestuff, and synthetic route is as follows:
[0081] The synthetic route diagram of compound I is as follows:
[0082]
[0083] The synthetic route diagram of compound II is as follows:
[0084]
[0085] Wherein, the first step reaction is a diazotization reaction, and the second step reaction is a coupling reaction; in the second step reaction, only the component raw materials (compound C1, compound C2) for coupling are different.
[0086] The structure of the raw material compound involved in the embodiment 7-13 and the structure of the intermediate compound are shown in Table 2 below:
[0087] The structural formula of table 2 embodiment 7-13 part compound
[0088]
[0089]
[0090] The reaction process of above-mentioned each embodiment is as follows:
Embodiment 7
[0092] The first step, diazotization:
[0093] Take 139g dry As a raw material, add it to 1L alcohol and 1L water, add 40mL concentrated hydrochloric acid (36%), add a slightly excess sodium nitrite aqueous solution with a mass fraction of 23% at 0°C, and carry out diazotization reaction at 0-5°C , Determine the end point of the reaction with starch KI test paper.
[0094] The second step, coupling:
[0095] Take the equimolar ratio of 4-aminobenzoyl fluoride in the diazotization step Soluble in Na 2 CO 3 In the solution, keep the medium at weakly alkaline 7.5-8.5 or weakly acidic at 5.6-6.5, slowly add the diazotization solution obtained in the first step into the dissolved Na 2 CO 3 In the solution, react at 0-5°C for 40 minutes. After the reaction, salting out and filtering, drying the solid below 40°C to obtain the dye with a yield of 85%.
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