Medium-temperature type azobenzene disperse dye and preparation method and application thereof
A disperse dye and azo technology, which is applied in azo dyes, monoazo dyes, dyeing methods, etc., can solve problems such as unsatisfactory washing fastness, lack of varieties of medium-temperature disperse dyes, and unenvironmental protection of benzyl chloride. Achieve excellent sublimation fastness, bright color and good washing fastness
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Embodiment 1
[0038] Add 50 g of bottom water into a 250 mL flask, add 29.2 g (0.2 mol) of N-cyanoethylaniline, 4.0 g (0.1 mol) of MgO, and 0.6 g of sodium bromide while stirring, and beat for 15 min. After raising the temperature to 85°C, 35.3 g (0.2 mol) of 1-chloromethylnaphthalene was slowly added dropwise for about 2 to 2.5 hours. After dropping, keep at 90~95°C for 3 hours to the end to obtain coupling components, in which N-cyanoethylaniline 90%, cool down to precipitate, filter, beat with 200g of 10% hydrochloric acid for coupling.
[0039]Weigh 27.6g of p-nitroaniline and 47g of water into a 250ml flask, and beat for 1 hour. Add 55.5g of 30% hydrochloric acid and then beat for 1h. Add 200g of ice water to a 1L beaker, add the above-mentioned paranitrate beating material in a thin stream, control the temperature at about 0°C, and quickly pour the prepared sodium nitrite solution. Use starch potassium iodide test paper to ensure that the sodium nitrate is always excessive, and keep...
Embodiment 2
[0042] Add 50g of bottom water into a 250mL flask, and add 32.0g (0.2mol) of N-cyanoethyl m-toluidine, NaHCO 3 33.6g (0.4mol), sodium bromide 3.2g, beating for 15min. Raise the temperature to 70°C and slowly add 70.6 g (0.4 mol) of 1-chloromethylnaphthalene dropwise for about 3 to 3.5 hours. After dropping, keep at 70~75°C for 16h to the end to obtain the coupling component, among which, N-cyanoethyl m-toluidine 90%, drop the temperature and precipitate, filter, beat with 200g 10% hydrochloric acid for coupling .
[0043] Weigh 27.6g of p-nitroaniline and 47g of water into a 250ml flask, and beat for 1 hour. Add 55.5g of 30% hydrochloric acid and then beat for 1h. Add 200g of ice water to a 1L beaker, add the above-mentioned paranitrate beating material in a thin stream, control the temperature at about 0°C, and quickly pour the prepared sodium nitrite solution. Use starch potassium iodide test paper to ensure that the sodium nitrate is always excessive, and keep it at 5-...
Embodiment 3
[0046] Add 60g of bottom water into a 250mL flask, and add 29.2g (0.2mol) of N-cyanoethylaniline, Mg(OH) under stirring 2 11.6g (0.2mol), sodium bromide 1.5g, beating for 15min. Raise the temperature to 115°C and start to slowly add 41.9 g (0.22 mol) of 1-(2-chloroethyl)naphthalene dropwise for about 2 to 2.5 hours. After dropping, keep at 120~125°C for 8h to the end to obtain the coupling component, in which N-cyanoethylaniline90%. Cool down and precipitate, filter, beat with 250g 10% hydrochloric acid and wait for coupling.
[0047] Weigh 27.6g of p-nitroaniline and 47g of water into a 250ml flask, and beat for 1 hour. Add 55.5g of 30% hydrochloric acid and then beat for 1h. Add 200g of ice water to a 1L beaker, add the above-mentioned paranitrate beating material in a thin stream, control the temperature at about 0°C, and quickly pour the prepared sodium nitrite solution. Use starch potassium iodide test paper to ensure that the sodium nitrate is always excessive, and ...
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