CN102993773A - Method for preparing black active dye with high fixation rate - Google Patents
Method for preparing black active dye with high fixation rate Download PDFInfo
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- CN102993773A CN102993773A CN2012104203792A CN201210420379A CN102993773A CN 102993773 A CN102993773 A CN 102993773A CN 2012104203792 A CN2012104203792 A CN 2012104203792A CN 201210420379 A CN201210420379 A CN 201210420379A CN 102993773 A CN102993773 A CN 102993773A
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Abstract
The invention discloses a method for preparing a black active dye with a high fixation rate. The method comprises the steps of step I, carrying out an acid coupling reaction to obtain an acid coupling product; step II, carrying out an alkali coupling reaction to obtain an alkali coupling product, and uniformly stirring for later use; and step III, adding 100g of ice-water mixture and 30ml of technical hydrochloric acid into a beaker, adding the mixture for 30min at the temperature of 0-15 DEG C while stirring, after adding of the mixture is completely, controlling potassium iodide-starch test paper to be light blue, controlling the temperature at 5-20 DEG C, reacting for 2h, removing excessive nitrous acid by using sulfamic acid to obtain diazonium salt suspension liquid, adding the diazonium salt suspension liquid into the acid coupling product, uniformly stirring, then adding the alkali coupling product while controlling the temperature to be 15-20 DEG C, adjusting pH to be between 4.5 and 6.5, stirring for 1-3h, and directly carrying out spray-drying to obtain the black dye with the formula shown in the specification.
Description
Technical field
The present invention relates to a kind of preparation method of high colour-fast rate black and active dye.
Background technology
Black and active dye particularly C.I. reactive black 5 is that global current application is wider, the kind of output maximum, but pitch black degree is inadequate, so reach aterrimus, all adopt both at home and abroad at present take the C.I. reactive black 5 as the basis, utilize compounded technology to obtain, but the λ max of C.I. reactive black 5 is between 590-600nm, be actually a navy dyestuff, to piecing together the high black dyes of pitch black degree some a fly in the ointment always arranged.
Summary of the invention
The invention provides a kind of
The preparation method of high colour-fast rate black and active dye,Its preparation
The high colour-fast rate black and active dyeλ max is convenient to like this it and can be got the high black and active dye of pitch black degree with orange, red component blending between 605-610nm.
The present invention has adopted following technical scheme:
A kind of preparation method of high colour-fast rate black and active dye, it may further comprise the steps:Step 1, acid idol reaction: put mixture of ice and water 150ml in the beaker, take by weighing 100% para-ester 28.1 grams, join mixture of ice and water and pulled an oar 2 hours, then add successively 30% hydrochloric acid 12ml, add sodium nitrite solution 6.9 grams when being controlled at 5-10 ℃, finishing rear holding temperature 5-10 ℃ reacts, when reaction solution is little blue reaction 2 hours to starch potassium iodide paper, eliminate excessive nitrous acid with a little thionamic acid, then will roll over hundred H sour 34.1 and restrain and join in the diazo liquid, 10-15 ℃ of control temperature, stirred 4-6 hour, diazonium salt disappears for terminal point, can obtain like this acidic coupling object; Step 2, alkali idol reaction: in beaker, add water 350ml, take by weighing 100% 2,4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline 46.9 grams, with 100% 2,4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline is put into water making beating 1 hour, stirs the lower 15%Na of adding
2CO
3Solution is regulated PH between 6-7, makes it all after the dissolving, regulates PH between 7.1-7.3 with 15% soda ash liquid, then adds 100% Sodium Nitrite 6.9 grams and obtains the even thing of alkali, stirs evenly for subsequent use; Step 3, add mixture of ice and water 100 grams in the beaker, and technical hydrochloric acid 30ml, under stirring mixture is added, 30 minutes joining days, temperature finishes at 0-15 ℃, the little blueness of control starch potassium iodide paper, temperature 5-20 ℃, reacted 2 hours, eliminate excessive nitrous acid with thionamic acid, obtain diazonium salt suspension, above-mentioned diazonium salt suspension is joined in the acidic coupling object, and 15-20 ℃ of adding of the rear control temperature that stirs alkali idol thing transfers PH between 4.5-6.5, stirred 1-3 hour, directly the black dyes of following formula is done to get in spray:
The present invention
In the step 1Contain 100% Sodium Nitrite in the sodium nitrite solution.
The present invention has following beneficial effect;Reactive dyestuffs of the present invention have good dyeing behavior, level-dyeing property and lifting force, maximum absorbing wavelength is that λ max wavelength than the C.I. reactive black 5 between 605-610nm will be grown, each the component dyestuff of it and other of being more convenient for has good compatibleness and lifting force, its DYED FABRICS has more excellent pitch black degree and the level-dyeing property of dyeing, reactive dyestuffs of the present invention have increased the quantity of active group at molecular structure, and degree of fixation is higher more than 15% than C.I. reactive black 5.The present invention can utilize prior art by contraposition or a diazonium salt that position beta-hydroxyethyl sulfone sulfate ester aniline diazotization obtains, with H acid acid coupling, then with 2, the diazonium salt of 4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline carries out alkaline coupling, desalination spraying drying and getting, reaction conditions is gentle, is easy to suitability for industrialized production.
Embodiment
The invention discloses
A kind of preparation method of high colour-fast rate black and active dye, it may further comprise the steps:Step 1, acid idol reaction: put mixture of ice and water 150ml in the beaker, take by weighing 100% para-ester 28.1 grams, join mixture of ice and water and pulled an oar 2 hours, then add successively 30% hydrochloric acid 12ml, add sodium nitrite solution 6.9 grams when being controlled at 5-10 ℃, contain 100% Sodium Nitrite in the sodium nitrite solution, finish rear holding temperature 5-10 ℃ and react, when reaction solution is little blue reaction 2 hours to starch potassium iodide paper, eliminate excessive nitrous acid with a little thionamic acid, then will roll over hundred H acid, 34.1 grams and join in the diazo liquid, 10-15 ℃ of control temperature stirred 4-6 hour, diazonium salt disappears for terminal point, can obtain like this acidic coupling object; Step 2, alkali idol reaction: in beaker, add water 350ml, take by weighing 100% 2,4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline 46.9 grams, with 100% 2,4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline is put into water making beating 1 hour, stirs the lower 15%Na of adding
2CO
3Solution is regulated PH between 6-7, makes it all after the dissolving, regulates PH between 7.1-7.3 with 15% soda ash liquid, then adds 100% Sodium Nitrite 6.9 grams and obtains the even thing of alkali, stirs evenly for subsequent use; Step 3, add mixture of ice and water 100 grams in the beaker, and technical hydrochloric acid 30ml, under stirring mixture is added, 30 minutes joining days, temperature finishes at 0-15 ℃, the little blueness of control starch potassium iodide paper, temperature 5-20 ℃, reacted 2 hours, eliminate excessive nitrous acid with thionamic acid, obtain diazonium salt suspension, above-mentioned diazonium salt suspension is joined in the acidic coupling object, and 15-20 ℃ of adding of the rear control temperature that stirs alkali idol thing transfers PH between 4.5-6.5, stirred 1-3 hour, directly the black dyes of following formula is done to get in spray.
Claims (2)
1. the preparation method of a high colour-fast rate black and active dye, it may further comprise the steps:
Step 1, acid idol reaction: put mixture of ice and water 150ml in the beaker, take by weighing 100% para-ester 28.1 grams, join mixture of ice and water and pulled an oar 2 hours, then add successively 30% hydrochloric acid 12ml, add sodium nitrite solution 6.9 grams when being controlled at 5-10 ℃, finishing rear holding temperature 5-10 ℃ reacts, when reaction solution is little blue reaction 2 hours to starch potassium iodide paper, eliminate excessive nitrous acid with a little thionamic acid, then will roll over hundred H sour 34.1 and restrain and join in the diazo liquid, 10-15 ℃ of control temperature, stirred 4-6 hour, diazonium salt disappears for terminal point, can obtain like this acidic coupling object;
Step 2, alkali idol reaction: in beaker, add water 350ml, take by weighing 100% 2,4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline 46.9 grams, with 100% 2,4-two (beta-hydroxyethyl sulfonyl sulfuric ester) aniline is put into water making beating 1 hour, stirs the lower 15%Na of adding
2CO
3Solution is regulated PH between 6-7, makes it all after the dissolving, regulates PH between 7.1-7.3 with 15% soda ash liquid, then adds 100% Sodium Nitrite 6.9 grams and obtains the even thing of alkali, stirs evenly for subsequent use;
Step 3, add mixture of ice and water 100 grams in the beaker, and technical hydrochloric acid 30ml, under stirring mixture is added, 30 minutes joining days, temperature finishes at 0-15 ℃, the little blueness of control starch potassium iodide paper, temperature 5-20 ℃, reacted 2 hours, eliminate excessive nitrous acid with thionamic acid, obtain diazonium salt suspension, above-mentioned diazonium salt suspension is joined in the acidic coupling object, and 15-20 ℃ of adding of the rear control temperature that stirs alkali idol thing transfers PH between 4.5-6.5, stirred 1-3 hour, directly the black dyes of following formula is done to get in spray.
The chemical formula of black dyes.
2. the preparation method of high colour-fast rate black and active dye according to claim 1 is characterized in that containing 100% Sodium Nitrite in the step 1 Sodium Nitrite solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104203792A CN102993773A (en) | 2011-12-13 | 2012-10-29 | Method for preparing black active dye with high fixation rate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110414779.8 | 2011-12-13 | ||
| CN201110414779 | 2011-12-13 | ||
| CN2012104203792A CN102993773A (en) | 2011-12-13 | 2012-10-29 | Method for preparing black active dye with high fixation rate |
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| CN102993773A true CN102993773A (en) | 2013-03-27 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4585460A (en) * | 1982-09-30 | 1986-04-29 | Ciba-Geigy Corporation | Reactive dyes, process for their preparation and use thereof: bis-vinyl or substituted ethyl sulphenyl azo reactive dyes for textiles |
| EP0197418A2 (en) * | 1985-04-04 | 1986-10-15 | Bayer Ag | Reactive azo dyes |
| US4897469A (en) * | 1987-04-07 | 1990-01-30 | Basf Aktiengesellschaft | Aniline series azo reactive dyes ortho- or para-substituted by vinyl sulfonyl reactive groups |
| CA1276141C (en) * | 1984-11-12 | 1990-11-13 | Hartmut Springer | Fiber-reactive monoazo compounds, process for their preparation and their use as dyes |
| US4992589A (en) * | 1984-07-20 | 1991-02-12 | Hoechst Aktiengesellschaft | Substituted phenyl hydroxyethyl sulfones, and process for their preparation |
| CN101081939A (en) * | 2007-05-25 | 2007-12-05 | 褚平忠 | Black reactive dye and preparation method thereof |
-
2012
- 2012-10-29 CN CN2012104203792A patent/CN102993773A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4585460A (en) * | 1982-09-30 | 1986-04-29 | Ciba-Geigy Corporation | Reactive dyes, process for their preparation and use thereof: bis-vinyl or substituted ethyl sulphenyl azo reactive dyes for textiles |
| US4992589A (en) * | 1984-07-20 | 1991-02-12 | Hoechst Aktiengesellschaft | Substituted phenyl hydroxyethyl sulfones, and process for their preparation |
| CA1276141C (en) * | 1984-11-12 | 1990-11-13 | Hartmut Springer | Fiber-reactive monoazo compounds, process for their preparation and their use as dyes |
| EP0197418A2 (en) * | 1985-04-04 | 1986-10-15 | Bayer Ag | Reactive azo dyes |
| US4897469A (en) * | 1987-04-07 | 1990-01-30 | Basf Aktiengesellschaft | Aniline series azo reactive dyes ortho- or para-substituted by vinyl sulfonyl reactive groups |
| CN101081939A (en) * | 2007-05-25 | 2007-12-05 | 褚平忠 | Black reactive dye and preparation method thereof |
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Application publication date: 20130327 |