CN101215427A - Method of preparing navy blue active dyestuff - Google Patents
Method of preparing navy blue active dyestuff Download PDFInfo
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- CN101215427A CN101215427A CNA2008100521287A CN200810052128A CN101215427A CN 101215427 A CN101215427 A CN 101215427A CN A2008100521287 A CNA2008100521287 A CN A2008100521287A CN 200810052128 A CN200810052128 A CN 200810052128A CN 101215427 A CN101215427 A CN 101215427A
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Abstract
The invention discloses a process for preparing a dark blue reactive dye, which is prepared through the process of condensing, diazotizing, coupling acid and base, nano-filtering and merchandising. Phase transition catalyst is added in the process of reacting, which improves selectivity of the main reaction in a condensation reaction, inhibits the happening of the side effect, and leads the reaction to be close to a theoretical value. Raw material proposition is more reasonable through central control means. Products which are produced can reach to the quality requirements without needing salting out, refining and purifying. The density of products in reacting stock solution at the last procedure is improved, and primary pulp spraying technique is achieved. No process waste water is produced in the whole reacting process, and clean manufacturing technique is achieved.
Description
Technical field
The present invention relates to a kind of reactive dyestuffs preparation method, especially a kind of preparation method of dark blue reactive dye.
Background technology
Matching stain, acid mordant dye, metallized dye are generally used in the dyeing of wool textile.The acid dyeing dyefastness is general, and hair fibre is had damage, can't be used for the dyeing of worsted fabric.Though acid mordant dye, metallized dye fastness have improved, the coloured light dimness, and also dyeing the time has heavy metal Cr
6+Exist, cause dyeing waste-water to be difficult to administer.
Along with the continuous development of wool industry, people are more and more higher to the quality requirements of wool textile, and the comfortable safety of wool fabric becomes new emphasis.High-grade wool textile-cashmere requires more strict to the black dyes kind of dyeing usefulness: the degree of fixation height, colour fastness is good, level-dyeing property is strong, and dyeing is little to fibre-tendering,
The plain dark blue G of moral dragon is one of reactive dye for wool kind, meets the strict demand of wool industry.Structure is as follows:
The production technique by product is more at present, must adopt the purified method of saltouing in the production process, thereby produce a large amount of saliferous high-colour intensity wastewaters.
As shown in Figure 1, former operational process of craft is as follows:
1, condensation:
Add 2.4-diamino benzene sulfonic acid sodium in water, the dissolving back adds ice, controlled temperature 3-8 ℃.Stir adding bromo propionyl chloride down, time spent 2-3 hour, add the sodium carbonate solution that concentration is 8-15% simultaneously, control pH=5-7.After adding the bromo propionyl chloride,, under the pH=5-7 condition, reacted 1.5-2.5 hour in 3-8 ℃.
2, saltout:
In the condensated liquid of step 1, add the sodium-chlor of its cumulative volume 15-20%, saltoutd 2-3 hour, filter.Filtrate is removed wastewater disposal basin, and filter cake is prepared diazotization.
3, diazotization:
Filter cake water making beating with step 2 adds hydrochloric acid and ice, and controlled temperature adds sodium nitrite solution again at 5--8 ℃, 5-8 ℃ of diazotization, and reaction times 1.5-2.5 hour.
4, acid coupling, alkaline coupling:
In the diazonium liquid of step 3, the time spent 2-3 hour even good H acid solution (concentration is at 20--30%) of dissolving in advance that adds, reaction is 5 hours under 8-12 ℃.Transfer pH=6-8 with yellow soda ash, reacted again after finishing 1-2 hour.
5, saltout:
In the reaction solution of step 4, add the Repone K of cumulative volume 15--20%, saltoutd 2-3 hour, filter.Filtrate is removed wastewater disposal basin, and filter cake is the dyestuff work in-process.
6, drying:
The filter cake of step 5 is put into baking box, dry in 80-100 ℃, filtration cakes torrefaction.
7, commercialization:
The exsiccant filter cake is pulverized, and adding sodium sulfate is pieced together mixed, stdn.Qualified back packing obtains hair reactive navy blue G commodity.
But former technology has the following disadvantages:
In the first step condensation reaction, main reaction is:
Many side reactions take place simultaneously:
Except by product, also have unreacted 2.4-diamino benzene sulfonic acid sodium, these impurity directly influence the quality of condenses, finally influence the quality of dyestuff, so condenses must be made with extra care purification.What adopt at present is salting-out process.
Both contained condenses in the filtrate after saltouing
Also contain above-mentioned by product, and unreacted 2.4-diamino benzene sulfonic acid sodium.Except that principal product, also contain the unreacted 2.4-diamino benzene sulfonic acid of part sodium in the filter cake.
In the acid coupling reaction, former technology does not have middle control means, can't accurately judge the degree that reaction is carried out, and can only guarantee that acid coupling reacts completely by prolonging soaking time.But, directly influence next step alkaline even summation reaction because after prolonging the reaction times, diazonium salt has part and decomposes, and causes the diazonium salt ullage.For avoiding the diazonium salt ullage, have only the add-on that reduces H acid according to estimation, thereby make diazonium salt and the imbalance of H acid proportioning, cause coloured light dark partially, unstable product quality.For guaranteeing the stable of quality product, need saltout once more, remove the impurity such as diazonium salt of decomposition.Contain a large amount of inorganic salt and part organic dye in the filtrate that produces, difficulty of governance is big, expense is high.
Summary of the invention
Technical problem to be solved by this invention is, a kind of selectivity that improves main reaction in the condensation reaction is provided, and suppressed the generation of side reaction, by middle control means, make proportioning raw materials more reasonable, adopt membrane technique, realized the preparation method of the dark blue reactive dye of magma spray art.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of dark blue reactive dye may further comprise the steps:
A. mixing of phase-transfer catalyst and bromo propionyl chloride: 2, add phase-transfer catalyst in 3-two bromo propionyl chloros, mix standby;
The preparation of b.H acid solution: in water, add H acid, transfer pH=7-8 with sodium hydroxide solution, after H acid is all dissolved, standby;
C. condensation: add 2.4-diamino benzene sulfonic acid sodium in water, the dissolving back adds ice, controlled temperature 2-8 ℃, stir the bromo propionyl chloride that is mixed with phase-transfer catalyst that adds step a down, time spent 2-3 hour, add the sodium carbonate solution that concentration is 8-15% simultaneously, control pH=5-7; After adding the bromo propionyl chloride,, under the pH=5-7 condition, reacted 1.5-2.5 hour in 2-8 ℃;
D. diazotization: in the condensated liquid with step c, add hydrochloric acid and ice, controlled temperature adds sodium nitrite solution again at 5-8 ℃, 5-8 ℃ of diazotization, and reaction times 1.5-2.5 hour;
E. acid coupling, alkaline coupling: in the diazonium liquid of steps d, evenly adding step b in time spent 2-3 hour dissolves good H acid solution, adds the back sampling, the degree of carrying out with instrumental method detection of acidic coupled reaction; After acid coupling is finished, detect the residual content of diazonium salt again with instrumental method; If the not enough alkaline coupling of remaining diazonium salt uses, then need add diazonium salt; If remaining diazonium salt still has residue after satisfying alkaline even summation, then add H acid; Till remaining diazonium salt satisfies alkaline even summation reaction needed just; After whole detections were qualified, adding was immediately carried out yellow soda ash and is carried out alkaline even summation, and control pH=6-8 reacted 1-2 hour, and the reaction end obtains dark blue solution;
D. receive membrane filtration: the reaction solution of step e is carried out secondary and receives membrane filtration and concentrate with receiving membrane filter appts, be concentrated to dialyzate when identical with the concentrated solution volume till;
E. commercialization: the solution after steps d concentrated carries out stdn, adjusts coloured light to standard, adjusts intensity again and reaches standard, uses the spray-drying tower spraying drying, and dry product is directly packed, and obtains dark blue reactive dye.
Described phase-transfer catalyst is one or more the mixture in acetone, pyridine or the trolamine.
Adjust intensity with a kind of in sodium sulfate, the organic additive or the mixture of the two.
Described organic additive is a kind of in dispersing agent NNO, glucose, EDTA or the sorbic alcohol.
When the membrane filtration dialyzate of receiving for the first time carried out receiving second time membrane filtration, control concentrated the back strength of solution and reaches strength of solution when receiving membrane filtration, and dialyzate reclaims use.
The H acid concentration of preparing among the described step b is 20--30%.
The invention has the beneficial effects as follows: the invention solves the deficiency of original production process, at first, improved the selectivity of main reaction in the condensation reaction, suppressed the generation of side reaction, make reaction near theoretical value by adding phase-transfer catalyst.Secondly by unique middle control means, make proportioning raw materials more reasonable.The product of the producing refining purification of must not saltouing can reach specification of quality.By adopting membrane technique, improve the concentration of product in reaction stoste in last procedure once more, realized the magma spray art.Entire reaction course does not have processing wastewater and produces, and has realized process for cleanly preparing.
Description of drawings
Fig. 1 is preparation method's schema of prior art dark blue reactive dye.
Fig. 2 is preparation method's schema of dark blue reactive dye of the present invention.
Embodiment
The preparation method of dark blue reactive dye of the present invention may further comprise the steps:
A. mixing of phase-transfer catalyst and bromo propionyl chloride: 2, add phase-transfer catalyst in 3-two bromo propionyl chloros, mix standby;
The preparation of b.H acid solution: in water, add H acid, transfer pH=7-8 with sodium hydroxide solution, after H acid is all dissolved, standby;
C. condensation: add 2.4-diamino benzene sulfonic acid sodium in water, the dissolving back adds ice, controlled temperature 2-8 ℃, stir the bromo propionyl chloride that is mixed with phase-transfer catalyst that adds step a down, time spent 2-3 hour, add the sodium carbonate solution that concentration is 8-15% simultaneously, control pH=5-7; After adding the bromo propionyl chloride,, under the pH=5-7 condition, reacted 1.5-2.5 hour in 2-8 ℃;
D. diazotization: in the condensated liquid with step c, add hydrochloric acid and ice, controlled temperature adds sodium nitrite solution again at 5--8 ℃, 5-8 ℃ of diazotization, and reaction times 1.5-2.5 hour;
E. acid coupling, alkaline coupling: in the diazonium liquid of steps d, evenly adding step b in time spent 2-3 hour dissolves good H acid solution, adds the back sampling, the degree of carrying out with instrumental method detection of acidic coupled reaction; After acid coupling is finished, detect the residual content of diazonium salt again with instrumental method; If the not enough alkaline coupling of remaining diazonium salt uses, then need add diazonium salt; If remaining diazonium salt still has residue after satisfying alkaline even summation, then add H acid; Till remaining diazonium salt satisfies alkaline even summation reaction needed just; After whole detections were qualified, adding was immediately carried out yellow soda ash and is carried out alkaline even summation, and control pH=6-8 reacted 1-2 hour, and the reaction end obtains dark blue solution;
D. receive membrane filtration: the reaction solution of step e is carried out secondary and receives membrane filtration and concentrate with receiving membrane filter appts, be concentrated to dialyzate when identical with the concentrated solution volume till;
E. commercialization: the solution after steps d concentrated carries out stdn, adjusts coloured light to standard, adjusts intensity again and reaches standard, uses the spray-drying tower spraying drying, and dry product is directly packed, and obtains dark blue reactive dye.
Described phase-transfer catalyst is one or more the mixture in acetone, pyridine or the trolamine.
Adjust intensity with a kind of in sodium sulfate, the organic additive or the mixture of the two.
Described organic additive is a kind of in dispersing agent NNO, glucose, EDTA or the sorbic alcohol.
When the membrane filtration dialyzate of receiving for the first time carried out receiving second time membrane filtration, control concentrated the back strength of solution and reaches strength of solution when receiving membrane filtration, and dialyzate reclaims use.
The H acid concentration of preparing among the described step b is 20--30%.
Below in conjunction with Fig. 2 and specific embodiment the present invention is described in further detail:
Embodiment 1
1. mixing of transfer catalyst and bromo propionyl chloride:
At 1226kg2, add 123kg acetone in 3-two bromo propionyl chloros, standby after mixing.
2.H acid solution preparation:
In 1800L water, add H acid 748kg, transfer pH=7-8 with the 30-40% sodium hydroxide solution, after the sour all dissolvings of H, standby.
3. condensation:
Add 2.4-diamino benzene sulfonic acid sodium 1000kg in 16000L water, the dissolving back adds ice, controlled temperature 2-8 ℃.Time spent 2-3 hour, stir the mixture that adds step 1 down, with the sodium carbonate solution control pH=5-7 of 8-15%.Finish,, under the pH=5-7 condition, kept 1.5-2.5 hour, get the condenses reaction solution in 2-8 ℃.
4. diazotization:
In the condenses reaction solution with step 3, add 30% hydrochloric acid 1333kg, at 5--8 ℃, add the sodium nitrite solution that is dissolved with 329kg with the ice controlled temperature again, strength of solution is at 30-40%.At 8--13 ℃ of reaction times 1.5-2.5 hour.Add thionamic acid, remove excessive nitrite.
5. acid coupling, alkaline coupling
In the diazonium salt reaction solution of step 4, evenly added the H acid solution of step 2 in time spent 2-3 hour, with 10-15 ℃ of ice controlled temperature.Kept 1 hour.Sampling, the degree of carrying out with instrumental method detection of acidic coupled reaction.
After acid coupling is finished, detect the residual content of diazonium salt again with instrumental method.Use as crossing the alkaline inadequately even summation of remaining diazonium salt, then need add diazonium salt; If remaining diazonium salt still has residue after satisfying alkaline even summation, then add H acid.Till remaining diazonium salt satisfies alkaline even summation reaction needed just.The control of diazonium salt amount detects data according to computer fully.
After whole detections are qualified, add yellow soda ash immediately, carry out alkaline even summation.Control pH=6-8 reacted 1-2 hour.Obtain reactive navy blue G solution.
6. receive membrane filtration:
With the dye solution of step 5, concentrate with receiving membrane filter appts.Be concentrated to dialyzate when identical with the concentrated solution volume till.When the membrane filtration dialyzate of receiving for the first time carries out receiving second time membrane filtration, should control and concentrate the strength of solution that back strength of solution reaches when receiving membrane filtration and get final product.Dialyzate reclaims and uses.
7. commercialization:
Solution after step 6 concentrated carries out stdn, adjust coloured light and conform to standard substance, sampling after experiment is with the spray-drying tower drying, the detection dye strength.According to strength values, determine the glucose add-on.Adjust intensity and reach standard, use the spray-drying tower spraying drying, dry product is directly packed, and obtains dark blue reactive dyestuffs.
Embodiment 2
1. mixing of transfer catalyst and bromo propionyl chloride:
At 1226kg2, add 63kg acetone in 3-two bromo propionyl chloros, the 60kg trolamine, standby after mixing.
2.H acid solution preparation:
In 1800L water, add H acid 748kg, transfer pH=7-8 with the 30-40% sodium hydroxide solution, after the sour all dissolvings of H, standby.
3. condensation:
Add 2.4-diamino benzene sulfonic acid sodium 1000kg in 16000L water, the dissolving back adds ice, controlled temperature 2-8 ℃.Time spent 2-3 hour, stir the mixture that adds step 1 down, with the sodium carbonate solution control pH=5-7 of 8-15%.Finish,, under the pH=5-7 condition, kept 1.5-2.5 hour in 2-8 ℃.Get the condenses reaction solution.
4. diazotization:
In the condenses reaction solution with step 3, add 30% hydrochloric acid 1333kg, at 5--8 ℃, add the sodium nitrite solution that is dissolved with 329kg with the ice controlled temperature again, strength of solution is at 30-40%.At 8--13 ℃ of reaction times 1.5-2.5 hour.Add thionamic acid, remove excessive nitrite.
5. acid coupling, alkaline coupling
In the diazonium salt reaction solution of step 4, evenly added the H acid solution of step 2 in time spent 2-3 hour, with 10-15 ℃ of ice controlled temperature.Kept 1 hour.Sampling, the degree of carrying out with instrumental method detection of acidic coupled reaction.
After acid coupling is finished, detect the residual content of diazonium salt again with instrumental method.Use as crossing the alkaline inadequately even summation of remaining diazonium salt, then need add diazonium salt; If remaining diazonium salt still has residue after satisfying alkaline even summation, then add H acid.Till remaining diazonium salt satisfies alkaline even summation reaction needed just.The control of diazonium salt amount detects data according to computer fully.
After whole detections are qualified, add yellow soda ash immediately, carry out alkaline even summation.Control pH=6-8 reacted 1-2 hour.Obtain dark blue living solution.
6. receive membrane filtration:
With the dye solution of step 5, concentrate with receiving membrane filter appts.Be concentrated to dialyzate when identical with the concentrated solution volume till.When the membrane filtration dialyzate of receiving for the first time carries out receiving second time membrane filtration, should control and concentrate the strength of solution that back strength of solution reaches when receiving membrane filtration and get final product.Dialyzate reclaims and uses.
7. commercialization:
Solution after step 6 concentrated carries out stdn, adjust coloured light and conform to standard substance, sampling after experiment is with the spray-drying tower drying, the detection dye strength.According to strength values, determine the dispersing agent NNO add-on.Adjust intensity and reach standard, use the spray-drying tower spraying drying, dry product is directly packed, and obtains dark blue reactive dyestuffs commodity.
Embodiment 3
1, mixing of transfer catalyst and bromo propionyl chloride:
At 1226kg2, add 43kg acetone in 3-two bromo propionyl chloros, the 40kg pyridine, the 40kg trolamine, standby after mixing.
2, H acid solution preparation:
In 1800L water, add H acid 748kg, transfer pH=7-8 with the 30-40% sodium hydroxide solution, after the sour all dissolvings of H, standby.
3, condensation:
Add 2.4-diamino benzene sulfonic acid sodium 1000kg in 16000L water, the dissolving back adds ice, controlled temperature 2-8 ℃.Time spent 2-3 hour, stir the mixture that adds step 1 down, with the sodium carbonate solution control pH=5-7 of 8-15%.Finish,, under the pH=5-7 condition, kept 1.5-2.5 hour in 2-8 ℃.Get the condenses reaction solution.
4, diazotization:
In the condenses reaction solution with step 3, add 30% hydrochloric acid 1333kg, at 5--8 ℃, add the sodium nitrite solution that is dissolved with 329kg with the ice controlled temperature again, strength of solution is at 30-40%.At 8--13 ℃ of reaction times 1.5-2.5 hour.Add thionamic acid, remove excessive nitrite.
5, acid coupling, alkaline coupling
In the diazonium salt reaction solution of step 4, evenly added the H acid solution of step 2 in time spent 2-3 hour, with 10-15 ℃ of ice controlled temperature.Kept 1 hour.Sampling, the degree that the detection of acidic coupled reaction is carried out.
After acid coupling is finished, detect the residual content of diazonium salt again.Use as crossing the alkaline inadequately even summation of remaining diazonium salt, then need add diazonium salt; If remaining diazonium salt still has residue after satisfying alkaline even summation, then add H acid.Till remaining diazonium salt satisfies alkaline even summation reaction needed just.The control of diazonium salt amount detects data according to computer fully.
After whole detections are qualified, add yellow soda ash immediately, carry out alkaline even summation.Control pH=6-8 reacted 1-2 hour.Obtain dark blue living solution.
6, receive membrane filtration:
With the dye solution of step 5, concentrate with receiving membrane filter appts.Be concentrated to dialyzate when identical with the concentrated solution volume till.
7, commercialization:
Solution after step 6 concentrated carries out stdn, adjust coloured light and conform to standard substance, sampling after experiment is with the spray-drying tower drying, the detection dye strength.According to strength values, determine the EDTA add-on.Adjust intensity and reach standard, use the spray-drying tower spraying drying, dry product is directly packed, and obtains dark blue reactive dyestuffs commodity.
In sum, the present invention takes following novel method:
1, in condensation reaction, adds phase-transfer catalyst, the main reaction selectivity of condensation is improved, suppress side reaction.The bromo propionyl chloride is slightly soluble in water, is oily matter in water, and the two side reactions of contracting of hydrolysis easily take place absorption principal product--condenses.After adding phase-transfer catalyst, increased the solubleness of bromo propionyl chloride in water, thereby increased the probability of collision with 2.4-diamino benzene sulfonic acid sodium, main reaction is speeded up, main reaction is near theoretical value.
2, the purification step of saltouing is cancelled in control during coupled reaction increases.When acid coupling, diazonium salt is excessive, and the gold-tinted of product surpasses claimed range; The H excessive acid, the ruddiness of product surpasses claimed range.Neither qualified.Improved technology is monitored the acid coupling reaction process with detecting instrument, reaction product near theoretical value after, according to detecting data the ratio of diazonium salt and H acid is done accurately adjustment, until best proportioning.Both guaranteed the reasonableness of diazonium salt and H acid proportioning, and shortened the unnecessary time again, thereby guaranteed quality product.Need not making with extra care purification, can to reach product qualified, thereby removed the technology of saltouing.
3, adopt membrane technique, improve magma dyestuff content, realize spraying drying.Because the magma solid content low (containing the finished product dyestuff) that technology produces uses drying process with atomizing energy consumption height, the time is long, and cost is big, is unfavorable for the magma drying process with atomizing.Novel process adopts to be received membrane technique and concentrates, and improves the magma solid content and reaches 20--25%, has solved an above-mentioned difficult problem, has realized process for cleanly preparing.
4, phase-transfer catalyst: phase-transfer catalyst is that acetone, pyridine, trolamine use separately or two kinds of mixing or three kinds of mixing uses.
5, organic additive: dispersing agent NNO, glucose, EDTA, sorbic alcohol.
The present invention adopts the method that adds phase-transfer catalyst, condensation reaction is carried out fully, and significantly reduced side reaction, thereby condenses need not saltoutd refining.The control of control of the terminal point of acid coupling and diazonium salt amount has guaranteed that the coloured light of dyestuff is qualified, thereby it is refining also not need to carry out saltouing of dyestuff.Membrane technique and liquid phase are pieced together mixed The Application of Technology, make dye solution obtain enrichment, have realized the magma spraying drying.Novel process has been saved two and has been gone on foot the process for refining of saltouing, and has realized the magma spraying drying of dye solution, does not produce processing wastewater, reaches the purpose of wastewater zero discharge, has good exemplary role and promotional value.
Product utilization novel process of the present invention has realized the process for cleanly preparing of no processing wastewater, constant product quality.
In sum, among the embodiment that content of the present invention is not confined to, the knowledgeable people in the same area can propose other embodiment easily within technical director's thought of the present invention, but this embodiment comprises within the scope of the present invention.
Claims (6)
1. the preparation method of a dark blue reactive dye may further comprise the steps:
A. mixing of phase-transfer catalyst and bromo propionyl chloride: 2, add phase-transfer catalyst in 3-two bromo propionyl chloros, mix standby;
The preparation of b.H acid solution: in water, add H acid, transfer pH=7-8 with sodium hydroxide solution, after H acid is all dissolved, standby;
C. condensation: add 2.4-diamino benzene sulfonic acid sodium in water, the dissolving back adds ice, controlled temperature 2-8 ℃, stir the bromo propionyl chloride that is mixed with phase-transfer catalyst that adds step a down, time spent 2-3 hour, add the sodium carbonate solution that concentration is 8-15% simultaneously, control pH=5-7; After adding the bromo propionyl chloride,, under the pH=5-7 condition, reacted 1.5-2.5 hour in 2-8 ℃;
D. diazotization: in the condensated liquid with step c, add hydrochloric acid and ice, controlled temperature adds sodium nitrite solution again at 5--8 ℃, 5-8 ℃ of diazotization, and reaction times 1.5-2.5 hour;
E. acid coupling, alkaline coupling: in the diazonium liquid of steps d, evenly adding step b in time spent 2-3 hour dissolves good H acid solution, adds the back sampling, the degree of carrying out with instrumental method detection of acidic coupled reaction; After acid coupling is finished, detect the residual content of diazonium salt again with instrumental method; If the not enough alkaline coupling of remaining diazonium salt uses, then need add diazonium salt; If remaining diazonium salt still has residue after satisfying alkaline even summation, then add H acid; Till remaining diazonium salt satisfies alkaline even summation reaction needed just; After whole detections were qualified, adding was immediately carried out yellow soda ash and is carried out alkaline even summation, and control pH=6-8 reacted 1-2 hour, and the reaction end obtains dark blue solution;
D. receive membrane filtration: the reaction solution of step e is carried out secondary and receives membrane filtration and concentrate with receiving membrane filter appts, be concentrated to dialyzate when identical with the concentrated solution volume till;
E. commercialization: the solution after steps d concentrated carries out stdn, adjusts coloured light to standard, adjusts intensity again and reaches standard, uses the spray-drying tower spraying drying, and dry product is directly packed, and obtains dark blue reactive dye.
2. the preparation method of dark blue reactive dye according to claim 1 is characterized in that, described phase-transfer catalyst is one or more the mixture in acetone, pyridine or the trolamine.
3. the preparation method of dark blue reactive dye according to claim 1 is characterized in that, adjusts intensity with a kind of in the sodium sulfate, organic additive or the mixture of the two.
4. the preparation method of dark blue reactive dye according to claim 3 is characterized in that, described organic additive is a kind of in dispersing agent NNO, glucose, EDTA or the sorbic alcohol.
5. the preparation method of dark blue reactive dye according to claim 1, it is characterized in that, when the membrane filtration dialyzate of receiving for the first time carried out receiving second time membrane filtration, control concentrated the back strength of solution and reaches strength of solution when receiving membrane filtration, and dialyzate reclaims use.
6. the preparation method of dark blue reactive dye according to claim 1 is characterized in that, the H acid concentration of preparing among the described step b is 20--30%.
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| CN101481529A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Preparation of reactive dye for fur |
| CN101481524A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Preparation of reactive red 3G dye |
| WO2009092210A1 (en) * | 2008-01-22 | 2009-07-30 | Tianjin Dek Chemical Co., Ltd | A black active dye and the preparation thereof |
| CN101987300A (en) * | 2010-08-16 | 2011-03-23 | 天津德凯化工股份有限公司 | Phase transfer catalyst composition and preparation method thereof |
| CN102115614A (en) * | 2009-12-30 | 2011-07-06 | 上海雅运纺织化工有限公司 | Navy blue reactive dye composite and dyeing application thereof to fiber |
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| WO2009092210A1 (en) * | 2008-01-22 | 2009-07-30 | Tianjin Dek Chemical Co., Ltd | A black active dye and the preparation thereof |
| CN101481529A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Preparation of reactive dye for fur |
| CN101481524A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Preparation of reactive red 3G dye |
| CN101812244B (en) * | 2009-11-16 | 2013-06-19 | 天津德凯化工股份有限公司 | Reactive dye for dyeing nylon and preparation method thereof |
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| CN102115614B (en) * | 2009-12-30 | 2013-05-29 | 上海雅运纺织化工股份有限公司 | Navy blue reactive dye composite and dyeing application thereof to fiber |
| CN101987300A (en) * | 2010-08-16 | 2011-03-23 | 天津德凯化工股份有限公司 | Phase transfer catalyst composition and preparation method thereof |
| CN101987300B (en) * | 2010-08-16 | 2013-06-19 | 天津德凯化工股份有限公司 | Phase transfer catalyst composition and preparation method thereof |
| CN103642273A (en) * | 2013-11-21 | 2014-03-19 | 天津德凯化工股份有限公司 | Active black dye composition suitable for dyeing polyamide fibers |
| CN103642273B (en) * | 2013-11-21 | 2017-12-15 | 天津德凯化工股份有限公司 | A kind of active black dye composition suitable for Fypro dyeing |
| CN105566946A (en) * | 2015-12-22 | 2016-05-11 | 浙江亿得化工有限公司 | Composite reactive blue dye for wool and preparation method of composite reactive blue dye for wools |
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