CN101469138A - Stable high concentration liquid reactive dye mixture - Google Patents
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- CN101469138A CN101469138A CNA2007101254715A CN200710125471A CN101469138A CN 101469138 A CN101469138 A CN 101469138A CN A2007101254715 A CNA2007101254715 A CN A2007101254715A CN 200710125471 A CN200710125471 A CN 200710125471A CN 101469138 A CN101469138 A CN 101469138A
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Abstract
The invention relates to a liquid activated dye mixture with stability and high concentration. The liquid activity dye mixture comprises two or more than two dye compositions with structures which is shown as the right, wherein R1 is hydrogen, an alkoxyl group, an amino group, a hydroxyl group, SO3M or an amino-triazine derivant; R2 and R3 are hydrogen, an alkyl group, an alkoxyl group, an amino group, a hydroxyl group, acylamino or SO3M; R4 is a substituted benzene sulfonic acid group, a naphthalene sulfonic acid group, morpholinyl, pyrimidinyl, a pyridone group or a pyrazolone group derivant; M is hydrogen, an ammonium ion, a triethanolamine ion, a tri-isopropanolamine ion or an alkali metal ion. The liquid activated dye mixture has good stability, high solubility, and good level-dyeing property, substantially improves the dyeing rate, fastness rate and dyeing depth of the dye.
Description
[technical field]
The present invention relates to dye field, relate in particular to a kind of stable high concentration liquid reactive dye mixture.
[background technology]
Combining by covalent linkage of reactive dyestuffs and fiber realize, thus reactive dyestuffs on fiber, have good water-fastly wash, wet colour fastness such as moisture-proof friction, be the dye of present cellulose dyeing consumption maximum.Reactive dyestuffs can also be used for protein fibres such as wool, silk except can being used for cellulosic fibres such as cotton, fiber crops, viscose glue.The reactive dyestuffs chromatogram is complete, and is bright-colored, cheap, and adaptability is strong, and fastness is good, now developed into the cotton most important dye class in the dyestuff of using, becomes the dye that the world gives priority to and pays close attention to.
In printing and dyeing industry; Guan Yong solid property dyestuffs such as powder shape in the past; when sizing mixing or prepare dye liquor; the dyestuff dust is the most troubling problem; not only influence environment; be an impediment to labour protection; and often stick on the apparatus of batching or in the dye liquor of preparation and be suspended with the macrobead dyestuff that does not disperse or dissolve; the dyestuff of little, the dispersing property difference of solubleness particularly; wettability and dispersing property are all relatively poor; form agglomerate easily, these all can cause fault when textile dyeing, influence quality product.Advantages such as and there are not the problems referred to above substantially in liquid dye, and liquid dye have good flowability, can improve the solubleness of dyestuff, and liquid dye in use have simple to operation, and dissolving is fast, and color is gorgeous.
Liquid reactive dye also has three kinds of systems with the liquid dye of other dye class are the same, and is a kind of based on water, be the ideal liquid dye, but the solubleness of most of reactive dyestuffs in water is limited, make high density and need adopt special preparation technology; Another kind is based on solvent, relates to problems such as solvent recuperation and labour protection, as a kind of improvement, also adopts the mixture of water and solvent to make liquid dye; The third is that reactive dyestuffs are suspended in the water, becomes water dispersion.
There is not dry problem in liquid dye, but have the problem of long-term storage, and dyestuff is preserved under differing temps in liquid phase, are the technological difficulties of Working liquids dyestuff.General liquid dye should meet the following requirements: liquid should be stablized, and can store under long-term, big temperature difference condition; Has good flowability; Do not contain Toxic matter; The pH value is neutral; Can be with similar or other class dyestuffs are miscible or piece together to mix; At normal temperatures or be easy in the cold water disperse or dissolve; Should improve dye strength as far as possible; Applicable to multiple dyeing etc.
[summary of the invention]
Goal of the invention of the present invention provides a kind of stable high concentration liquid reactive dye mixture, to reach the storage stability that improves liquid reactive dye and the purpose of light stability.
For reaching above-mentioned purpose, technical scheme provided by the invention is, a kind of stable high concentration liquid reactive dye mixture is provided, and comprises the dye component that two or more has following structure:
Wherein, R
1Be hydrogen, alkoxyl group, amino, hydroxyl, SO
3M or triazine aminoderivative;
R
2, R
3Be hydrogen, alkyl, alkoxyl group, amino, carbonyl, amido or SO
3M;
R
4Be substituted benzenesulfonic acid base, naphthene sulfonic acid base, morpholinyl, pyrimidyl, pyriconyl or pyrazolone radical derivative;
M is hydrogen, ammonium ion, triethanol ammonium ion, three Virahol ammonium ion or alkalimetal ions.
Preferably, comprise two kinds of described dye components in the described dye mixture, the weight percent relation of these two kinds of dye components is 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4.
Preferably, comprise three kinds of described dye components in the described dye mixture, in these three kinds of dye components any two kinds of components and with the weight percent of the third component relation be 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4.
Preferably, comprise four kinds of described dye components in the described dye mixture, in these four kinds of dye components any two kinds of components and with the weight percent of other two kinds of components relation be 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4; Or any three kinds of components and with the weight percent of the 4th kind of component relation be 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4.
Preferably, the shared weight percent of reactive dyestuffs is 10%-50% in the described dye mixture.
Preferably, the pH buffer reagent that is selected from polyphosphoric acid salt, hydrophosphate, dihydrogen phosphate or polycarboxylic acid derivative that also contains 0.1%-5% in the described dye mixture.
Preferably, the content of described pH buffer reagent is 0.5%-2%.
Preferably, the preferred dicarboxylic acid derivatives of described pH buffer reagent, more preferably Succinic Acid and basic metal thereof or alkaline earth salt.
In the stable high concentration liquid reactive dye mixture provided by the present invention, the content of the ammoniacal liquor in the finished product, trolamine, tri-isopropanolamine or alkali-metal halogenide of equal value or vitriol is not more than 1% of dye mixture gross weight.
The present invention also provides a kind of preparation method of aforementioned stable high concentration liquid reactive dye mixture, comprises the steps:
S1 will contain the condensation component of at least two kinds of azo active dyestuffs of a plurality of sulfonic acid groups, in the presence of ammoniacal liquor, trolamine, tri-isopropanolamine or alkali metal hydroxide of equal value, by primary condensation reaction at least, obtain corresponding condensation product;
S2 by diazotization reaction, obtains corresponding diazonium salt with the diazonium salt component of at least a azo active dyestuff;
S3 is the condensation product and the diazonium salt that obtain among step S1 and the S2, in the presence of ammoniacal liquor, trolamine, tri-isopropanolamine or alkali metal hydroxide of equal value, mixes and carries out coupled reaction, obtains the liquid reactive dye mixture crude product;
S4 aforesaid liquid reactive dye mixture crude product process promptly gets stable high concentration liquid reactive dye mixture after concentrating and making with extra care.
Preferably, described liquid reactive dye mixture crude product is not more than 1% of dye mixture gross weight through the content that concentrates the ammoniacal liquor, trolamine, tri-isopropanolamine or alkali-metal halogenide of equal value or the vitriol that are contained in the finished product after making with extra care.
Aforementioned stable high concentration liquid reactive dye mixture provided by the present invention, also can adopt following step preparation:
S1 ' will contain the condensation component of at least two kinds of azo active dyestuffs of a plurality of sulfonic acid groups, in the presence of ammoniacal liquor, trolamine, tri-isopropanolamine or alkali metal hydroxide of equal value, by primary condensation reaction at least, obtain condensation product A1;
S2 ' is the condensation product A1 that obtains, or with the diazonium salt B component 1 of other at least a azo active dyestuffs, by diazotization reaction, obtains corresponding diazonium salt A2 or B2;
S3 ' mixes diazonium salt B2 with condensation product A1, in the presence of the alkali metal hydroxide of ammoniacal liquor, trolamine, tri-isopropanolamine or equivalence, by coupled reaction, obtain the reactive azo dyes intermediate;
Or,
One the contract diazonium salt A2 of product and the condensation component that contains at least two kinds of azo active dyestuffs of a plurality of sulfonic acid groups mixed, in the presence of the alkali metal hydroxide of ammoniacal liquor, trolamine, tri-isopropanolamine or equivalence, by coupled reaction, obtain the reactive azo dyes intermediate;
S4 ' is with the reactive azo dyes intermediate that obtains, mix with the condensation component of at least two kinds of azo active dyestuffs that contain a plurality of sulfonic acid groups, in the presence of the alkali metal hydroxide of ammoniacal liquor, trolamine, tri-isopropanolamine or equivalence, by primary condensation reaction at least, obtain the liquid reactive dye mixture crude product;
S5 ' liquid reactive dye mixture crude product process promptly gets stable high concentration liquid reactive dye mixture after concentrating and making with extra care.
Preferably, described liquid reactive dye mixture crude product is not more than 1% of dye mixture gross weight through the content that concentrates the ammoniacal liquor, trolamine, tri-isopropanolamine or alkali-metal halogenide of equal value or the vitriol that are contained in the finished product after making with extra care.
Aforementioned stable high concentration liquid reactive dye mixture provided by the present invention except that adopting aforementioned chemical synthesis process preparation, also can adopt the dye component that will have described structure directly to prepare in the mode of physical mixed.
Stable high concentration liquid reactive dye mixture solubleness height provided by the present invention, good level-dyeing property have significantly improved dye uptake, the fixation rate of dyestuff and have got color depth; Simultaneously, compare with other mixed types of the prior art or compound liquid reactive dye, dye mixture of the present invention has more excellent stability in storage and light stability, it is almost constant to store more than 3 months its pH value in 0 ℃ of-60 ℃ of scope, and can layering, flocculation, precipitation and crystallization.
[embodiment]
The dye component proportioning
In the numerous embodiments of stable high concentration liquid reactive dye mixture provided by the invention, the dye component of each embodiment is as shown in the table, and wherein the numerical value of each component is the percent value (wt%) that accounts for reactive dyestuffs gross weight in the dye solution:
Embodiment 1
Get 184.4 gram cyanuric chlorides and be dissolved in the 800 gram frozen water, adding is dissolved in the gram of 188.2 in 500 ml waters 2 under the violent stirring, and the 4-diamino benzene sulfonic acid carries out contracting, and keeps the pH value at 1.8-2.5 with lithium hydroxide, keeps 0 ℃-10 ℃ reactions of temperature 2-3 hour.One contracts product under agitation, adds the sodium nitrite solution of 172 grams 40%, and 400 gram ice cubes and 165 grams, 35% hydrochloric acid soln, continues to stir 1 hour down at 0 ℃-10 ℃, complete to diazotization.With diazonium salt and 254.3 1-(3 '-sulfonic group phenyl)-3-methyl-5-pyrazolone couplings that restrain that obtain, adjust the pH value to 4.5-6.0 with lithium hydroxide, be heated to 15 ℃-25 ℃ gradually, continue reaction 1-2 hour.Then add 69.3 gram Sulphanilic Acid and 101 grams 2 in coupling product, 5-disulfonic acid base aniline, reaction solution are heated to 30 ℃-40 ℃ gradually, adjust the pH value to 4.5-6.0 with lithium hydroxide, react 1-2 hour, finish two and contract.
Reaction solution obtains 2380 gram concentrated liquids through reverse osmosis ultra-filtration equipment desalination and concentrated.Stir down, add 20 gram Soduxins and 20 gram ε-Ji Neixianan, promptly obtain stable liquid reactive dye mixture commodity.
By analysis, this liquid reactive dye solid content is 32%, contains 3 kinds of reactive dyestuffs of following structure:
Its Chinese style 1a is the lithium salts of C.I. reaction yellow 18, accounts for 44% of reactive dyestuffs gross weight in the dye solution, and formula 1b dyestuff accounts for 40% of reactive dyestuffs gross weight in the dye solution, and formula 1c dyestuff accounts for 16% of reactive dyestuffs gross weight in the dye solution.
With the liquid reactive dye mixture of this method preparation, it is almost constant to store more than 3 months its pH value in 0 ℃ of-60 ℃ of scope, and can layering, flocculation, precipitation and crystallization, have good preservation stability.This liquid reactive dye mixture is used for the deep yellow that printing cellulose fibres can obtain level dyeing, and the dye uptake height, gets when more every kind of assembly of color depth union dyeing material list is solely used to be significantly increased.
Embodiment 2
Get 184.4 gram cyanuric chlorides and be dissolved in the 800 gram frozen water, adding is dissolved in the gram of 239.3 in 500 ml waters J acid under the violent stirring, keeps the pH value at 2-3 with ammoniacal liquor, keeps 0 ℃-10 ℃ of temperature, reacts 2 hours.One contracts product under agitation, adds 173.2 gram 3-aniline sulfonic acids, and reaction solution is heated to 30 ℃-40 ℃ gradually, adjusts the pH value to 5.0-6.5 with ammoniacal liquor, reacts 1-2 hour, finishes two and contracts.With 52 gram Sulphanilic Acid, 268.5 gram 2-naphthylamines-4,6, the 8-trisulfonic acid is dissolved in the water, and add 172 and restrain 40% sodium nitrite solution, and 300 gram ice cubes and 165 grams, 35% hydrochloric acid soln, stirred 1-1.5 hour down at 0 ℃-10 ℃, extremely fully diazotization.With the diazonium salt that obtains and the two product couplings of contracting that generate before, adjust the pH value to 6.5-7.0 with ammoniacal liquor, be heated to 20 ℃-25 ℃ gradually, continued stirring reaction 1-2 hour, finish until reaction.
Reaction solution obtains 3876 gram concentrated liquids through reverse osmosis ultra-filtration equipment desalination and concentrated.Stir down, add 40 gram Succinic Acid and 40 gram ε-Ji Neixianan, promptly obtain stable liquid reactive dye mixture commodity.
By analysis, this liquid reactive dye solid content is 24%, contains 2 kinds of reactive dyestuffs of following structure:
Its Chinese style 2a is reactive brilliant orange KM-7R, accounts for 75% of reactive dyestuffs gross weight in the dye solution, and formula 2b accounts for 25% of reactive dyestuffs gross weight in the dye solution, and M is an ammonium ion.
Liquid reactive dye mixture with this method preparation, solubleness when the solubleness of dyestuff is solely used than every kind of assembly union dyeing material list improves greatly, has good preservation stability, it is almost constant to store more than 3 months its pH value in 0 ℃ of-60 ℃ of scope, and can layering, flocculation, precipitation and crystallization.This liquid reactive dye mixture be used for printing cellulose fibres can obtain bright-coloured orange, the dye uptake height, and color depth is pieced together when the union dyeing material list is solely used for more every kind and is significantly increased.
Embodiment 3
Get 700 gram frozen water and 184.4 gram cyanuric chlorides under violent stirring, spray into and be scattered in 319.3 in 600 ml waters grams H acid, carry out contracting, add the trolamine aqueous solution of about 200 grams 85%, keep the pH value at 1.0-2.0, keep 5 ℃-10 ℃ reactions of temperature about 2 hours.46.6 gram aniline and 144.2 grams 1 under the 5-naphthalene disulfonic acid stirs, add the sodium nitrite solution and 165 grams, 35% hydrochloric acid soln of 172 grams 40% in frozen water, stirred 1-2 hour down at 5 ℃-10 ℃, and are complete to diazotization.The diazonium salt that obtains and cyanuric chloride with one of the H acid product coupling of contracting, are adjusted the pH value to 5.0-6.0 with about 700 grams, 85% trolamine aqueous solution, be heated to 15 ℃-20 ℃ gradually, continue to react 2-3 hour, disappear to diazonium salt.Then add position ester between 140 gram para-esters and 154.7 gram N-ethyls in coupling product, reaction solution is heated to 30 ℃-40 ℃ gradually, adds about 270 grams, 85% tri-isopropanolamine aqueous solution and adjusts the pH value to 5.5-6.5, reacts 2-3 hour, finishes two and contracts.
Reaction solution obtains 3920 gram concentrated liquids through reverse osmosis ultra-filtration equipment desalination and concentrated.Stir down, add 30 gram Succinic Acid and 30 gram ε-Ji Neixianan, promptly obtain stable liquid reactive dye mixture commodity.
By analysis, this liquid reactive dye solid content is 42%, contains 4 kinds of reactive dyestuffs of following structure:
Wherein dyestuff 3a is C.I. and reacts red 261, account for 20.7% of reactive dyestuffs gross weight in the dye solution, dyestuff 3b accounts for 21.1% of reactive dyestuffs gross weight in the dye solution, dyestuff 3c is that C.I. reacts red 241, account for 28.9% of reactive dyestuffs gross weight in the dye solution, dyestuff 3d accounts for 29.3% of reactive dyestuffs gross weight in the dye solution, and M is triethanol ammonium ion or three Virahol ammonium ions, and triethanol ammonium ion and three Virahol ammonium ion mol ratios are 3:1 in the liquid reactive dye mixture.
With the liquid reactive dye mixture of this method preparation, it is almost constant to store more than 3 months its pH value in 0 ℃ of-60 ℃ of scope, and can layering, flocculation, precipitation and crystallization, have good preservation stability.This liquid reactive dye mixture is used for the scarlet that printing cellulose fibres can obtain level dyeing, and the dye uptake height, gets when more every kind of assembly of color depth union dyeing material list is solely used to be significantly increased.
Embodiment 4
Get 184.4 gram cyanuric chlorides in 700 gram frozen water under the violent stirring, spray into and be scattered in the gram of 319.3 in 600 ml waters H acid, carry out contracting, adding about 24 gram lithium hydroxides keeps the pH value at 2-3, keep 0 ℃-10 ℃ of temperature, add 36 gram urea, continue reaction 2 hours.123.2 gram Para-Anisidines are dissolved in the water, add 172 and restrain 40% sodium nitrite solution, and 300 gram ice cubes and 165 grams, 35% hydrochloric acid soln, stirred 1-1.5 hour down at 0 ℃-10 ℃, extremely fully diazotization.With the diazonium salt that obtains and the product coupling of contracting that generates before, adjust the pH value to 6.5-7.0 with ammoniacal liquor, be heated to 20 ℃-25 ℃ gradually, continued stirring reaction 1-2 hour, finish until reaction.
Reaction solution obtains 2280 gram concentrated liquids through reverse osmosis ultra-filtration equipment desalination and concentrated.Stir down, add 20 gram Succinic Acid and 20 gram ε-Ji Neixianan, promptly obtain stable liquid reactive dye mixture commodity.
By analysis, this liquid reactive dye solid content is 28%, contains 2 kinds of reactive dyestuffs of following structure:
Its Chinese style 4a is C.I. reactive violet 8, account for 39% of reactive dyestuffs gross weight in the dye solution, formula 4b is reactive violet 2R, accounts for 61% of reactive dyestuffs gross weight in the dye solution, M is lithium ion or ammonium ion, and the mol ratio of lithium salts and ammonium salt is 1:1 in the liquid reactive dye mixture.
Liquid reactive dye mixture with this method preparation, solubleness when the solubleness of dyestuff is solely used than every kind of assembly union dyeing material list improves greatly, has good preservation stability, it is almost constant to store more than 3 months its pH value in 0 ℃ of-60 ℃ of scope, and can layering, flocculation, precipitation and crystallization.This liquid reactive dye mixture is used for the purple that printing cellulose fibres can obtain level dyeing, the dye uptake height, and more every kind of color depth is pieced together when the union dyeing material list is solely used and is significantly increased.
Embodiment 5
Get dye component 1a, 1b and/or 1c and dye component 5a and/or 5b as follows in the foregoing description 1, ratio according to (1:9)～(9:1), uniform mixing in the presence of water, pH buffer reagent promptly gets stable high concentration liquid reactive dye mixture provided by the invention.
Its Chinese style 5a is the C.I. REACTIVE Yellow 145, and formula 5b is a C.I. reactive yellow 176, and M is ammonium ion or lithium ion or trolamine ion, tri-isopropanolamine ion.
Stability test
Get the liquid reactive dye mixture of gained among the foregoing description 1-4, store 360 days in 0 ℃ of-60 ℃ of scope, carry out stability test, its result is as shown in the table:
| Concentration (%) | 30 days | 90 days | 180 days | 270 days | 360 days | |
| Embodiment 1 dye solution | 32 | ○ | ○ | ○ | ○ | ▲ |
| Embodiment 2 dye solutions | 24 | ○ | ○ | ○ | ○ | ○ |
| Embodiment 3 dye solutions | 42 | ○ | ○ | ○ | ○ | ▲ |
| Embodiment 4 dye solutions | 28 | ○ | ○ | ○ | ○ | ○ |
In the last table, the no layering of symbol " zero " expression, flocculation, precipitation and crystallization, few precipitation is separated out in symbol " ▲ " expression.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a stable high concentration liquid reactive dye mixture is characterized in that, comprises the dye component that two or more has following structure:
Wherein, R
1Be hydrogen, alkoxyl group, amino, hydroxyl, SO
3M or triazine aminoderivative;
R
2, R
3Be hydrogen, alkyl, alkoxyl group, amino, carbonyl, amido or SO
3M;
R
4Be substituted benzenesulfonic acid base, naphthene sulfonic acid base, morpholinyl, pyrimidyl, pyriconyl or pyrazolone radical derivative;
M is hydrogen, ammonium ion, triethanol ammonium ion, three Virahol ammonium ion or alkalimetal ions.
2. stable high concentration liquid reactive dye mixture according to claim 1 is characterized in that, wherein comprises two kinds of described dye components, and the weight percent relation of these two kinds of dye components is 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4.
3. stable high concentration liquid reactive dye mixture according to claim 1, it is characterized in that, wherein comprise three kinds of described dye components, in these three kinds of dye components any two kinds of components and with the weight percent of the third component relation be 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4.
4. stable high concentration liquid reactive dye mixture according to claim 1, it is characterized in that, wherein comprise four kinds of described dye components, in these four kinds of dye components any two kinds of components and with the weight percent of other two kinds of components relation be 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4; Or any three kinds of components and with the weight percent of the 4th kind of component relation be 1:9～9:1, preferred 3:7～7:3, more preferably 4:6～6:4.
5. stable high concentration liquid reactive dye mixture according to claim 1 is characterized in that, the shared weight percent of reactive dyestuffs is 10%-50% in the described dye mixture.
6. stable high concentration liquid reactive dye mixture according to claim 1 or 5, it is characterized in that, also contain the pH buffer reagent that is selected from polyphosphoric acid salt, hydrophosphate, dihydrogen phosphate or polycarboxylic acid derivative of 0.1%-5% in the described dye mixture; The preferred 0.5%-2% of the content of this pH buffer reagent; The preferred dicarboxylic acid derivatives of this pH buffer reagent, more preferably Succinic Acid and basic metal thereof or alkaline earth salt.
7. as the preparation method of claim 1 or 5 described stable high concentration liquid reactive dye mixtures, its step comprises:
S1 will contain the condensation component of at least two kinds of azo active dyestuffs of a plurality of sulfonic acid groups, in the presence of ammoniacal liquor, trolamine, tri-isopropanolamine or alkali metal hydroxide of equal value, by primary condensation reaction at least, obtain corresponding condensation product;
S2 by diazotization reaction, obtains corresponding diazonium salt with the diazonium salt component of at least a azo active dyestuff;
S3 is the condensation product and the diazonium salt that obtain among step S1 and the S2, in the presence of ammoniacal liquor, trolamine, tri-isopropanolamine or alkali metal hydroxide of equal value, mixes and carries out coupled reaction, obtains the liquid reactive dye mixture crude product;
S4 aforesaid liquid reactive dye mixture crude product process promptly gets stable high concentration liquid reactive dye mixture after concentrating and making with extra care.
8. the preparation method of stable high concentration liquid reactive dye mixture according to claim 7, it is characterized in that, after described liquid reactive dye mixture crude product process concentrated and makes with extra care, wherein the content of the ammoniacal liquor that is contained, trolamine, tri-isopropanolamine or alkali-metal halogenide of equal value or vitriol was not more than 1% of dye mixture gross weight.
9. as the preparation method of claim 1 or 5 described stable high concentration liquid reactive dye mixtures, its step comprises:
S1 ' will contain the condensation component of at least two kinds of azo active dyestuffs of a plurality of sulfonic acid groups, in the presence of ammoniacal liquor, trolamine, tri-isopropanolamine or alkali metal hydroxide of equal value, by primary condensation reaction at least, obtain condensation product A1;
S2 ' is the condensation product A1 that obtains, or with the diazonium salt B component 1 of other at least a azo active dyestuffs, by diazotization reaction, obtains corresponding diazonium salt A2 or B2;
S3 ' mixes diazonium salt B2 with condensation product A1, in the presence of the alkali metal hydroxide of ammoniacal liquor, trolamine, tri-isopropanolamine or equivalence, by coupled reaction, obtain the reactive azo dyes intermediate;
Or,
The diazonium salt A2 of condensation product and the condensation component of at least two kinds of azo active dyestuffs that contain a plurality of sulfonic acid groups are mixed, in the presence of the alkali metal hydroxide of ammoniacal liquor, trolamine, tri-isopropanolamine or equivalence, by coupled reaction, obtain the reactive azo dyes intermediate;
S4 ' is with the reactive azo dyes intermediate that obtains, mix with the condensation component of at least two kinds of azo active dyestuffs that contain a plurality of sulfonic acid groups, in the presence of the alkali metal hydroxide of ammoniacal liquor, trolamine, tri-isopropanolamine or equivalence, by primary condensation reaction at least, obtain the liquid reactive dye mixture crude product;
S5 ' liquid reactive dye mixture crude product process promptly gets stable high concentration liquid reactive dye mixture after concentrating and making with extra care.
10. the preparation method of stable high concentration liquid reactive dye mixture according to claim 9, it is characterized in that, after described liquid reactive dye mixture crude product process concentrated and makes with extra care, wherein the content of the ammoniacal liquor that is contained, trolamine, tri-isopropanolamine or alkali-metal halogenide of equal value or vitriol was not more than 1% of dye mixture gross weight.
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| CN104559320A (en) * | 2014-04-28 | 2015-04-29 | 无锡润新染料有限公司 | Composite active brilliant orange dye composition |
| CN107501996A (en) * | 2017-09-07 | 2017-12-22 | 上海万得化工有限公司 | A kind of synthetic method of black and active dye compound |
| CN107699001A (en) * | 2017-09-01 | 2018-02-16 | 浙江劲光实业股份有限公司 | A kind of preparation method of active scarlet dye |
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| CN104559320A (en) * | 2014-04-28 | 2015-04-29 | 无锡润新染料有限公司 | Composite active brilliant orange dye composition |
| CN107699001A (en) * | 2017-09-01 | 2018-02-16 | 浙江劲光实业股份有限公司 | A kind of preparation method of active scarlet dye |
| CN107501996A (en) * | 2017-09-07 | 2017-12-22 | 上海万得化工有限公司 | A kind of synthetic method of black and active dye compound |
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