CN102504588A - Turquoise blue active dye, as well as preparation method and application thereof - Google Patents
Turquoise blue active dye, as well as preparation method and application thereof Download PDFInfo
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- CN102504588A CN102504588A CN2011102934093A CN201110293409A CN102504588A CN 102504588 A CN102504588 A CN 102504588A CN 2011102934093 A CN2011102934093 A CN 2011102934093A CN 201110293409 A CN201110293409 A CN 201110293409A CN 102504588 A CN102504588 A CN 102504588A
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Abstract
The invention provides a turquoise blue active dye, as well as a preparation method and an application thereof. The dye has a structure in the specification, wherein the sum of x and y is 3.5. The dye has the advantages of small average grain diameter, low salt content, bright color in dyeing, high dyeing degree, stability, good reproducibility, use availability in ink-jet printing, excellent application performance and convenience in use; and preparation and application of the dye can reduce environmental pollution, and the cost for required raw materials is low.
Description
Technical field
The present invention relates to a kind of reactive dyestuffs, especially a kind of turquoise blue reactive dyestuffs and preparation method thereof and the application in ink-jet printed.
Background technology
Ink-jet printed technology is exactly one of them main field, and this technology mainly contains two kinds: i.e. continous inkjet and drop on demand ink jet.These two kinds of printing techniques all have particular requirement to dyestuff in the ink or pigment dyestuff, like the purity of the pH value of the electric conductivity of the chemical structure of dyestuff, median size, the formation aqueous solution, dyestuff, the dyestuff content etc. of inorganic salt particularly.Development along with digital technique; Accurately control dyeing course with computingmachine, can enhance productivity and yield rate, reduce production costs; Reduce the pollution level of waste water to greatest extent; And present ink-jet is bigger with the dyestuff median size, and saltiness is high, dye uptake is low and fastness is low, can not satisfy ink-jet printed demand fully.
Summary of the invention
In order to solve the problems of the technologies described above, to the invention provides a kind of technical scheme and be: a kind of turquoise blue reactive dyestuffs have following general structure:
Wherein
X+y=3.5 in the formula, x＞0, y＞0;
R
1For:
R
2For:
Further preferably, R in the above-mentioned dyestuff
1For:
R
2For:
The preparation method of above-mentioned dyestuff, this method comprises the steps:
A, chlorosulfonation, ice are analysed
The cooling of adding chlorsulfonic acid circulating water after the reaction of adding CuPc, adds the sulfur oxychloride reaction again in enamel pot, gets the chlorosulphonation feed liquid; Adjust temperature once more, the chlorosulphonation feed liquid of gained is joined ice with thread analyse in the jar, controlled temperature stirs; Obtain ice and analyse liquid, ice is analysed liquid join in the solid-liquid separator, separate, get filter cake; The cold water washing filter cake is removed spent acid to the pH=7 that filtrates, and collects filter cake;
B, A substance dissolves
The A material is added in the entry, transfer pH=7, material is dissolved entirely with 30% sodium hydroxide solution, clarification, wherein A is a kind of in m-sulfanilic acid, Sulphanilic Acid, the ORTHO AMINO PHENOL SULPHONIC;
C, B substance dissolves
The B material is added in the entry, transfer pH=4, material is dissolved entirely with 15% sodium carbonate solution, clarification, wherein the B material is 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline or 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline;
D, condensation
A step gained filter cake is joined in the mixing solutions of b, c step gained solution, keep pH=7～8 with 30% sodium hydroxide solution, stirring reaction, reaction pH=7～8 are used the aluminium base silica gel thin-layer plate endpoint detection of TLC at last; Obtain the product of structural formula (I).
The preparation method of above-mentioned dyestuff further preferably, this method comprises the steps:
A, chlorosulfonation, ice are analysed
In enamel pot, add chlorsulfonic acid, the circulating water cooling, 40～50 ℃ of controlled temperature were adjusted 140 ℃ of temperature with the CuPc adding in 2 hours consuming time; 140～145 ℃ of holding temperatures were reacted 3 hours, and adjustment temperature to 65～70 ℃ are kept 2 hours consuming time; With 630 kilograms of addings of sulfur oxychloride, 65～70 ℃ of holding temperatures were reacted after 2 hours, 90 ℃ of adjustment temperature, 90～95 ℃ of holding temperatures; Reacted 1 hour, and adjusted temperature to 115 ℃ again, 115～120 ℃ of holding temperatures were reacted 3 hours;
20～25 ℃ of temperature of adjustment join ice with the chlorosulphonation feed liquid of gained with thread and analyse in the jar controlled temperature, 2 hours consuming time; Holding temperature-5～5 ℃ stirred 1 hour, must ice and analyse liquid, ice is analysed liquid join in the solid-liquid separator; Separate, filter cake, again with temperature-5～5 ℃ cold water washing filter cake to the pH ≈ 7 that filtrates; Remove spent acid, collect filter cake, filtrating is deposited in the spent acid storage tank;
B, A substance dissolves
In enamel pot, put into Di Shui, add the A material, transfer pH=7 with 30% sodium hydroxide solution, material is dissolved entirely, clarify, the mass percent concentration of solution is 10%, and wherein A is a kind of in m-sulfanilic acid, Sulphanilic Acid, the ORTHO AMINO PHENOL SULPHONIC;
C, B substance dissolves
In enamel pot, put into Di Shui, add the B material, transfer pH=4 with 15% sodium carbonate solution; Material is dissolved entirely; Clarification, the mass percent concentration of solution is 10%, wherein the B material is 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline or 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline;
D, condensation
A step gained filter cake is joined in b, the c mixed in step solution, and adjustment temperature to 35 ℃ is kept pH=7～8 with 30% sodium hydroxide solution; Stirring reaction 15～20 hours; 35～40 ℃ of temperature of reaction, reaction pH=7～8 are used the aluminium base silica gel thin-layer plate endpoint detection of TLC at last; Obtain the product of structural formula (I).
Above-mentioned any preparation method, this method also comprises the post-processing step of product, and this post-processing step comprises:
E, interpolation auxiliary agent
With sodium sulfate, mixed phosphate, one or more among Sodium hexametaphosphate 99, EDTA, the NNO join in the product solution of structural formula (I), stir, and are subsequent use;
F, removal insolubles
E step gained reaction solution is joined in the solid-liquid separator, separate, washery refuse is removed insolubles, collects feed liquid simultaneously in storage tank;
G, purification
With the feed liquid of collecting through membrane filtration, and with the concentration of the feed liquid percentage concentration 25% that improves the quality.One time membrane filtration waste water joins in the look liquid, continues membrane filtration.Secondary membrane filtration waste water as dyestuff at the bottom of water jacket use;
The adjustment of h, coloured light and intensity
From the reaction storage tank, extract feed liquid 200ml, dry and dyeing with disk; According to coloration result, add an amount of other batch dyestuff, carry out the coloured light adjustment, add glucose in proportion according to the UV intensity of dyestuff again and Sodium sulfate anhydrous.min(99) carries out the adjustment of intensity;
I, drying
The look liquid of h step is joined in the feed liquid preheater, adjust 210 ℃ of spray tower inlet temperatures, carry out spraying drying with 95～100 ℃ temperature outs.
Used raw material all is a disclosed known compound in the prior art in the aforesaid method, all can buy from market to obtain.
Chemically-reactive dyes of the present invention is suitable for multiple material is dyeed and stamp, and particularly hydroxyl or nitrogenous filamentary material comprise the cellulosic fibre material of paper, silk, leather, wool, tynex and urethane, particularly all kinds.Described filamentary material is a native cellulose fibre for example, like cotton, flax and hemp and Mierocrystalline cellulose and regenerated cellulose.Dyestuff of the present invention also is suitable for the hydroxyl fiber that exists in the BLENDED FABRIC is dyeed and stamp.
Reactive dye of the present invention is particluarly suitable for using ink jet printing method that fabric fiber material, paper or plastics film are printed dyeing or stamp; Dyestuff should have low saline salinity when being used for ink jet printing method; The dyestuff that has than supersalinity can carry out desalination like technology such as ultrafiltration, r-o-or dialysis and reach low saline salinity through for example membrane separation process.
The dyestuff product of resulting structures formula of the present invention (I), the average diameter grain is little, and saltiness is low; Beautiful in colour during dyeing, dye uptake is high, and is stable; Favorable reproducibility is particularly useful for using in the ink-jet cloth printing, and application performance is excellent; Easy to use, preparation of this dyestuff simultaneously and application can reduce environmental pollution, and the desired raw material cost is low.
Embodiment
Following embodiment just to the explanation of technical scheme of the present invention, does not form any restriction to technical scheme of the present invention and protection domain.
Embodiment 1
A, chlorosulfonation, ice are analysed
In enamel pot, add 1750 kilograms of chlorsulfonic acids. circulating water cooling, 40～50 ℃ of controlled temperature.CuPc added in 2 hours consuming time.140 ℃ of adjustment temperature, 140～145 ℃ of holding temperatures were reacted 3 hours.65 ℃ of adjustment temperature, 65～70 ℃ of holding temperatures, 2 hours consuming time with 630 kilograms of addings of sulfur oxychloride.65～70 ℃ of holding temperatures were reacted 2 hours.90 ℃ of adjustment temperature, 90～95 ℃ of holding temperatures were reacted 1 hour.115 ℃ of adjustment temperature.115～120 ℃ of holding temperatures were reacted 3 hours.
20～25 ℃ of temperature of adjustment join ice with the chlorosulphonation feed liquid of gained with thread and analyse in the jar controlled temperature.2 hours consuming time, the chlorosulphonation feed liquid is added.Holding temperature-5～5 ℃ stirred 1 hour.Ice is analysed liquid join in the solid-liquid separator, separate.To the pH ≈ 7 that filtrates, remove spent acid with temperature-5～5 ℃ cold water washing filter cake.Collect filter cake.Filtrating is deposited in the spent acid storage tank.
B, Sulphanilic Acid dissolving
In enamel pot, put into 1000 liters in end water, add Sulphanilic Acid 154Kg, transfer pH=7, material is dissolved entirely, clarification with 30% sodium hydroxide solution.Volume is 1550 liters, and the mass percent concentration of solution is 10%.
C, 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline dissolving
In enamel pot, put into 2700 liters in end water, add 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline 368.5Kg, transfer pH=4, material is dissolved entirely, clarification with 15% sodium carbonate solution.Volume is 3700 liters, and the mass percent concentration of solution is 10%.
D, condensation
A step gained filter cake is joined in b, the c mixed in step solution adjustment temperature to 35 ℃.Keep pH=7～8 with 30% sodium hydroxide solution, stirring reaction 15～20 hours.35～40 ℃ of temperature of reaction, reaction pH=7～8.Use the aluminium base silica gel thin-layer plate endpoint detection of TLC at last.
E, interpolation auxiliary agent
With 50 kilograms sodium sulfate, mixed phosphate, one or more among Sodium hexametaphosphate 99, EDTA, the NNO join in the d step gained reaction solution, stir 15 minutes, and are subsequent use.
F, removal insolubles
E step reaction liquid is joined in the solid-liquid separator, separate, washery refuse is removed insolubles, collects feed liquid simultaneously in storage tank.1.3 the waste residue about kilogram is used for engineering soil.
G, purification
With the filtrating of collecting through membrane filtration, and with the concentration of the feed liquid percentage concentration 25% that improves the quality.One time membrane filtration waste water joins in the look liquid, continues membrane filtration.Secondary membrane filtration waste water as dyestuff at the bottom of water jacket use.
The adjustment of h, coloured light and intensity
From the reaction storage tank, extract feed liquid 200ml, dry and dyeing with disk.According to coloration result, add an amount of other batch dyestuff, carry out the coloured light adjustment.Add glucose in proportion according to the UV intensity of dyestuff again and Sodium sulfate anhydrous.min(99) carries out the adjustment of intensity.
I, drying
The look liquid of h step is joined in the feed liquid preheater, adjust 210 ℃ of spray tower inlet temperatures, carry out spraying drying with 95～100 ℃ temperature outs.
J, the packing of product
The dyestuff of spraying drying gained is packed by the specification of 25 kilograms in every case.Get formula turquoise blue dyestuff
When wherein 2-methoxyl group in the c step-4-β hydroxyethyl sulfuryl sulfate ester aniline being replaced with 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline, the emerald green blue dye of formula:
Embodiment 2
A, chlorosulfonation, ice are analysed
In enamel pot, add 1750 kilograms of chlorsulfonic acids. circulating water cooling, 40～50 ℃ of controlled temperature.CuPc being added in 2 hours consuming time. 110 ℃ of adjustment temperature, 110～115 ℃ of holding temperatures were reacted 4 hours.55 ℃ of adjustment temperature, 55～60 ℃ of holding temperatures, 2 hours consuming time with 350 kilograms of addings of sulfur oxychloride.55～60 ℃ of holding temperatures were reacted 3 hours.90 ℃ of adjustment temperature, 90～95 ℃ of holding temperatures were reacted 1 hour.105 ℃ of adjustment temperature.105～110 ℃ of holding temperatures were reacted 3 hours.
10～15 ℃ of temperature of adjustment join ice with the chlorosulphonation feed liquid of gained with thread and analyse in the jar controlled temperature.2 hours consuming time, the chlorosulphonation feed liquid is added.0～10 ℃ of holding temperature stirred 1 hour.Ice is analysed liquid join in the solid-liquid separator, separate.To the pH=7 that filtrates, remove spent acid with 0～10 ℃ of cold water washing filter cake of temperature.Collect filter cake.Filtrating is deposited in the spent acid storage tank.
B, ORTHO AMINO PHENOL SULPHONIC dissolving
In enamel pot, put into 2000 liters in end water, add ORTHO AMINO PHENOL SULPHONIC 235.7Kg, transfer pH=7, material is dissolved entirely, clarification with 30% sodium hydroxide solution.Volume is 2950 liters, and the quality percentage concentration of solution is 8%.
C, 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline dissolving
In enamel pot, put into 1300 liters in end water, add 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline 221.1Kg, transfer pH=4, material is dissolved entirely, clarification with 15% sodium carbonate solution.Volume is 1850 liters, and the quality percentage concentration of solution is 12%.
D, condensation
A step gained filter cake is joined in b, the c mixed in step solution adjustment temperature to 35 ℃.Keep pH=7～8 with 30% sodium hydroxide solution, stirring reaction 15～20 hours.35～40 ℃ of temperature of reaction, reaction pH=7～8.Use the aluminium base silica gel thin-layer plate endpoint detection of TLC at last.
E, interpolation auxiliary agent
With 50 kilograms sodium sulfate, mixed phosphate, in the d step gained reaction solution that one or more among Sodium hexametaphosphate 99, EDTA, the NNO join, stirred 15 minutes, subsequent use.
F, removal insolubles
E step reaction liquid is joined in the solid-liquid separator, separate, washery refuse is removed insolubles, collects feed liquid simultaneously in storage tank.1.3 the waste residue about kilogram is used for engineering soil.
G, purification
With the filtrating of collecting through membrane filtration, and with the concentration of the feed liquid percentage concentration 25% that improves the quality.One time membrane filtration waste water joins in the look liquid, continues membrane filtration.Secondary membrane filtration waste water as dyestuff at the bottom of water jacket use.
The adjustment of h, coloured light and intensity
From the reaction storage tank, extract feed liquid 200ml, dry and dyeing with disk.According to coloration result, add an amount of other batch dyestuff, carry out the coloured light adjustment.Add glucose in proportion according to the UV intensity of dyestuff again and Sodium sulfate anhydrous.min(99) carries out the adjustment of intensity.
I, drying
The look liquid of step h is joined in the feed liquid preheater, adjust 210 ℃ of spray tower inlet temperatures, carry out spraying drying with 95～100 ℃ temperature outs.
J, the packing of product
The dyestuff of spraying drying gained is packed by the specification of 25 kilograms in every case.Get formula turquoise blue dyestuff
When wherein 2-methoxyl group in the c step-4-β hydroxyethyl sulfuryl sulfate ester aniline being replaced with 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline, the emerald green blue dye of formula:
Embodiment 3
A, chlorosulfonation, ice are analysed
In enamel pot, add 1750 kilograms of chlorsulfonic acids. circulating water cooling, 40～50 ℃ of controlled temperature.CuPc being added in 2 hours consuming time. 115 ℃ of adjustment temperature, 115～120 ℃ of holding temperatures were reacted 4 hours.60 ℃ of adjustment temperature, 60～65 ℃ of holding temperatures, 2 hours consuming time with 420 kilograms of addings of sulfur oxychloride.60～65 ℃ of holding temperatures were reacted 3 hours.90 ℃ of adjustment temperature, 90～95 ℃ of holding temperatures were reacted 1 hour.105 ℃ of adjustment temperature.105～110 ℃ of holding temperatures were reacted 3 hours.
15～20 ℃ of temperature of adjustment join ice with the chlorosulphonation feed liquid of gained with thread and analyse in the jar controlled temperature.2 hours consuming time, the chlorosulphonation feed liquid is added.0～10 ℃ of holding temperature stirred 1 hour.Ice is analysed liquid join in the solid-liquid separator, separate.To the pH=6 that filtrates, remove spent acid with 0～10 ℃ of cold water washing filter cake of temperature.Collect filter cake.Filtrating is deposited in the spent acid storage tank.
B, m-sulfanilic acid dissolving
In enamel pot, put into 1000 liters in end water, add m-sulfanilic acid 184.5Kg, transfer pH=7, material is dissolved entirely, clarification with 30% sodium hydroxide solution.Volume is 1550 liters, and the quality percentage concentration of solution is 12%.
C, 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline dissolving
In enamel pot, put into 2000 liters in end water, add 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline 313.2Kg, transfer pH=4, material is dissolved entirely, clarification with 15% sodium carbonate solution.Volume is 3150 liters, and the quality percentage concentration of solution is 10%.
D, condensation
A step gained filter cake is joined in b, the c mixed in step solution adjustment temperature to 35 ℃.Keep pH=7～8 with 30% sodium hydroxide solution, stirring reaction 15～20 hours.35～40 ℃ of temperature of reaction, reaction pH=7～8.Use the aluminium base silica gel thin-layer plate endpoint detection of TLC at last.
E, interpolation auxiliary agent
With 50 kilograms sodium sulfate, mixed phosphate, one or more among Sodium hexametaphosphate 99, EDTA, the NNO join in the d step gained reaction solution, stir 15 minutes, and are subsequent use.
F, removal insolubles
E step reaction liquid is joined in the solid-liquid separator, separate, washery refuse is removed insolubles, collects feed liquid simultaneously in storage tank.1.3 the waste residue about kilogram is used for engineering soil.
G, purification
With the filtrating of collecting through membrane filtration, and with the concentration of the feed liquid percentage concentration 25% that improves the quality.One time membrane filtration waste water joins in the look liquid, continues membrane filtration.Secondary membrane filtration waste water as dyestuff at the bottom of water jacket use.
The adjustment of h, coloured light and intensity
From the reaction storage tank, extract feed liquid 200ml, dry and dyeing with disk.According to coloration result, add an amount of other batch dyestuff, carry out the coloured light adjustment.Add glucose in proportion according to the UV intensity of dyestuff again and Sodium sulfate anhydrous.min(99) carries out the adjustment of intensity.
I, drying
The look liquid of h step is joined in the feed liquid preheater, adjust 210 ℃ of spray tower inlet temperatures, carry out spraying drying with 95～100 ℃ temperature outs.
J, the packing of product
The dyestuff of spraying drying gained is packed by the specification of 25 kilograms in every case.Get formula turquoise blue dyestuff
When wherein 2-methoxyl group in the c step-4-β hydroxyethyl sulfuryl sulfate ester aniline being replaced with 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline, the emerald green blue dye of formula:
Claims (7)
1. turquoise blue reactive dyestuffs is characterized in that this dyestuff has following general structure:
X+y=3.5 wherein, x＞0, y＞0;
R
1For:
R
2For:
2. dyestuff according to claim 1, R
1For:
R
2For:
3. the preparation method of dyestuff according to claim 1, this method comprises the steps:
A, chlorosulfonation, ice are analysed
The cooling of adding chlorsulfonic acid circulating water after the reaction of adding CuPc, adds the sulfur oxychloride reaction again in enamel pot, gets the chlorosulphonation feed liquid; Adjust temperature once more, the chlorosulphonation feed liquid of gained is joined ice with thread analyse in the jar, controlled temperature stirs; Obtain ice and analyse liquid, ice is analysed liquid join in the solid-liquid separator, separate, get filter cake; The cold water washing filter cake is removed spent acid to the pH=7 that filtrates, and collects filter cake;
B, A substance dissolves
The A material is added in the entry, transfer pH=7, material is dissolved entirely with 30% sodium hydroxide solution, clarification, wherein A is a kind of in m-sulfanilic acid, Sulphanilic Acid, the ORTHO AMINO PHENOL SULPHONIC;
C, B substance dissolves
The B material is added in the entry, transfer pH=4, material is dissolved entirely with 15% sodium carbonate solution, clarification, wherein the B material is 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline or 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline;
D, condensation
A step gained filter cake is joined in the mixing solutions of b, c step gained solution, keep pH=7～8 with 30% sodium hydroxide solution, stirring reaction, reaction pH=7～8 are used the aluminium base silica gel thin-layer plate endpoint detection of TLC at last; Obtain the product of structural formula (I).
4. the preparation method of dyestuff according to claim 3, this method comprises the steps:
A, chlorosulfonation, ice are analysed
In enamel pot, add chlorsulfonic acid, the circulating water cooling, 40～50 ℃ of controlled temperature were adjusted 140 ℃ of temperature with the CuPc adding in 2 hours consuming time; 140～145 ℃ of holding temperatures were reacted 3 hours, and adjustment temperature to 65～70 ℃ are kept 2 hours consuming time; With 630 kilograms of addings of sulfur oxychloride, 65～70 ℃ of holding temperatures were reacted after 2 hours, 90 ℃ of adjustment temperature, 90～95 ℃ of holding temperatures; Reacted 1 hour, and adjusted temperature to 115 ℃ again, 115～120 ℃ of holding temperatures were reacted 3 hours;
20～25 ℃ of temperature of adjustment join ice with the chlorosulphonation feed liquid of gained with thread and analyse in the jar controlled temperature, 2 hours consuming time; Holding temperature-5～5 ℃ stirred 1 hour, must ice and analyse liquid, ice is analysed liquid join in the solid-liquid separator; Separate, filter cake, again with temperature-5～5 ℃ cold water washing filter cake to the pH ≈ 7 that filtrates; Remove spent acid, collect filter cake, filtrating is deposited in the spent acid storage tank;
B, A substance dissolves
In enamel pot, put into Di Shui, add the A material, transfer pH=7 with 30% sodium hydroxide solution, material is dissolved entirely, clarify, the mass percent concentration of solution is 10%, and wherein A is a kind of in m-sulfanilic acid, Sulphanilic Acid, the ORTHO AMINO PHENOL SULPHONIC;
C, B substance dissolves
In enamel pot, put into Di Shui, add the B material, transfer pH=4 with 15% sodium carbonate solution; Material is dissolved entirely; Clarification, the mass percent concentration of solution is 10%, wherein the B material is 2-methoxyl group-4-β hydroxyethyl sulfuryl sulfate ester aniline or 2-methoxyl group-5-β hydroxyethyl sulfuryl sulfate ester aniline;
D, condensation
A step gained filter cake is joined in b, the c mixed in step solution, and adjustment temperature to 35 ℃ is kept pH=7～8 with 30% sodium hydroxide solution; Stirring reaction 15～20 hours; 35～40 ℃ of temperature of reaction, reaction pH=7～8 are used the aluminium base silica gel thin-layer plate endpoint detection of TLC at last; Obtain the product of structural formula (I).
5. according to arbitrary described preparation method in claim 3 or 4, this method also comprises the post-processing step of product, and this post-processing step comprises:
E, interpolation auxiliary agent
With sodium sulfate, mixed phosphate, one or more among Sodium hexametaphosphate 99, EDTA, the NNO join in the product solution of structural formula (I), stir, and are subsequent use;
F, removal insolubles
E step gained reaction solution is joined in the solid-liquid separator, separate, washery refuse is removed insolubles, collects feed liquid simultaneously in storage tank;
G, purification
With the feed liquid of collecting through membrane filtration, and with the concentration of the feed liquid percentage concentration 25% that improves the quality.One time membrane filtration waste water joins in the look liquid, continues membrane filtration.Secondary membrane filtration waste water as dyestuff at the bottom of water jacket use;
The adjustment of h, coloured light and intensity
From the reaction storage tank, extract feed liquid 200ml, dry and dyeing with disk; According to coloration result, add an amount of other batch dyestuff, carry out the coloured light adjustment, add glucose in proportion according to the UV intensity of dyestuff again and Sodium sulfate anhydrous.min(99) carries out the adjustment of intensity;
I, drying
The look liquid of h step is joined in the feed liquid preheater, adjust 210 ℃ of spray tower inlet temperatures, carry out spraying drying with 95～100 ℃ temperature outs.
6. the described dyestuff of claim 1 is in the dyeing of hydroxyl or nitrogenous fibre materials or the application in the stamp.
7. the application of dyestuff according to claim 1 in fabric fiber material, paper or plastics film being printed dyeing or stamp through ink jet printing method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102934093A CN102504588A (en) | 2011-09-29 | 2011-09-29 | Turquoise blue active dye, as well as preparation method and application thereof |
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| CN2011102934093A CN102504588A (en) | 2011-09-29 | 2011-09-29 | Turquoise blue active dye, as well as preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295437A (en) * | 2015-12-02 | 2016-02-03 | 天津德凯化工股份有限公司 | Turquoise blue dye for inkjet printing and preparation method thereof |
| CN105331143A (en) * | 2015-12-02 | 2016-02-17 | 天津德凯化工股份有限公司 | Turquoise blue dye and preparing method thereof |
| CN105482496A (en) * | 2015-12-02 | 2016-04-13 | 天津德凯化工股份有限公司 | Turquoise blue dye for inkjet printing |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106431A (en) * | 1993-10-15 | 1995-08-09 | 赫彻斯特股份公司 | Water soluble phthalocyanine without metal preparation and application of same |
| CN101418136A (en) * | 2008-11-11 | 2009-04-29 | 天津市德凯化工有限公司 | Blue reactive dyes for wool and preparation method thereof |
-
2011
- 2011-09-29 CN CN2011102934093A patent/CN102504588A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106431A (en) * | 1993-10-15 | 1995-08-09 | 赫彻斯特股份公司 | Water soluble phthalocyanine without metal preparation and application of same |
| CN101418136A (en) * | 2008-11-11 | 2009-04-29 | 天津市德凯化工有限公司 | Blue reactive dyes for wool and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 程侣柏: ""含乙烯砜活性基团中间体及染料的合成 II、合成含羟基乙基砜硫酸酯的染料及中间体"", 《大连工学院学刊》, no. 2, 31 December 1962 (1962-12-31), pages 107 - 114 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295437A (en) * | 2015-12-02 | 2016-02-03 | 天津德凯化工股份有限公司 | Turquoise blue dye for inkjet printing and preparation method thereof |
| CN105331143A (en) * | 2015-12-02 | 2016-02-17 | 天津德凯化工股份有限公司 | Turquoise blue dye and preparing method thereof |
| CN105482496A (en) * | 2015-12-02 | 2016-04-13 | 天津德凯化工股份有限公司 | Turquoise blue dye for inkjet printing |
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