CN102675916B - Nano disperse black combined dye and preparation method thereof - Google Patents
Nano disperse black combined dye and preparation method thereof Download PDFInfo
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- CN102675916B CN102675916B CN2012101352511A CN201210135251A CN102675916B CN 102675916 B CN102675916 B CN 102675916B CN 2012101352511 A CN2012101352511 A CN 2012101352511A CN 201210135251 A CN201210135251 A CN 201210135251A CN 102675916 B CN102675916 B CN 102675916B
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Abstract
The invention discloses a nano disperse black combined dye and a preparation method thereof, and relates to the field of processing in dye and intermediate industries. The combined dye comprises a dye and an aid, the mass ratio of the dye to the aid is 1: (1-4.5), and the dye is one or more of compounds shown as a formula I; the aid is formed by mixing anionic surfactant and nonionic surfactant in a mass ratio of (100-85)%: (0-15)%; in the formula I, R1 is H, Cl, Br or CN; R2 is H, Cl or NO2; R3 is H or OCH3; R4 is H or NHCOCH3; and R5 and R6 are mutually independent C2H5, C2H4OCOCH3, C2H4OCH3 or C2H4CN. Under the same dyeing condition, compared with the conventional black disperse dye for dyeing a polyester fabric, the nano disperse black combined dye has the advantages that the L value of the fabric is reduced by 21.3 percent, and the K/S value is improved by 18.6 percent.
Description
Technical field:
The present invention relates to dye well intermediate industry manufacture field, be specially the black combination of a kind of nano-dispersed dye well its preparation method.
Background technology:
Polyster fibre (polyethylene terephthalate) macromolecular chain marshalling, degree of crystallinity is also larger, and do not contain hydroxyl, amino and sodium sulfonate class water absorbability group on macromolecular chain structure, the moisture regain of fiber is only 0.4%, therefore, polyester piece good can not dye with water-soluble dye, but adopts the dispersed dye of the nonpolar structure of small molecules to complete painted in modes such as high-temperature pressure dyeing, pad-dry-cure dyeing or carrier dyeings.
Polyester piece good dyes the dispersed black dye that black is used at present, mainly to be formed by several different dispersed dye blendings according to the dyestuff color matching theory, dye particle is larger, and how between 1 μ m-2 μ m, larger grain diameter is unfavorable for the adsorption and diffusion of dyestuff in polyster fibre.From dye level,, according to the dyeing of present routine, dye to obtain the darker color of the black degree of depth, larger difficulty is still arranged, can not meet the market requirement.
, for solving the problems of the technologies described above, make the present invention.
Summary of the invention:
Based on above-mentioned requirements, a first aspect of the present invention purpose is to provide the black combination of a kind of nano-dispersed dye well its preparation method, be intended to by forming the selection of each related component kind of black dyes and ratio, by the application of high temperature resistant composite dye dispersant and the improvement of processing technology, prepare a kind of nanoscale dispersed dye that can dye the higher black degree of depth of system, further increase the black expression power that dyes the black terylene fabric product.
For achieving the above object, the technical scheme of taking is as follows:
The black combination of a kind of nano-dispersed dyestuff is characterized in that: comprise dyestuff and auxiliary agent, dyestuff is 1:1-4.5 with the mass ratio that helps, and dyestuff is one or more of compound shown in the formula I; Auxiliary agent is that anion surfactant and nonionogenic tenside mix according to mass ratio 100%-85%:0%-15%;
The formula I;
In the formula I: R
1For H, CI, Br or CN; R
2For H, CI or NO
2R
3For H or OCH
3R
4For H or NHCOCH
3R
5, R
6Be respectively separate C
2H
5, C
2H
4OCOCH
3, C
2H
4OCH
3Or C
2H
4CN.
Further arrange and be:
Described dyestuff comprises dyestuff A, dyestuff B, dyestuff C, and the mass ratio of dyestuff A, dyestuff B, dyestuff C is 87.5%-57%:12%-35%:0.5%-8%; Wherein: dyestuff A is formed by the one or more combination in the dyestuff of following structure:
A-Ⅰ；
A-Ⅱ；
A-Ⅲ；
Dyestuff B is formed by the one or more combination in the dyestuff of following structure:
B-Ⅰ；
B-Ⅱ；
B-Ⅲ；
B-Ⅳ；
B-Ⅴ；
Dyestuff C is formed by the one or more combination in the dyestuff of following structure:
C-Ⅰ；
C-Ⅱ；
C-Ⅲ；
C-Ⅳ。
Described anion surfactant is selected from one or both in sulfonated lignin, naphthalenesulfonate formaldehyde condensation compound, methyl naphthalene sulfonic acid salt formaldehyde condensation products, benzyl naphthalene sulfonic formaldehyde condensation compound and phenolic condensation compound sulfonate; Be particularly preferably one or both of sodium lignosulfonate, dispersion agent NNO, Dispersant MF, dispersing agent C NF.
Described nonionogenic tenside is selected from any one in polyoxyethylene glycol, polyoxyethylene sorbitan fatty acid ester, Soxylat A 25-7 and oxyethane polycondensate.
A second aspect of the present invention purpose is to provide the preparation method of the black combination of a kind of nano-dispersed dyestuff, it is characterized in that: dyestuff is mixed with the mass ratio of auxiliary agent according to 1:1-4.5, through sizing mixing, ultrasonic, grinding, homogeneous, spraying drying process the black combination of nano-dispersed dyestuff.
Further:
Dyestuff is mixed according to mass ratio 1:1-4.5 with auxiliary agent, add pure water to be modulated into the pulpous state premix, after this premix supersound process 20min-60min, send into the grinding of Mechanical Sealed Type ball mill and coated dispersion processing in 4-6 hour, grind and adopt circulating grinding technics, screen cloth separation system screen cloth used is 0.13mm nickel material, grinding bead is the zirconium white of 0.5mm particle diameter, the grinding bead consumption is the 200%-500% of grinding material quality, after grinding is completed, the lapping liquid high pressure homogenizing is processed, more spray-dried processing namely obtains the black combination of nano-dispersed dyestuff.
Beneficial effect of the present invention is as follows:
The black combination of nano-dispersed provided by the invention dyestuff, being conducive to terylene absorbs and can obtain more aterrimus Color, with the high-temperature pressure dyeing dyeing, compare with the conventional black disperse dye polyester piece good dyeing under same dyeing condition, having reduced 21.3%(with the black L value that makes up the polyester piece good of dyeing of nano-dispersed is that the black depth value has increased by 21.3%), the K/S value has improved 18.6%, and the polyester piece good dyeing uniformity is good, and coloured light is pure.The present invention, for exploitation nanometer particle size dispersed black dye, meets aterrimus Polyester Textiles dyeing processing and has higher realistic meaning with the demand of dyestuff.
The invention will be further described below in conjunction with embodiment.
Embodiment:
Preparation Example:
With dyestuff and auxiliary agent according to certain mass than mixing, add water and be modulated into the pulpous state premix, after this premix supersound process 20min-60min, send into the grinding of Mechanical Sealed Type ball mill and coated dispersion processing in 4-6 hour, grind and adopt circulating grinding technics, screen cloth separation system screen cloth used is 0.13mm nickel material, grinding bead is the zirconium white of 0.5mm particle diameter, the grinding bead consumption is the 200%-500% of grinding material quality, after grinding is completed, the lapping liquid high pressure homogenizing is processed, more spray-dried processing namely obtains the black combination of nano-dispersed dyestuff.
According to above-mentioned Preparation Example, adjust different dyes and auxiliary agent proportioning, obtain following embodiment:
Embodiment 1:
The component A, the 10.5g structural formula that with the 37.5g structural formula are (A-I) are component C, the 90g sodium lignosulfonate of (C-I) for B component, the 2g structural formula of (B-I), after adding water 260g mixing, make premix through stirring, afterwards according to Preparation Example, make that fastness is good, particle diameter is at the black combination of the nano-dispersed dyestuff of 15nm-100nm.
Embodiment 2-16:
According to each component concentration ratio data shown in table 1, with 50g component A, B component, component C and 90g auxiliary agent, add after water 260g mixes and make premix through agitation as appropriate, afterwards according to Preparation Example, make that fastness is good, particle diameter is at the black combination of the commercialization nano-dispersed dyestuff of 15nm-100nm.
Each component of table 1, embodiment 2-16 combination dyestuff forms.
Embodiment 17:
With the 34g structural formula for the component A of (A-I), 13g structural formula for the B component of (B-I), 3g structural formula for the mixture of the component C of (C-I), 90g sodium lignosulfonate and dispersion agent NNO, add water 260g and mix and make premix by stirring, afterwards according to Preparation Example, make that fastness is good, particle diameter is at the black combination of the nano-dispersed dyestuff of 15nm-100nm.
Performance Detection:
The black combination of nano-dispersed dyestuff with embodiment 1-17 preparation, dye according to following dyeing:
Dyeing flow process: polyester piece good → concise pre-treatment → dehydration → oven dry → pre-setting → dyeing → washing → reduction clearing → washing → oven dry.
Dyeing prescription:
The black combination of nano-dispersed dyestuff: 3.5%(owf, with respect to the quality of polyester piece good);
Acetic acid: 0.5g/l, the adjusting dye liquor pH value is 4.5-5.0;
Bath raio: 30:1;
Dyeing temperature: 130 ℃;
Dyeing time: 60min.
The dyeing aftertreatment: after dyeing polyester piece good first through washing, then use 1.0g/l concentration reduction clearing liquid at 80 ℃ of lower carrying out washing treatment 10 min, wash afterwards, dry.
The polyester piece good of with the nano-dispersed of the present invention's preparation, deceiving after tested, the combination dyeing: fastness to wet rubbing is 5 grades, and dry fastness is 5 grades, and soaping fastness is the 4-5 level, and the variable color fastness of soaping is the 4-5 level.Compare through the conventional black disperse dye polyester piece good dyeing with under same dyeing condition: it is that the black degree of depth has increased by 21.3% that the L value of fabric has reduced 21.3%(), the K/S value has improved 18.6%, and the polyester piece good dyeing uniformity is good, and coloured light is pure.
Claims (2)
1. a nano-dispersed is deceived the combination dyestuff, it is characterized in that: comprise dyestuff and auxiliary agent, the mass ratio of dyestuff and auxiliary agent is 1:1-4.5, and described dyestuff comprises dyestuff A, dyestuff B, dyestuff C, and the mass ratio of dyestuff A, dyestuff B, dyestuff C is 87.5%-57%:12%-35%:0.5%-8%; Described auxiliary agent is that anion surfactant and nonionogenic tenside mix according to mass ratio 100%-85%:0%-15%;
Wherein: dyestuff A is formed by the one or more combination in the dyestuff of following structure:
A-Ⅰ；
A-Ⅱ；
A-Ⅲ；
Dyestuff B is formed by the one or more combination in the dyestuff of following structure:
B-Ⅰ；
B-Ⅱ；
B-Ⅲ；
B-Ⅳ；
B-Ⅴ；
Dyestuff C is formed by the one or more combination in the dyestuff of following structure:
C-Ⅰ；
C-Ⅱ；
C-Ⅲ；
C-Ⅳ。
2. a kind of nano-dispersed according to claim 1 is deceived the combination dyestuff, and it is characterized in that: described anion surfactant is selected from one or both in sulfonated lignin, naphthalenesulfonate formaldehyde condensation compound, methyl naphthalene sulfonic acid salt formaldehyde condensation products, benzyl naphthalene sulfonic formaldehyde condensation compound and phenolic condensation compound sulfonate.
3, the black combination of a kind of nano-dispersed according to claim 2 dyestuff is characterized in that: described anion surfactant is selected from one or both of sodium lignosulfonate, dispersion agent NNO, Dispersant MF, dispersing agent C NF.
4, the black combination of a kind of nano-dispersed according to claim 1 dyestuff, it is characterized in that: described nonionogenic tenside is selected from any one in polyoxyethylene glycol, polyoxyethylene sorbitan fatty acid ester, Soxylat A 25-7 and oxyethane polycondensate.
5, the preparation method of the black combination of the described nano-dispersed of claim 1-4 any one dyestuff, it is characterized in that: dyestuff is mixed with the mass ratio of auxiliary agent according to 1:1-4.5, through sizing mixing, ultrasonic, grinding, homogeneous, spraying drying process the black combination of nano-dispersed dyestuff.
6, according to claim 5, nano-dispersed is deceived the preparation method of combination dyestuff, it is characterized in that: dyestuff is mixed according to mass ratio 1:1-4.5 with auxiliary agent, add pure water to be modulated into the pulpous state premix, after this premix supersound process 20min-60min, send into the grinding of Mechanical Sealed Type ball mill and coated dispersion processing in 4-6 hour, grind and adopt circulating grinding technics, screen cloth separation system screen cloth used is 0.13mm nickel material, grinding bead is the zirconium white of 0.5mm particle diameter, the grinding bead consumption is the 200%-500% of grinding material quality, after grinding is completed, the lapping liquid high pressure homogenizing is processed, spray-dried processing namely obtains the black combination of nano-dispersed dyestuff again.
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| CN2012101352511A CN102675916B (en) | 2012-05-04 | 2012-05-04 | Nano disperse black combined dye and preparation method thereof |
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| CN2012101352511A CN102675916B (en) | 2012-05-04 | 2012-05-04 | Nano disperse black combined dye and preparation method thereof |
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| CN102675916B true CN102675916B (en) | 2013-11-20 |
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| CN103937291B (en) * | 2014-04-02 | 2016-07-27 | 上海贝通色彩科技有限公司 | A kind of stamp Disperse black azo dye mixture and preparation method thereof |
| CN103965651B (en) * | 2014-05-23 | 2016-04-20 | 约克夏染料（中山）有限公司 | A kind of high washing fastness admixture of disperse dyes and application thereof |
| CN104151864A (en) * | 2014-08-27 | 2014-11-19 | 广东省均安牛仔服装研究院 | Preparation method of nano-scale indigo dye suspended matter |
| CN105113285B (en) * | 2015-09-19 | 2018-01-05 | 苏州大学 | A kind of pulp-shaped dispersed dyes and preparation method and application |
| CN105524487A (en) * | 2015-12-03 | 2016-04-27 | 太湖亚太精化有限公司 | Disperse dye composition and disperse dye and preparation method and application thereof |
| CN113831759A (en) * | 2021-09-16 | 2021-12-24 | 浙江理工大学 | Liquid disperse dye for high-temperature dip dyeing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0244337B2 (en) * | 1983-07-22 | 1990-10-03 | Mitsui Toatsu Chemicals | MIZUFUYOSEIBUNSANSENRYOSOSEIBUTSU OYOBIKOREOMOCHIITAHORIESUTERUSENINOSENSHOKUMATAHANATSUSENHO |
| GB8805690D0 (en) * | 1988-03-10 | 1988-04-07 | Ici Plc | Disperse dyes |
| EP0661352A1 (en) * | 1993-12-21 | 1995-07-05 | DyStar Japan Ltd. | Method for dyeing hydrophobic fibers black and dye useful for the method |
| DE19636380A1 (en) * | 1996-09-09 | 1998-03-12 | Dystar Textilfarben Gmbh & Co | Disperse dye mixtures |
| CN100503740C (en) * | 2007-01-05 | 2009-06-24 | 浙江龙盛染料化工有限公司 | Dispersed black dye composition |
| CN102002259B (en) * | 2010-11-04 | 2013-12-25 | 浙江闰土股份有限公司 | High-fastness black and blue disperse dye composite |
| CN102653635A (en) * | 2012-03-15 | 2012-09-05 | 江苏之江化工有限公司 | Printing black disperse dyes |
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