CN102675916A - Nano disperse black combined dye and preparation method thereof - Google Patents

Nano disperse black combined dye and preparation method thereof Download PDF

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CN102675916A
CN102675916A CN2012101352511A CN201210135251A CN102675916A CN 102675916 A CN102675916 A CN 102675916A CN 2012101352511 A CN2012101352511 A CN 2012101352511A CN 201210135251 A CN201210135251 A CN 201210135251A CN 102675916 A CN102675916 A CN 102675916A
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dyestuff
nano
dispersed
combination
dye
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CN102675916B (en
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刘越
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University of Shaoxing
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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

The black combination of a kind of nano-dispersed dye well its preparation method
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; Percent crystallinity is also bigger; And not containing hydroxyl, amino and sodium sulfonate class water absorbability group on the macromolecular chain structure, the moisture regain of fiber is merely 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 accomplish painted with 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 be to piece together to mix by several kinds of different dispersed dye according to the dyestuff color matching theory to form; Dye particle is bigger, and how between 1 μ m-2 μ m, bigger grain diameter is unfavorable for the adsorption and diffusion of dyestuff in polyster fibre.See from dye level, according to the dyeing of present routine, dye the darker color of the black degree of depth, big difficulty is still arranged, satisfied not 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; First aspect purpose of the present invention provides the black combination of a kind of nano-dispersed dye well its preparation method; Be intended to through constituting the selection of each related component kind of black dyes and ratio; Through the application of high temperature resistant compound 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 realizing above-mentioned purpose, the technical scheme of being taked is following:
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 AS and nonionogenic tenside mix according to mass ratio 100%-85%:0%-15%;
Figure 2012101352511100002DEST_PATH_IMAGE001
The formula I;
In the formula I: R 1Be H, CI, Br or CN; R 2Be H, CI or NO 2R 3Be H or OCH 3R 4Be H or NHCOCH 3R 5, R 6Be respectively separate C 2H 5, C 2H 4OCOCH 3, C 2H 4OCH 3Or C 2H 4CN.
Further be provided with and be:
Said 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:
Figure 442196DEST_PATH_IMAGE002
A-Ⅰ；
Figure 2012101352511100002DEST_PATH_IMAGE003
A-Ⅱ；
A-Ⅲ；
Dyestuff B is formed by the one or more combination in the dyestuff of following structure:
Figure 2012101352511100002DEST_PATH_IMAGE005
B-Ⅰ；
Figure 328954DEST_PATH_IMAGE006
B-Ⅱ；
Figure 2012101352511100002DEST_PATH_IMAGE007
B-Ⅲ；
Figure 661846DEST_PATH_IMAGE008
B-Ⅳ；
Figure 2012101352511100002DEST_PATH_IMAGE009
B-Ⅴ；
Dyestuff C is formed by the one or more combination in the dyestuff of following structure:
Figure 476219DEST_PATH_IMAGE010
C-Ⅰ；
C-Ⅱ；
Figure 485632DEST_PATH_IMAGE012
C-Ⅲ；
Figure 2012101352511100002DEST_PATH_IMAGE013
C-Ⅳ。
Described AS 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 the phenolic condensation compound sulphonate; Be preferably one or both of sodium lignosulfonate, dispersion agent NNO, Dispersant MF, dispersing agent C NF especially.
Described nonionogenic tenside is selected from any one in polyoxyethylene glycol, polyoxyethylene sorbitan fatty ester, Soxylat A 25-7 and the oxyethane polycondensate.
Second aspect purpose of the present invention provides 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 size 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 and be modulated into the pulpous state premix, behind 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, the used screen cloth of screen cloth separation system is a 0.13mm nickel material, and 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 completion, the lapping liquid high pressure homogenizing is handled, spray-dried again processing promptly gets the black combination of nano-dispersed dyestuff.
Beneficial effect of the present invention is following:
The black combination of nano-dispersed provided by the invention dyestuff; Help the terylene absorption and can obtain more aterrimus Color,, compare with the conventional black disperse dye polyester piece good dyeing under the same dyeing condition with the dyeing of high-temperature pressure dyeing technology; Reduced by 21.3% (being that the black depth value has increased by 21.3%) with the black L value that makes up the polyester piece good of dyeing of nano-dispersed; 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 is for exploitation nanometer particle size dispersed black dye, satisfies aterrimus terylene textile dyeing processing and has higher realistic meaning with the demand of dyestuff.
Below in conjunction with embodiment the present invention is described further.
Embodiment:
Preparation embodiment:
With dyestuff and auxiliary agent according to certain mass than mixing, add water and be modulated into the pulpous state premix, behind 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, the used screen cloth of screen cloth separation system is a 0.13mm nickel material, and 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 completion, the lapping liquid high pressure homogenizing is handled, spray-dried again processing promptly gets the black combination of nano-dispersed dyestuff.
Based on above-mentioned preparation embodiment, adjustment different dyes and auxiliary agent proportioning get following embodiment:
Embodiment 1:
With the 37.5g structural formula is that the component A of (A-I), B component, the 2g structural formula that the 10.5g structural formula is (B-I) are component C, the 90g sodium lignosulfonate of (C-I); After adding water 260g mixing; Process premix through stirring; Afterwards according to preparation embodiment, 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 the table 1; With 50g component A, B component, component C and 90g auxiliary agent; Add and process premix through agitation as appropriate after water 260g mixes; Afterwards according to preparation embodiment, 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 constitutes.
Figure 2012101352511100002DEST_PATH_IMAGE015
。
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 after stir and process premix; Afterwards according to preparation embodiment, 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 is 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: dyeing back polyester piece good is earlier through washing, use again 1.0g/l concentration reduction clearing liquid at 80 ℃ of following carrying out washing treatment 10 min, wash afterwards, dry.
Through test, deceive the polyester piece good of combination dyeing with the nano-dispersed of the present invention's preparation: fastness to wet rubbing is 5 grades, and dry fastness is 5 grades, and the staining fastness of soaping is the 4-5 level, and the variable color fastness of soaping is the 4-5 level.Warp is compared with the conventional black disperse dye polyester piece good dyeing under the same dyeing condition: the L value of fabric has reduced by 21.3% (being that the black degree of depth has increased by 21.3%), and the K/S value has improved 18.6%, and the polyester piece good dyeing uniformity is good, and coloured light is pure.

Claims (7)

1. a nano-dispersed is deceived the combination dyestuff, it 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 AS and nonionogenic tenside mix according to mass ratio 100%-85%:0%-15%;
The formula I;
In the formula I: R 1Be H, CI, Br or CN; R 2Be H, CI or NO 2R 3Be H or OCH 3R 4Be H or NHCOCH 3R 5, R 6Be respectively separate C 2H 5, C 2H 4OCOCH 3, C 2H 4OCH 3Or C 2H 4CN.
2. the black combination of a kind of nano-dispersed according to claim 1 dyestuff, it is characterized in that: said dyestuff comprises dyestuff A, dyestuff B, dyestuff C, 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:
Figure 2012101352511100001DEST_PATH_IMAGE004
A-Ⅰ；
Figure 2012101352511100001DEST_PATH_IMAGE006
A-Ⅱ；
Figure 2012101352511100001DEST_PATH_IMAGE008
A-Ⅲ；
Dyestuff B is formed by the one or more combination in the dyestuff of following structure:
Figure 2012101352511100001DEST_PATH_IMAGE010
B-Ⅰ；
Figure 2012101352511100001DEST_PATH_IMAGE012
B-Ⅱ；
Figure 2012101352511100001DEST_PATH_IMAGE014
B-Ⅲ；
Figure 2012101352511100001DEST_PATH_IMAGE016
B-Ⅳ；
Figure 2012101352511100001DEST_PATH_IMAGE018
B-Ⅴ；
Dyestuff C is formed by the one or more combination in the dyestuff of following structure:
Figure 2012101352511100001DEST_PATH_IMAGE020
C-Ⅰ；
Figure 2012101352511100001DEST_PATH_IMAGE022
C-Ⅱ；
Figure 2012101352511100001DEST_PATH_IMAGE024
C-Ⅲ；
Figure 2012101352511100001DEST_PATH_IMAGE026
C-Ⅳ。
3. the black combination of a kind of nano-dispersed according to claim 1 and 2 dyestuff, it is characterized in that: described AS 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 the phenolic condensation compound sulphonate.
4. the black combination of a kind of nano-dispersed according to claim 3 dyestuff is characterized in that: described AS is selected from one or both of sodium lignosulfonate, dispersion agent NNO, Dispersant MF, dispersing agent C NF.
5. the black combination of a kind of nano-dispersed according to claim 1 and 2 dyestuff, it is characterized in that: described nonionogenic tenside is selected from any one in polyoxyethylene glycol, polyoxyethylene sorbitan fatty ester, Soxylat A 25-7 and the oxyethane polycondensate.
6. each said nano-dispersed of claim 1-5 is deceived the preparation method of combination dyestuff; It is characterized in that: dyestuff is mixed with the mass ratio of auxiliary agent according to 1:1-4.5, through size mixing, ultrasonic, grinding, homogeneous, spraying drying process the black combination of nano-dispersed dyestuff.
7. according to the preparation method of the black combination of the said nano-dispersed of claim 6 dyestuff, it is characterized in that: dyestuff is mixed according to mass ratio 1:1-4.5 with auxiliary agent, add pure water and be modulated into the pulpous state premix; Behind 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; The used screen cloth of screen cloth separation system is a 0.13mm nickel material; Grinding bead is the zirconium white of 0.5mm particle diameter, and the grinding bead consumption is the 200%-500% of grinding material quality, after grinding is accomplished; The lapping liquid high pressure homogenizing is handled, and spray-dried again processing promptly gets the black combination of nano-dispersed dyestuff.
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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN103937291A (en) * 2014-04-02 2014-07-23 上海贝通色彩科技有限公司 Printing disperse black azo dye mixture and preparation method thereof
CN103965651A (en) * 2014-05-23 2014-08-06 约克夏染料（中山）有限公司 High-washing-fastness disperse dye mixture 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
CN105113285A (en) * 2015-09-19 2015-12-02 苏州大学 Slurry disperse dye and preparation method and appliance
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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CN100999619A (en) * 2007-01-05 2007-07-18 浙江龙盛染料化工有限公司 Disperse black dye composition
CN102002259A (en) * 2010-11-04 2011-04-06 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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US4916769A (en) * 1988-03-10 1990-04-17 Imperial Chemical Industries Plc Disperse mono-azo dye mixture for dyeing synthetic textiles
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103937291A (en) * 2014-04-02 2014-07-23 上海贝通色彩科技有限公司 Printing disperse black azo dye mixture and preparation method thereof
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
CN103965651A (en) * 2014-05-23 2014-08-06 约克夏染料（中山）有限公司 High-washing-fastness disperse dye mixture and application 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
CN105113285A (en) * 2015-09-19 2015-12-02 苏州大学 Slurry disperse dye and preparation method and appliance
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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