CN104371368A - Superfine reduction liquid dye, preparation method thereof and application thereof in printing of cellulosic fiber - Google Patents
Superfine reduction liquid dye, preparation method thereof and application thereof in printing of cellulosic fiber Download PDFInfo
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- CN104371368A CN104371368A CN201410647135.7A CN201410647135A CN104371368A CN 104371368 A CN104371368 A CN 104371368A CN 201410647135 A CN201410647135 A CN 201410647135A CN 104371368 A CN104371368 A CN 104371368A
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Abstract
The invention relates to a superfine reduction liquid dye, preparation method thereof and application thereof in printing of cellulosic fiber, belonging to the technical field of textile chemical industry. The superfine reduction liquid dye is characterized by being prepared by carrying out refined grinding on a reduced dye filter cake by virtue of a grinding machine. A production process is simple and is convenient to operate, the particle size of the prepared superfine reduction liquid dye is 100nm-300nm, the centrifugation deposition rate is only 3%-8%, and the storage stability is good; the superfine reduction liquid dye can be applied to the printing of the cellulosic fiber, the dust pollution in pulping and material-conversion procedures can be effectively avoided, and the material-conversion efficiency is improved; meanwhile, compared with powdery dyes, the superfine reduction liquid dye has the advantages that the printing promotion of the superfine-reduction liquid dye is better, and the color yield can be increased by 5%-16%.
Description
Technical field
The present invention relates to the aqueous dye well preparation method of a kind of ultra-fine reduction and the application at cellulosic fibre stamp, belong to technical field of textile chemical engineering.
Background technology
Because vat dyes is water insoluble, current commercialization vat dyes is generally superfine powdery vat dyes.In the commercialization course of processing of powdery vat dyes, Wet ultrafine grinding is one of important course of processing.The technique that current domestic vat dyes crushing process generally adopts be pasty material pre-dispersed-sanding-pan-sand mill-clarifixator technical process, grinding time is long, and Grin-ding energ7 is large.
In addition, powder dye can produce dust pollution in stamp making beating material process, and easily occurs that workshop material is uneven or not exclusively, causes the stamp cloth specimen shade even color dot etc. that differs abnormal.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of ultra-fine reduction liquid dyes is provided, avoid producing dust pollution in stamp making beating material process, reduce material inequality or incomplete situation.
Another object of the present invention is, provides a kind of preparation method of ultra-fine reduction liquid dyes, shortens the process time, raises the efficiency, and reduces energy consumption.
Another object of the present invention, there is provided a kind of ultra-fine reduction liquid dyes in the application of cellulosic fibre stamp, it is more complete that ultra-fine reduction liquid dyes evaporates color development in process at stamp, and in Final finishing is soaped, loose colour is less, favourable fastness and environmental protection, make printing quality better.
According to technical scheme provided by the invention, described ultra-fine reduction liquid dyes, it is characterized in that, comprise following component, component ratio by mass number meter: vat dyes filter cake 10 ~ 30 parts, dispersion agent 10 ~ 20 parts, wetting agent 5 ~ 30 parts, pH value regulator 0.1 ~ 0.5 part, defoamer 0.1 ~ 0.5 part and 19 ~ 74.8 parts, water.
In an embodiment, described dispersion agent is one or more in sulfonated alkyl naphathalene, sulfonated alkyl naphathalene formaldehyde condensation products, sulfonated lignin, polyacrylic acid, sodium polyacrylate.
In an embodiment, described wetting agent is one or more in ethanol, ethylene glycol, n-propyl alcohol, Pentyl alcohol, propylene glycol, glycerol, glycol ether, urea.
In an embodiment, described pH value regulator is one or more in Monoethanolamine MEA BASF, diethanolamine, trolamine, ammoniacal liquor.
In an embodiment, described defoamer is one or more in DOW CORNING defoamer AFE-3168, DOW CORNING defoamer AFE-0050, DOW CORNING defoamer AFE-0700, DOW CORNING defoamer AFE-0800, development of evil in febrile disease defoamer TF-509.
The preparation method of described ultra-fine reduction liquid dyes, is characterized in that, adopt following processing step, component ratio by mass number meter:
(1) by 10 ~ 30 parts of vat dyes filter cakes, 10 ~ 20 parts of dispersion agents, 5 ~ 30 parts of wetting agents, 0.1 ~ 0.5 part of pH value regulator, 0.1 ~ 0.5 part of defoamer and 19 ~ 74.8 parts of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 20 ~ 30min of mulser, rotating speed is 500 ~ 2000 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 5 ~ 20 hours, rotating speed is 1000 ~ 3000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains described ultra-fine reduction liquid dyes.
The present invention also provides the application of a kind of ultra-fine reduction liquid dyes stamp on cotton fibre, flaxen fiber, viscose fiber, copper ammonia fibre, cellulose acetate fibre, sky silk or modalic fiber.
Ultra-fine reduction liquid dyes of the present invention, for the stamp of cellulosic fibre, can avoid dust pollution in stamp process, and improve the efficiency of making beating material operation, the dye utilization rate of PRINTED FABRIC is good, can increase 5-16% compared to powder dye dye yield.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
The vat dyes filter cake used in the present invention refers to without retrofits such as dispersion, grindings, also not comprise the auxiliary agents such as dispersion agent, namely pure dyestuff by the product that vat dyes intermediate obtains through chemosynthesis operation.
Testing method of the present invention, specific as follows:
(1) particle diameter and Zeta potential test: by the aqueous dye-dilution of ultra-fine reduction 2000 times prepared, adopts Britain's MALVERN company Nano-ZS 90 type nano particle size and Zeta potential analyser to measure particle diameter and Zeta potential.
(2) test of liquid dyes centrifugation rate: the ultra-fine reduction liquid dyes taking 100g, put into the centrifuge tube of 100mL, adopt supercentrifuge to be under the condition of 1500rpm at rotating speed, after centrifugal 60min, pour out the unprecipitated dye liquid in upper strata and weigh and be designated as M1.Each sample test 3 times, gets its mean value.Centrifugation rate/%=(100-M1)/100.
Embodiment one: a kind of preparation method of ultra-fine reduction liquid dyes, adopts following processing step, component ratio by mass number meter:
(1) by 23 parts of vat yellow dyestuff filter-cakes, 10 parts of dispersing agent C NF, 6 parts of dispersion agent M-9,13 parts of glycerol, 4 parts of ethylene glycol, 0.2 part of trolamine, 0.2 part of defoamer TF-509 and 43.6 part of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 30min of mulser, rotating speed is 1500 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 8 hours, rotating speed is 2000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains described ultra-fine vat yellow liquid dyes.
The ultra-fine vat yellow liquid dyes particle diameter that embodiment one prepares is 145nm, and Zeta potential is-44.5mV, and centrifugation rate is 3.4%, and stability in storage is good.When stamp concentration is 4.0%, compared to powder dye, the dye yield of ultra-fine vat yellow liquid dyes stamp on cotton fibre Woven Fabrics improves 15.2%.
Embodiment two: a kind of preparation method of ultra-fine reduction liquid dyes, adopts following processing step, component ratio by mass number meter:
(1) 25 parts of 3b vat red 3b dyestuff filter-cakes, 10 parts of Dispersant MFs, 7 parts of dispersion agent REAX are measured 83A, 15 portions of glycol ethers, 3 parts of urea, 0.3 part of trolamine, 0.2 part of defoamer TF-509 and 39.5 part of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 30min of mulser, rotating speed is 1500 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 12 hours, rotating speed is 2000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains described ultra-fine 3b vat red 3b liquid dyes.
The ultra-fine 3b vat red 3b liquid dyes particle diameter that embodiment two prepares is 161.7nm, and Zeta potential is-41.2mV, and centrifugation rate is 3.5%, and stability in storage is good.When stamp concentration is 4.0%, compared to powder dye, the dye yield of ultra-fine 3b vat red 3b liquid dyes stamp on viscose fiber Woven Fabrics improves 13.4%.
Embodiment three: a kind of preparation method of ultra-fine reduction liquid dyes, adopts following processing step, component ratio by mass number meter:
(1) by 13 parts of reduction purple dye filter cakes, 6 parts of dispersion agent NNO, 4 parts of dispersion agent REAX 85A, 10 parts of glycerol, 5 portions of glycol ethers, 5 parts of urea, 0.4 part of trolamine, 0.2 part of defoamer TF-509 and 56.4 part of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 30min of mulser, rotating speed is 1500 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 10 hours, rotating speed is 2000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains the described purple liquid dyes of ultra-fine reduction.
The purple liquid dyes particle diameter of the ultra-fine reduction that embodiment three prepares is 185.3nm, and Zeta potential is-40.8mV, and centrifugation rate is 4.2%, and stability in storage is good.When stamp concentration is 4.0%, compared to powder dye, the dye yield of the purple liquid dyes of ultra-fine reduction stamp on cotton Woven Fabrics improves 10.5%.
Embodiment four: a kind of preparation method of ultra-fine reduction liquid dyes, adopts following processing step, component ratio by mass number meter:
(1) by 25 parts of vat blue dyestuff filter-cakes, 7 parts of Dispersant MFs, 7 parts of dispersion agent REAX 85A, 12 parts of glycerol, 5 parts of urea, 0.3 part of trolamine, 0.4 part of defoamer TF-509 and 43.3 part of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 30min of mulser, rotating speed is 1500 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 15 hours, rotating speed is 1500 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains described ultra-fine vat blue liquid dyes.
The ultra-fine vat blue liquid dyes particle diameter that embodiment four prepares is 194.6nm, and Zeta potential is-36.9mV, and centrifugation rate is 6.7%, and stability in storage is good.When stamp concentration is 4.0%, compared to powder dye, the dye yield of ultra-fine vat blue liquid dyes stamp on cotton Woven Fabrics improves 7.8%.
Embodiment five: a kind of preparation method of ultra-fine reduction liquid dyes, adopts following processing step, component ratio by mass number meter:
(1) by 27 parts of reduction dark blue dye filter cakes, 7 parts of dispersing agent C NF, 10 parts of dispersion agent REAX 81A, 10 portions of glycol ethers, 6 parts of glycerine, 0.2 part of trolamine, 0.3 part of defoamer TF-509 and 39.5 part of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 30min of mulser, rotating speed is 1500 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 15 hours, rotating speed is 2000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains the described dark blue liquid dyes of ultra-fine reduction.
The dark blue liquid dyes particle diameter of the ultra-fine reduction that embodiment five prepares is 243.6nm, and Zeta potential is-42.5mV, and centrifugation rate is 4.9%, and stability in storage is good.When stamp concentration is 4.0%, compared to powder dye, the dye yield of the dark blue liquid dyes of ultra-fine reduction stamp on Modal Woven Fabrics improves 8.9%.
Embodiment six: a kind of preparation method of ultra-fine reduction liquid dyes, adopts following processing step, component ratio by mass number meter:
(1) by 30 parts of B150reactive Black B 150 dyestuff filter-cakes, 8 parts of dispersion agent NNO, 10 parts of dispersion agent M-13,12 portions of glycol ethers, 5 parts of ethylene glycol, 0.3 part of trolamine, 0.4 part of defoamer TF-509 and 34.3 part of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 30min of mulser, rotating speed is 2000 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 18 hours, rotating speed is 3000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains described ultra-fine B150reactive Black B 150 liquid dyes.
The ultra-fine B150reactive Black B 150 liquid dyes particle diameter that embodiment six prepares is 220.9nm, and Zeta potential is-51.6mV, and centrifugation rate is 7.8%, and stability in storage is good.When stamp concentration is 6.0%, compared to powder dye, the dye yield of ultra-fine B150reactive Black B 150 liquid dyes stamp on cotton Woven Fabrics improves 5.6%.
Claims (7)
1. a ultra-fine reduction liquid dyes, it is characterized in that, comprise following component, component ratio by mass number meter: vat dyes filter cake 10 ~ 30 parts, dispersion agent 10 ~ 20 parts, wetting agent 5 ~ 30 parts, pH value regulator 0.1 ~ 0.5 part, defoamer 0.1 ~ 0.5 part and 19 ~ 74.8 parts, water.
2. ultra-fine reduction liquid dyes as claimed in claim 1, is characterized in that: described dispersion agent is one or more in sulfonated alkyl naphathalene, sulfonated alkyl naphathalene formaldehyde condensation products, sulfonated lignin, polyacrylic acid, sodium polyacrylate.
3. ultra-fine reduction liquid dyes as claimed in claim 1, is characterized in that: described wetting agent is one or more in ethanol, ethylene glycol, n-propyl alcohol, Pentyl alcohol, propylene glycol, glycerol, glycol ether, urea.
4. ultra-fine reduction liquid dyes as claimed in claim 1, is characterized in that: described pH value regulator is one or more in Monoethanolamine MEA BASF, diethanolamine, trolamine, ammoniacal liquor.
5. ultra-fine reduction liquid dyes as claimed in claim 1, is characterized in that: described defoamer is one or more in DOW CORNING defoamer AFE-3168, DOW CORNING defoamer AFE-0050, DOW CORNING defoamer AFE-0700, DOW CORNING defoamer AFE-0800, development of evil in febrile disease defoamer TF-509.
6. a preparation method for ultra-fine reduction liquid dyes, is characterized in that, adopts following processing step, component ratio by mass number meter:
(1) by 10 ~ 30 parts of vat dyes filter cakes, 10 ~ 20 parts of dispersion agents, 5 ~ 30 parts of wetting agents, 0.1 ~ 0.5 part of pH value regulator, 0.1 ~ 0.5 part of defoamer and 19 ~ 74.8 parts of water mixing;
(2) mixture that step (1) obtains at room temperature is adopted the pre-dispersed 20 ~ 30min of mulser, rotating speed is 500 ~ 2000 revs/min;
(3) transferred to by the mixture after step (2) is pre-dispersed in sand mill and grind 5 ~ 20 hours, rotating speed is 1000 ~ 3000 revs/min, then precision is the PP filter bag filtration of 3 μm after filtration, namely obtains described ultra-fine reduction liquid dyes.
7. the application of ultra-fine reduction liquid dyes stamp on cotton fibre, flaxen fiber, viscose fiber, copper ammonia fibre, cellulose acetate fibre, sky silk or modalic fiber.
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| CN201410647135.7A CN104371368B (en) | 2014-11-14 | 2014-11-14 | Ultra-fine reduction liquid dyes and preparation method and in the application of cellulose fibre stamp |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317949A (en) * | 2016-07-26 | 2017-01-11 | 萧县凯奇化工科技有限公司 | Preparation method for ultra-fine revivification dyeing material |
| CN115594990A (en) * | 2022-09-08 | 2023-01-13 | 浙江亿得新材料股份有限公司（Cn） | Preparation method and application of energy-saving emission-reducing high-strength liquid vat dye composition |
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| US5922087A (en) * | 1995-04-20 | 1999-07-13 | Clariant Finance (Bvi) Limited | Stable liquid suspensions and method for analyzing same |
| CN102093755A (en) * | 2010-12-07 | 2011-06-15 | 江南大学 | Preparation method of superfine indigotin dye suspension |
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Patent Citations (3)
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| CN1058625A (en) * | 1990-08-01 | 1992-02-12 | B·F·福勒 | The method of carpet dyeing and device |
| US5922087A (en) * | 1995-04-20 | 1999-07-13 | Clariant Finance (Bvi) Limited | Stable liquid suspensions and method for analyzing same |
| CN102093755A (en) * | 2010-12-07 | 2011-06-15 | 江南大学 | Preparation method of superfine indigotin dye suspension |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317949A (en) * | 2016-07-26 | 2017-01-11 | 萧县凯奇化工科技有限公司 | Preparation method for ultra-fine revivification dyeing material |
| CN115594990A (en) * | 2022-09-08 | 2023-01-13 | 浙江亿得新材料股份有限公司（Cn） | Preparation method and application of energy-saving emission-reducing high-strength liquid vat dye composition |
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| CN104371368B (en) | 2016-06-29 |
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