CN100366683C - Process for preparing nano disperse blue 2BLN dye by reprecipitation-homogenization method - Google Patents
Process for preparing nano disperse blue 2BLN dye by reprecipitation-homogenization method Download PDFInfo
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- CN100366683C CN100366683C CNB2006100499689A CN200610049968A CN100366683C CN 100366683 C CN100366683 C CN 100366683C CN B2006100499689 A CNB2006100499689 A CN B2006100499689A CN 200610049968 A CN200610049968 A CN 200610049968A CN 100366683 C CN100366683 C CN 100366683C
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Abstract
The present invention discloses a nanometer dispersion blue 2BLN dye preparing technology through a re-precipitation and homogenizing method. The present invention comprises the steps that ball milling is carried out on filtering cakes of on dispersion blue 2BLN dyes, solvents and dispersing agents so as to obtain an emulsion; the emulsion is slowly added to a water solution of the dispersing agents drop by drop, wherein the dispersing agents realize strong ball milling in a ball milling medium; after strong ball milling, a dispersion dye solution is homogenized at a high pressure so as to obtain nanometer dispersion blue 2BLN liquid dyes. The average particle size of the dye solution of the present invention relates to 70 nm, D90 is smaller than 100 nm, and the stability performance does not change after the placement of 2 months at a room temperature. Compared with a micro-emulsion method, a laser irradiation method, etc., the process of the present invention has the characteristics of stable nanometer quality of the product, short technological flow, simple operation, low equipment requirement, easy industrialization, etc.
Description
Technical field
The present invention relates to a kind of preparation technology of dispersed dye, especially relate to a kind of preparation technology of nano level DISPERSE BLUE 2BLN dyestuff.
Background technology
The size and the distribution thereof of dye particles have very big influence to dyeing behavior.Especially along with the continuous development of terylene printing technology and the appearance of superfine Denier fibre, more and more higher to the particle diameter requirement of dispersed dye.At present, dispersed dye mainly lean on ball milling or sand milling technology to the processing of particle diameter.The dispersed dye of tradition grinding technics production have that particle diameter is big, the distribution range of particle diameter is wide, particle shape is irregular, sphere are arranged, rhombus, aciculiform and cylindrical, feature such as crystal formation is unclear, so exist big gap at aspects such as dispersiveness, high temperature dispersion stabilization and dye uptakes, rate of loss up to 50%, has had a strong impact on the application performance of product 10～30%, when serious generally speaking.
The research of nano-dispersed dyestuff is to utilize nanotechnology to transform the basis of dispersed dye product structure and traditional dyeing and finishing industry, is one of new focus of dyestuff chemistry industry member research both at home and abroad in recent years.The particle diameter and the tinctorial strength of nano-dispersed dyestuff are inversely proportional to, when particle diameter more hour, its tinctorial strength can increase.The nano-dispersed dyestuff is by dying on the non-film forming adhesion mechanism, and the bounding force of its particle is strong, need not film forming and promotes colour fastness.Therefore when printing and dyeing, can reduce bath raio, avoid producing large amount of sewage.Simultaneously the nano-dispersed dyestuff also has and is easy to use and is convenient to characteristics such as storage.
The Xiao Song technology company of Japan in 2003 adopts the mixed technology exploitation ultrafine nanometer dispersed dye of nanofabrication technique and dispersion agent, and median size is less than 100nm.The said firm plans blue, red and xanchromatic dispersed dye are carried out research of technique, wish to obtain each stratographic thin many dispersion dyestuffs, thereby the raising productive rate improves quality product and cuts down the consumption of energy.
Domestic Jilin Ke Yang Nanosolutions GmbH etc. has carried out the research of applying nano emulsion polymerization technology synthetic " nano ecological dyestuff ".Shanghai NaNuoWei new material Science Co., Ltd has developed superfine pigment China ink " NNW water-based paint China ink ", and has formed the scale production ability.The international difficult problem that the exploitation of nano-scale water pigment inks has broken through is high-quality, low-cost, mass-producing is made.
Nano-dispersed dyestuff technology of preparing belongs to the technology of preparing of organic molecule nano material, and this Study on Technology still is in the technical foundation conceptual phase at present, and the emphasis of research is aspect the commercialization processing technology two of the nanofabrication technique of physical action and dyestuff.The technology of preparing of organic molecule nano material has redeposition technology, microemulsion technology and laser radiation technology etc.Microemulsion technology is at thermodynamically stable, the isotropy that forms under the effect of tensio-active agent, appearance transparent or translucent, the dispersion system of particle diameter in 1～100nm scope with two kinds of non soluble liquids.Laser radiation technology is to utilize the laser radiation material surface to produce the moment High Temperature High Pressure, makes the material production nano_scale particle.The redeposition technology of preparing of organic molecule nano material is exactly that the compounding agent solution that will contain target compound injects the relatively poor solvent of another kind of solvability, generates organic nanometer granule because the sudden change of environment makes organic molecule produce precipitation.It is more simple, flexibly that reprecipitation method has the machine nano particle than microemulsion method and laser radiation legal system.High-pressure homogeneously can in homogenizing valve, form a huge pressure when being exactly in high pressure homogenizer under the material high pressure and fall with the valve member of high flow velocity (300～50 meter per second) by can the adjusting play, and produce multiple effects such as hole effect, intense impact and great shear forces, thereby original more coarse emulsion or suspension are processed into narrower, the stable organic nanometer granule of size distribution.
Summary of the invention
The invention provides a kind of redeposition-homogeneous legal system and be equipped with the technology of DISPERSE BLUE 2BLN dyestuff, with the DISPERSE BLUE 2BLN dyestuff under the effect of composite assistant and dispersion agent, ball milling obtains dye dispersion liquid together, then with dye dispersion liquid under the ball milling state, be injected in the aqueous solution of composite dispersing agent, the dye solution that obtains carries out the nanometer homogeneous by high pressure homogenizer again, prepares nano level DISPERSE BLUE 2BLN dyestuff.
Redeposition-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, comprise: DISPERSE BLUE 2BLN dyestuff filter cake and solvent, dispersion agent are carried out ball milling, obtain milk sap, this milk sap slowly is added drop-wise in the aqueous solution of the dispersion agent of strong ball milling in ball-milling medium, behind the strong ball milling, again dispersed dye liquid is carried out high-pressure homogeneous processing, obtain nano level DISPERSE BLUE 2BLN liquid dyes.
Described solvent comprises: ethanol, methyl alcohol, butanols, ethylene glycol, polyoxyethylene glycol, acetone, N, dinethylformamide (DMF) etc., mixture that also can above-mentioned solvent; Preferred alcohol.
Described dispersion agent comprises: lignosulfonic acid salt dispersion agent, as dispersant A S-3, dispersion agent Reax-85A; Methanonaphthalene sodium sulfonate class dispersion agent is as Dispersant MF, dispersion agent NNO etc.Non-ionic dispersing agent polyoxyethylene glycol, Soxylat A 25-7 etc.Preferred lignosulfonic acid salt dispersant A S-3, Dispersant MF, polyoxyethylene glycol etc.
Described ball-milling medium comprises: the zirconium oxide bead of φ 1～3mm, the quartz sand of the granulated glass sphere of φ 1～3mm and φ 1～3mm, the zirconium oxide bead of preferred φ 1mm.
It is 3～12h that described DISPERSE BLUE 2BLN dyestuff filter cake, solvent and dispersion agent are put into the time that ball-grinding machine carries out ball milling.
The part by weight of described dyestuff filter cake, solvent and dispersion agent is 1: (1～3): (0.6～1.2).
In the described aqueous solution that dye liquid is slowly splashed in ball-milling medium the dispersion agent under the strong ball milling, the weight ratio of the dye liquid and the aqueous solution is preferably 1: (3～5).
The aqueous solution optimum ratio of above-mentioned dispersion agent is: dispersion agent: water=1: (3～7).
The above-mentioned strong at least 5 hours ball milling time, the preferred 800～1400r/min of stirring velocity.
Described dispersed dye liquid is carried out high-pressure homogeneous, homogenization pressure 800～1400 crust, preferred 1200 crust.Homogeneous cycle index 3～9 times, preferred 6 times.
The preparation technology of nano level DISPERSE BLUE 2BLN dyestuff provided by the invention, it is simple to have preparation technology, and equipment requirements is low, characteristics such as easy industrialization.The nano level DISPERSE BLUE 2BLN size of preparing with the present invention is: D
90＜100 nanometers can be used for superfine Denier fibre dyeing.
Description of drawings
Fig. 1 is the size distribution figure of the nano level DISPERSE BLUE 2BLN liquid dyes of the present invention's preparation;
Fig. 2 is the size distribution table of the nano level DISPERSE BLUE 2BLN liquid dyes of the present invention's preparation.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but protection scope of the present invention is not limited to this.
Embodiment 1
With DISPERSE BLUE 2BLN filter cake 50g, ethanol, dispersant A S-3 put into ball mill to carry out ball milling 5h at 1: 2: 0.5, obtain uniform and stable milk sap.Add 20g dispersant A S-3 in 120g water, under the condition of carrying out the high speed ball milling, ball-milling medium is the zirconium oxide bead of φ 1～3mm, and the milk sap 75g that slow dropping has prepared drips off the back and continues ball milling 8h.The dye liquid that obtains is carried out high-pressure homogeneous circulation 3 times at last, and homogenization pressure is 1200bar, obtains nano level DISPERSE BLUE 2BLN dye solution at last.This dye solution median size (D after testing
50) be 70nm, 90% particle diameter (D
90) be 98nm.
With DISPERSE BLUE 2BLN filter cake 50g, double solvents (ethanol: ethylene glycol is 4: 1), dispersant A S-3 put into ball mill to carry out ball milling 3h at 1: 1: 0.5, obtain uniform and stable milk sap.Add 20g dispersant A S-3 in 120g water, under the condition of carrying out the high speed ball milling, ball-milling medium is the quartz sand of φ 1～3mm, and the milk sap 150g that slow dropping has prepared drips off the back and continues ball milling 6h.The dye liquid that obtains is carried out high-pressure homogeneous circulation 3 times at last, and homogenization pressure is 1200bar, obtains nano level DISPERSE BLUE 2BLN dye solution at last.This dye solution median size (D after testing
50) be 75nm, 90% particle diameter (D
90) be 97nm.
Embodiment 3
With DISPERSE BLUE 2BLN filter cake 50g, double solvents (ethanol: ethylene glycol is 3.5: 1), dispersion agent Reax-85A put into ball mill to carry out ball milling 5h at 1: 1: 0.5, obtain uniform and stable milk sap.Add 20g dispersion agent Reax-85A in 120g water, under the condition of carrying out the high speed ball milling, ball-milling medium is the granulated glass sphere of φ 1～3mm, and the milk sap 120g that slow dropping has prepared drips off the back and continues ball milling 6h.The dye liquid that obtains is carried out high-pressure homogeneous circulation 6 times at last, and homogenization pressure is 1200bar, obtains nano level DISPERSE BLUE 2BLN dye solution at last.This dye solution median size (D after testing
50) be 72nm, 90% particle diameter (D
90) be 94nm.
Claims (10)
1. redeposition-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, comprise: DISPERSE BLUE 2BLN dyestuff filter cake and solvent, dispersion agent are carried out ball milling, obtain milk sap, this milk sap slowly is added drop-wise in the aqueous solution of the dispersion agent of strong ball milling in ball-milling medium, behind the strong ball milling, again dispersed dye liquid is carried out high-pressure homogeneous processing, obtain nano level DISPERSE BLUE 2BLN liquid dyes.
2. redeposition according to claim 1-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: described solvent comprises ethanol, methyl alcohol, butanols, ethylene glycol, polyoxyethylene glycol, acetone, N, a kind of or its mixture in the dinethylformamide.
3. redeposition according to claim 2-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: described solvent is an ethanol.
4. redeposition according to claim 1-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: described dispersion agent comprises: a kind of in lignosulfonic acid salt dispersion agent, methanonaphthalene sodium sulfonate class dispersion agent, the non-ionic dispersing agent.
5. redeposition according to claim 1-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: described ball-milling medium comprises: the zirconium oxide bead of φ 1～3mm, the quartz sand of the granulated glass sphere of φ 1～3mm or φ 1～3mm.
6. redeposition according to claim 5-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: described ball-milling medium is the zirconium oxide bead of φ 1mm.
7. redeposition according to claim 1-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: the part by weight of described dyestuff filter cake, solvent and dispersion agent is 1: 1～3: 0.6～1.2.
8. redeposition according to claim 1-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: in the described aqueous solution that milk sap is slowly splashed in ball-milling medium the dispersion agent under the strong ball milling, the weight ratio of the milk sap and the aqueous solution is 1: 3～5.
9. redeposition according to claim 8-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: in the aqueous solution of the dispersion agent under the described strong ball milling, the aqueous solution proportioning of dispersion agent is: dispersion agent: water=1: 3～7.
10. redeposition according to claim 1-homogeneous legal system is equipped with the technology of DISPERSE BLUE 2BLN dyestuff, it is characterized in that: at least 5 hours time of described strong ball milling, high-pressure homogeneous operational condition is: homogenization pressure 800～1400 crust, homogeneous cycle index 3～9 times.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199366A (en) * | 2011-03-30 | 2011-09-28 | 嘉兴学院 | Biological dye containing prodigiosins, preparation method thereof and application thereof |
| CN104530756B (en) * | 2014-10-20 | 2016-06-01 | 华南理工大学 | A kind of Lignins nano-dispersed dye well its preparation method |
| CN104530762B (en) * | 2014-12-31 | 2017-06-23 | 浙江闰土染料有限公司 | Orange liquid disperse dyes and its preparation method and purposes |
| CN104497631B (en) * | 2014-12-31 | 2017-06-06 | 浙江闰土股份有限公司 | Blue liquid disperse dyes and its preparation method and purposes |
| CN104448933B (en) * | 2014-12-31 | 2017-07-07 | 浙江闰土股份有限公司 | Red liquid disperse dyes and its preparation method and purposes |
| CN106380893A (en) * | 2016-08-25 | 2017-02-08 | 上海盛丘材料科技有限公司 | Preparation method and dyeing method of liquid disperse dye composition |
| CN106948194A (en) * | 2017-02-10 | 2017-07-14 | 常州纺织服装职业技术学院 | A kind of superhigh molecular weight polyethylene fibers colouring method |
| CN111138886B (en) * | 2019-12-26 | 2021-05-04 | 东华大学 | Liquid disperse dye and preparation method and application thereof |
| CN113698628A (en) * | 2021-09-28 | 2021-11-26 | 上海健康医学院 | Preparation method of lignin dispersion liquid by high-pressure homogenization method |
| CN114836056A (en) * | 2022-05-18 | 2022-08-02 | 江苏吉华化工有限公司 | Liquid nano disperse dye and preparation method thereof |
| CN115627658A (en) * | 2022-10-27 | 2023-01-20 | 广东睿智环保科技有限责任公司 | Printing ink for low-temperature sublimation transfer printing paper and preparation method and application thereof |
Citations (2)
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| US6174361B1 (en) * | 1998-08-13 | 2001-01-16 | Clariant Gmbh | Process for preparing N,N′-dimethylperylene-3,4,9,10-tetracarboxylic diimide in transparent pigment form |
| CN1649971A (en) * | 2002-04-16 | 2005-08-03 | 科莱恩有限公司 | Method for producing reducible organic pigments |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6174361B1 (en) * | 1998-08-13 | 2001-01-16 | Clariant Gmbh | Process for preparing N,N′-dimethylperylene-3,4,9,10-tetracarboxylic diimide in transparent pigment form |
| CN1649971A (en) * | 2002-04-16 | 2005-08-03 | 科莱恩有限公司 | Method for producing reducible organic pigments |
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Owner name: LONG MARCH CHEMICAL CO., LTD.;ZHEJIANG PROVINCE Free format text: FORMER OWNER: RUNTU CO., LTD., ZHEJIANG Effective date: 20140626 |
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Effective date of registration: 20140626 Address after: 312369, No. five, No. 5, Shangyu Industrial Park, Hangzhou Bay, Shaoxing, Zhejiang, Shangyu Patentee after: Zhejiang Changzheng Chemical Industry Co., Ltd. Address before: 312368 Zhejiang city of Shangyu Province town Patentee before: Zhejiang Runtu Co., Ltd. |