CN113047061A - Ultra-low viscosity color pigment and preparation method and application thereof - Google Patents

Ultra-low viscosity color pigment and preparation method and application thereof Download PDF

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Publication number
CN113047061A
CN113047061A CN202110292321.3A CN202110292321A CN113047061A CN 113047061 A CN113047061 A CN 113047061A CN 202110292321 A CN202110292321 A CN 202110292321A CN 113047061 A CN113047061 A CN 113047061A
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pigment
ultra
color pigment
low viscosity
polyether
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CN113047061B (en
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徐�明
艾丽
曹红梅
宗建红
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Changzhou Xilewei Textile Technology Co ltd
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Changzhou Xilewei Textile Technology Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • C09D11/32Inkjet printing inks characterised by colouring agents
    • C09D11/322Pigment inks
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/60General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
    • D06P1/613Polyethers without nitrogen
    • D06P1/6131Addition products of hydroxyl groups-containing compounds with oxiranes
    • D06P1/6133Addition products of hydroxyl groups-containing compounds with oxiranes from araliphatic or aliphatic alcohols
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/58Material containing hydroxyl groups
    • D06P3/60Natural or regenerated cellulose
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/30Ink jet printing

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Ink Jet Recording Methods And Recording Media Thereof (AREA)

Abstract

The invention discloses an ultra-low viscosity color pigment and a preparation method and application thereof. The ultralow-viscosity color pigment comprises an organic color pigment, a modifier and water, wherein the modifier comprises oleyl polyether, glycerol polyether, a polymer adhesive and a propionate crosslinking agent, and the mass ratio of the oleyl polyether to the glycerol polyether is 1: 0.3-0.9. The color pigment prepared by the invention has the characteristic of ultralow viscosity, and the viscosity is only 2-3 mPa.s.

Description

Ultra-low viscosity color pigment and preparation method and application thereof
Technical Field
The invention relates to a preparation technology of a water-based pigment, in particular to an ultralow-viscosity color pigment and a preparation method and application thereof.
Background
When the textile is subjected to ink-jet printing, the coating ink or the pigment ink is sprayed to the surface of the textile through a nozzle of an ink-jet printing device to form a required pattern, so that the special requirements on the properties of the coating ink or the pigment ink are met, such as small particle size, low viscosity, better rheological property, water dilution stability and the like of the coating or the pigment. The main technical content is to improve the color fastness of the coating or pigment and textile products by utilizing the radical polymerization reaction generated by vinyl monomers on fabrics: for example, patent application No. CN201710670752.2 discloses a coating ink comprising water-based inkjet resin and nano printing inkjet ink, wherein the water-based inkjet resin is prepared from methyl methacrylate, N-butyl acrylate, hydroxyethyl acrylate, acrylic acid, styrene, N-hydroxyethyl acrylamide, an emulsifier, sodium bicarbonate and an initiator, and the nano printing inkjet ink comprises carbon black pigment paste of cabot, water-based inkjet resin, glycerol, propylene glycol, diethylene glycol, 1, 2-pentanediol, triethylene glycol monobutyl ether, a surfactant and a bactericide; the ink has more excellent performances than the similar ink, and overcomes the defects of wet rubbing resistance, water washing resistance and the like of the textile direct injection ink. Patent application No. CN202010522728.6 discloses a photo-curing white paint ink formed by adding white paint, acrylate monomer and photoinitiator into polyurethane prepolymer, and the ink is considered to form a pigment-curing film cross-linked structure in the curing process. Not only improves the photopolymerization performance of the ink, but also improves the color fastness of the coating ink. Obviously, unlike the conventional radical-initiated polymerization of vinyl monomers, the fixing polymerization on fabrics does not form a good adhesive, and incomplete or uneven polymerization is easily caused due to the migration of acrylic acid and acrylic ester during the drying process and the difference of polymerization conditions, so that better rubbing color fastness is less likely to be obtained, and pattern colorations are caused by incomplete copolymerization and uneven distribution copolymerization formed on the surface.
Disclosure of Invention
The invention aims to provide an ultra-low viscosity color pigment and a preparation method thereof, wherein the prepared color pigment has the characteristic of ultra-low viscosity, the viscosity is only 2-3 mPa.s, and the requirements of inkjet printing and textile dyeing of textiles can be met.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
an ultra-low viscosity color pigment comprising an organic color pigment, a modifier and water; the modifier comprises oleyl polyether, glycerol polyether, polymer adhesive and propionate crosslinking agent; the organic color pigments include c.i. pigment yellow 64, c.i. pigment yellow 74, c.i. pigment orange 1, c.i. pigment orange 24, c.i. pigment orange 38, c.i. pigment violet 23 (permanent violet RL), c.i. pigment red 14, c.i. pigment red 112 (permanent red FGR), c.i. pigment red 146, c.i. pigment red 254 (brilliant red S2 BL), c.i. pigment blue 10, c.i. pigment blue 15 (phthalocyanine blue B), c.i. pigment blue 22, c.i. pigment green 7, c.i. pigment green 36 (phthalocyanine green 3G); the polymeric binder is S0501; the cross-linking agent is trimethylolpropane tri [3- (aziridine-1-yl) propionate ].
The invention discloses a preparation method of the ultra-low viscosity color pigment, which comprises the following steps: mixing organic color pigment, oleyl polyether, glycerol polyether and water, grinding for the first time, adding a polymer adhesive and a cross-linking agent, and grinding again to obtain the ultra-low viscosity color pigment.
In the invention, the mass ratio of the oleyl polyether to the glyceryl polyether is 1 to (0.3-0.9), preferably 1 to (0.5-0.8).
According to the invention, the sum of the mass of the organic color pigment, the mass of the oleyl polyether, the mass of the glycerol polyether and the mass of the water is 100 parts, the mass of the organic color pigment is 10-20 parts, the sum of the mass of the oleyl polyether and the mass of the glycerol polyether is 2.5-4.5 parts, the mass of the polymer adhesive is 20-40 parts, and the mass of the propionate crosslinking agent is 10-20 parts. Preferably, the amount of the polymer binder is 30-40% of the sum of the mass of the organic color pigment, the mass of the oleyl polyether, the mass of the glycerol polyether and the mass of the water; the dosage of the cross-linking agent is 10-20% of the sum of the mass of the organic color pigment, the mass of the oleyl polyether, the mass of the glycerol polyether and the mass of the water.
In the invention, the time for primary grinding is 2-4 hours; the time for the secondary grinding is 1-2 hours.
The invention discloses an application of the ultra-low viscosity color pigment in preparing ink-jet printing ink or printing fabrics. And diluting the ultralow-viscosity color pigment with water to obtain the color ink for textile printing.
According to the invention, a modifier is composed of oleyl polyether, glycerol polyether, a polymer adhesive and a propionate crosslinking agent, wherein the oleyl polyether is octadecenol polyoxyethylene ether, and EO is 20-24; the glycerol polyether is glycerol polyoxyethylene ether, wherein EO is 18-26. The particle size of the ultra-low viscosity color pigment obtained by two times of grinding is not more than 110 nm.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the ultralow-viscosity color pigment obtained by twice grinding has the ultralow viscosity characteristic, and the viscosity is only 2-3 mPa.s. Due to the ultra-low viscosity characteristic, the organic pigment is easier to permeate between the textile yarns, and the excellent pattern definition can be obtained by the textile ink-jet printing pretreatment. The transmission electron microscope shows that the prepared ultra-low viscosity color pigment has uniform coating property, and the binder/cross-linking agent can uniformly form interaction with the pigment particles.
Drawings
FIG. 1 is a graph showing the results of a particle size test for an ultra-low viscosity color pigment prepared in example 1;
FIG. 2 is the results of the particle size test for the ultra low viscosity color pigment prepared in example 2;
FIG. 3 is the results of the particle size test for the ultra low viscosity color pigment prepared in example 3;
FIG. 4 is the results of the particle size test for the ultra low viscosity color pigment prepared in example 4;
FIG. 5 is the results of the particle size test for the ultra low viscosity color pigment prepared in example 5;
FIG. 6 is the results of the particle size test for the ultra low viscosity color pigment prepared in example 6;
FIG. 7 is the results of the particle size test for the ultra low viscosity color pigment prepared in example 7;
FIG. 8 is the transmission electron microscope test results of the ultra low viscosity color pigment prepared in example 1;
FIG. 9 is a graph showing the effect of the ultra-low viscosity color pigment ink-jet printed cotton fabric prepared in example 1;
FIG. 10 is the results of ultra low viscosity color pigment rheology testing;
fig. 11 is the rheological test results of ultra low viscosity color pigments.
Detailed Description
The invention is further described below with reference to the following examples:
the invention takes organic color pigment, oleyl polyether, glycerol polyether, water, polymer adhesive and cross-linking agent as raw materials, does not need other additives and operation steps, and obtains the ultra-low viscosity color pigment by grinding twice, wherein the grain diameter is less than 110 nm; the ink is directly diluted by water to be used as ink-jet printing ink, and the prepared printed fabric has good color fastness.
All the raw materials of the invention are commercial products, such as oleyl polyether OV-20 (octadecenol polyoxyethylene ether, EO number is 20), oleyl polyether OV-24 (octadecenol polyoxyethylene ether, EO number is 24); glyceryl polyether G-18 (glyceryl polyoxyethylene ether, EO number is 18), glyceryl polyether G-20 (glyceryl polyoxyethylene ether, EO number is 20), glyceryl polyether G-26 (glyceryl polyoxyethylene ether, EO number is 26); the polymer binder was S0501 from debayurve binder, suzhou, inc; the propionate crosslinking agent is JS (trimethylolpropane tris [3- (aziridine-1-yl) propionate ]). The fabric was a conventional cotton fabric without pretreatment. The printing of the desired pattern on an ink jet printer is conventional. Unless otherwise specified, the preparation and testing of the present invention were carried out in a conventional room temperature environment.
Figure 340237DEST_PATH_IMAGE002
In Table 1, Y1 and Y2 represent the time of the initial polishing and the time of the regrinding, respectively, and the unit is hour, and the rotational speed of polishing is 4500 rpm.
Examples and comparative examples were prepared by adding an organic c.i. pigment, oleyl polyether, glyceryl polyether and water to a planetary ball mill, primarily grinding with zirconia beads, adding a binder S0501 and a crosslinking agent JS, and secondarily grinding to obtain an ultra-low viscosity color pigment.
Adding water into the ultra-low viscosity color pigment to 300 g to obtain printing ink (wherein the mass fraction of the organic pigment is 5.0%); the required pattern (cotton fabric, without pretreatment) is printed on an ink-jet printing machine conventionally, and the color ink-jet printing cotton fabric is prepared by drying (drying for 3 minutes at 100 ℃) and baking for 80 seconds at 170 ℃.
In the present invention, the grinding is a conventional method, using a conventional planetary ball mill, at a speed of 4500 rpm. The particle size test is a conventional technology, and the particle size of a solid is measured by a nanometer particle sizer for dispersed sampling, specifically on the nanometer particle sizer, and the particle size is represented by D50 and has a unit of nm. Color fastness to rubbing: GB/T3920 'color fastness to rubbing' test is adopted. Fastness to soaping: GB/T3921 'color fastness to soaping test of textile color fastness' is adopted for testing. The appearance of the ultra-low viscosity color pigment is tested by a transmission electron microscope, and the appearance of the pigment can be observed. Rheological property: the viscosity of the pigment can be observed as a function of shear rate, as measured on a rheometer.
The solid particle size test results of the ultra-low viscosity color pigments prepared in examples 1 to 7 are shown in FIGS. 1 to 7, and the particle sizes are 77.67nm, 95.68nm, 102.01 nm, 106.89 nm, 91.43nm, 81.09nm and 99.37 nm, respectively. It can be seen that the particle size of the coated pigment liquids prepared according to the invention is all less than 110nm, even 100 nm. In contrast, the solid particle size test results of the ultra-low viscosity color pigments prepared in comparative examples 1 to 3 were large, 123.22nm, 119.98nm, and 129.87nm, respectively.
FIG. 8 shows the morphology (TEM) of the ultra-low viscosity color pigment prepared in example 1, and it can be seen that the prepared pigment has uniform coating properties and the binder/crosslinker can uniformly interact with the pigment particles.
FIG. 9 is an ink jet printed cotton fabric of example 1 printed with a design pattern by a conventional ink jet printing machine. Therefore, the cotton fabric does not need to be pretreated, and excellent pattern definition can be obtained. The dry rubbing color fastness is grade 5, the wet rubbing color fastness is grade 5, and the soaping cotton color change and the cotton staining are grade 5.
In FIG. 10, curve A shows the coated pigment of example 1The rheology curve, Curve B, for the coated pigment of example 2, is characterized by an ultra-low viscosity with increasing shear rate, such as when the shear rate is 60s-1The viscosity of curve a and curve B were 1.41 and 1.91mpa.s, respectively; when the shear rate is 600s-1The viscosity of curve a and curve B were 1.33 and 1.61mpa.s, respectively; FIG. 11, wherein curve A is the rheology curve of example 5 and curve B is the rheology curve of example 6, shows that the shear rate increases, and the characteristics of ultra-low viscosity are exhibited, for example, when the shear rate is 60s-1The viscosity of curve a and curve B were 2.07 and 1.85 mpa.s, respectively; when the shear rate is 600s-1The viscosity of curve a and curve B was 1.84 and 1.93mpa.s, respectively. When the ink-jet ink is sprayed quickly, the pigment has excellent rheological property, has the characteristic of ultra-low viscosity, has small viscosity change, and can ensure that the coated pigment forms excellent definition on fabrics.

Claims (10)

1. An ultra-low viscosity color pigment, characterized in that the ultra-low viscosity color pigment comprises an organic color pigment, a modifier and water; the modifier comprises oleyl polyether, glycerol polyether, polymer adhesive and propionate crosslinking agent; the organic color pigment includes c.i. pigment yellow 64, c.i. pigment yellow 74, c.i. pigment orange 1, c.i. pigment orange 24, c.i. pigment orange 38, c.i. pigment violet 23, c.i. pigment red 14, c.i. pigment red 112, c.i. pigment red 146, c.i. pigment red 254, c.i. pigment blue 10, c.i. pigment blue 15, c.i. pigment blue 22, c.i. pigment green 7, c.i. pigment green 36.
2. The ultra-low viscosity color pigment of claim 1, wherein the polymeric binder is S0501; the cross-linking agent is trimethylolpropane tri [3- (aziridine-1-yl) propionate ].
3. The ultra-low viscosity color pigment according to claim 1, wherein the mass ratio of the oleyl polyether to the glycerol polyether is 1: 0.3-0.9.
4. The ultra-low viscosity color pigment according to claim 1, wherein the total mass of the organic color pigment, the oleyl polyether, the glycerol polyether and the water is 100 parts, the total mass of the organic color pigment is 10 to 20 parts, the total mass of the oleyl polyether and the glycerol polyether is 2.5 to 4.5 parts, the mass of the polymer binder is 20 to 40 parts, and the mass of the propionate crosslinking agent is 10 to 20 parts.
5. Use of the ultra-low viscosity color pigment of claim 1 for the preparation of ink jet printing inks or printed textiles; or in the preparation of printing pastes or dyed fabrics.
6. The method for preparing an ultra-low viscosity color pigment according to claim 1, comprising the steps of: mixing organic color pigment, oleyl polyether, glycerol polyether and water, grinding for the first time, adding a polymer adhesive and a cross-linking agent, and grinding again to obtain the ultra-low viscosity color pigment.
7. The preparation method of the ultra-low viscosity color pigment according to claim 6, wherein the time for the first grinding is 2-4 hours; the time for the secondary grinding is 1-2 hours.
8. The preparation method of the ultra-low viscosity color pigment according to claim 6, wherein the amount of the polymer binder is 30-40% of the sum of the mass of the organic color pigment, the mass of the oleyl polyether, the mass of the glycerol polyether and the mass of the water; the dosage of the cross-linking agent is 10-20% of the sum of the mass of the organic color pigment, the mass of the oleyl polyether, the mass of the glycerol polyether and the mass of the water.
9. The preparation method of the ultra-low viscosity color pigment according to claim 6, wherein the mass ratio of the oleyl polyether to the glycerol polyether is 1: 0.5-0.8.
10. The method for preparing an ultra-low viscosity color pigment according to claim 6, wherein the ultra-low viscosity color pigment is diluted with water to obtain a color ink for textile printing.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1817981A (en) * 2005-12-31 2006-08-16 浙江大学 Nanometer painting ink-jetting printing oil ink and production thereof
CN101531848A (en) * 2009-03-24 2009-09-16 深圳市墨库数码耗材有限公司 An environment-friendly digital ink-jet direct printing textile ink and method for preparing same
CN101659808A (en) * 2009-08-25 2010-03-03 江苏格美高科技发展有限公司 Aqueous jet ink printing pigment ink for textile and production method thereof
CN101760079A (en) * 2010-02-05 2010-06-30 刘寒剑 Pigment ink for cotton inkjet printing and preparation method thereof
CN107385963A (en) * 2017-08-14 2017-11-24 东莞长联新材料科技股份有限公司 Adhesive for pigment ink-jetting printing ink, the ink comprising it, preparation method and purposes
CN112375429A (en) * 2020-11-16 2021-02-19 卢洁贞 Digital printing pigment ink and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1817981A (en) * 2005-12-31 2006-08-16 浙江大学 Nanometer painting ink-jetting printing oil ink and production thereof
CN101531848A (en) * 2009-03-24 2009-09-16 深圳市墨库数码耗材有限公司 An environment-friendly digital ink-jet direct printing textile ink and method for preparing same
CN101659808A (en) * 2009-08-25 2010-03-03 江苏格美高科技发展有限公司 Aqueous jet ink printing pigment ink for textile and production method thereof
CN101760079A (en) * 2010-02-05 2010-06-30 刘寒剑 Pigment ink for cotton inkjet printing and preparation method thereof
CN107385963A (en) * 2017-08-14 2017-11-24 东莞长联新材料科技股份有限公司 Adhesive for pigment ink-jetting printing ink, the ink comprising it, preparation method and purposes
CN112375429A (en) * 2020-11-16 2021-02-19 卢洁贞 Digital printing pigment ink and preparation method thereof

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