CN108192251B - Nano titanium dioxide color paste and preparation method thereof - Google Patents
Nano titanium dioxide color paste and preparation method thereof Download PDFInfo
- Publication number
- CN108192251B CN108192251B CN201711331662.7A CN201711331662A CN108192251B CN 108192251 B CN108192251 B CN 108192251B CN 201711331662 A CN201711331662 A CN 201711331662A CN 108192251 B CN108192251 B CN 108192251B
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- nano titanium
- dispersant
- color paste
- mill
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/002—Pigment pastes, e.g. for mixing in paints in organic medium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Abstract
The invention belongs to the technical field of pigment color paste preparation, and particularly relates to a nano titanium dioxide color paste and a preparation method thereof. The nanometer titanium dioxide color paste provided by the invention comprises the following components in percentage by mass: 30-40% of surface modified nano titanium dioxide pigment, 5-10% of butyl acetate, 5-10% of propylene glycol methyl ether acetate, 4-10% of composite dispersant, 30-50% of acrylic resin and 10-20% of polyester resin. The nano titanium dioxide color paste pigment provided by the invention has the advantages of fine particle size, good storage stability and good weather resistance.
Description
Technical Field
The invention belongs to the technical field of pigment color paste preparation, and particularly relates to a nano titanium dioxide color paste and a preparation method thereof.
Background
The color paste is a semi-product formed by dispersing pigment or pigment and filling material in the paint vehicle. The pure oil is used as the adhesive to be called as the oily color paste. Resin paint is used as adhesive and is called resin color paste. The pigment and filler pulp which is formed by dispersing water as a medium and adding a surfactant is called water-based color paste. Titanium dioxide is a common white pigment, can provide better whiteness through scattered light, has excellent covering property, and is a common colorant in the industries of coating, papermaking, chemical fiber, natural latex and the like. The titanium white color paste formed by stably dispersing titanium white in a system by using the dispersing agent has a series of advantages of high titanium white content, low price, convenient use, no dust pollution, higher whiteness and covering power and the like. However, compared with other common pigments, the titanium white pigment has the defects of high surface hydroxyl content, strong hydrophilicity, high density, easy sedimentation in the prepared color paste and the like, and the titanium white color paste is easy to precipitate after being stored for a long time.
Chinese patent CN100384953C discloses a titanium dioxide aqueous color paste with certain hydrophobicity, which is composed of 6-12% of dispersant 1, 1-3% of dispersant 2, 0.1-0.5% of defoaming agent 1, 0.1-0.6% of defoaming agent 2, 6-12% of cosolvent, 0.2-0.6% of thickening agent, 50-70% of titanium dioxide pigment, 0.1-0.5% of preservative, 0.1-0.3% of pH regulator and 10-30% of water according to weight percentage, and proper dispersant and defoaming agent are added in the color paste, so that the color paste performance (such as tinting strength, hue, storage stability and the like) is ensured to be unchanged. However, the fineness of the color paste prepared by the method is larger. Chinese patent CN102146220B discloses a method for preparing titanium dioxide pigment color paste for automobile interior leather, which improves the dispersibility of titanium dioxide pigment in the color paste by selecting different types and dosage of dispersing agents, and after grinding, when the viscosity of the color paste is: 4000-20000mPa s, color paste particle size: 4-30 mu m, and stirring uniformly after the color of the titanium dioxide color card meets the tolerance range to obtain the titanium dioxide pigment color paste for the automobile interior leather. However, the method provided by the invention needs to grind more than 2 times, and the performance of the method needs to be further improved.
At present, the existing nano titanium dioxide color paste has the problems of thick pigment particle size, poor storage stability and weather resistance, so that the development of the nano titanium dioxide color paste with thin pigment particle size, good storage stability and good weather resistance is urgent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a nano titanium dioxide color paste and a preparation method thereof. The nano titanium dioxide color paste pigment provided by the invention has the advantages of fine particle size, good storage stability and good weather resistance.
The technical scheme of the invention is as follows:
the nanometer titanium dioxide color paste comprises the following components in percentage by mass: 30-40% of surface modified nano titanium dioxide pigment, 5-10% of butyl acetate, 5-10% of propylene glycol methyl ether acetate, 4-10% of composite dispersant, 30-50% of acrylic resin and 10-20% of polyester resin.
Further, the nanometer titanium dioxide color paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin.
Further, the surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by weight: 10-15 parts of nano titanium dioxide, 0.05-0.08 part of dispersing agent, 0.01-0.03 part of coupling agent and 240 parts of petroleum ether 180-one.
Furthermore, the surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether.
Preferably, the coupling agent consists of vinyl tri-tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane in a mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment comprises the following steps:
(1) adding a dispersing agent into petroleum ether, stirring and completely dissolving to obtain a dispersing solution;
(2) adding the nano titanium dioxide into the dispersion liquid obtained in the step (1), performing ultrasonic dispersion for 3min, adding a coupling agent, and performing ultrasonic dispersion for 7min to obtain an ultrasonic liquid;
(3) heating the ultrasonic liquid obtained in the step (2) to 85 ℃ in a water bath, keeping the temperature constant, and stirring until petroleum ether is completely volatilized to obtain a material;
(4) and (4) drying and grinding the material obtained in the step (3) to obtain the material.
Preferably, the composite dispersant is a combination of a wetting dispersant BYK-180 and a synergistic dispersant EFKA-5220, and the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 is 5-7: 1-2.
More preferably, the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
In addition, the invention also provides a preparation method of the nano titanium white paste, which comprises the following steps:
s1, adding acrylic resin and polyester resin according to the formula ratio, and stirring at the speed of 350-450r/min for 15-25min to obtain a material A;
s2, adding butyl acetate and propylene glycol monomethyl ether acetate with formula amounts into the material A obtained in the step S1, and stirring at the speed of 350-450r/min for 10-15min to obtain a material B;
s3, adding the compound dispersant with the formula amount into the material B obtained in the step S2, and stirring at the speed of 350-450r/min for 3-5min to obtain a material C;
s4, adding the surface modified nano titanium dioxide pigment with the formula amount into the material C obtained in the step S3, and stirring at the speed of 350-450r/min for 25-35min to obtain a material D;
s5, coarsely grinding the material D obtained in the step S4 once by a sand grinder to obtain a coarsely ground material;
s6, grinding the coarse ground material obtained in the step S5 by a sand mill to obtain the coarse ground material with the grinding fineness of less than or equal to 7 mu m.
Preferably, the step S1 is carried out at a speed of 410r/min for 20 min.
Preferably, the step S2 is carried out at a speed of 410r/min for 12 min.
Preferably, the step S3 is carried out at a speed of 410r/min for 4 min.
Preferably, the step S4 is carried out at a speed of 410r/min for 30 min.
Preferably, the rough grinding conditions of step S5 are: particle size of zirconia beads: 1.0-1.2mm, mill speed: 1380-: 53-57 ℃, internal pressure of mill: 0.55-0.65 MPa; the step S6 fine grinding conditions are: particle size of zirconia beads: 0.5-0.6mm, mill speed: 1380-: 53-57 ℃, internal pressure of mill: 0.55-0.65 MPa.
More preferably, the rough grinding conditions of step S5 are: particle size of zirconia beads: 1.0mm, mill speed: 1410r/min, slurry outlet temperature: 56 ℃, mill internal pressure: 0.60 MPa; the step S6 fine grinding conditions are: particle size of zirconia beads: 0.6mm, mill speed: 1410r/min, slurry outlet temperature: 56 ℃, mill internal pressure: 0.60 MPa.
The surface energy and the specific surface area of the nano titanium dioxide are large, so that aggregates are easy to form, the prepared color paste is easy to settle, and the like. According to the invention, through surface modification of the nano titanium dioxide, the properties of the nano titanium dioxide such as dispersion, wetting, adsorption and the like can be changed, the stability of the nano titanium dioxide in color paste can be enhanced, and meanwhile, the weather resistance of the obtained product can be enhanced.
In the invention, the composite dispersant consisting of the wetting dispersant BYK-180 and the synergistic dispersant EFKA-5220 according to a certain mass ratio not only has good dispersion effect on the surface modified nano titanium white pigment and improves the dispersion efficiency, but also can act synergistically with polyester resin to enhance the storage stability of the color paste. Meanwhile, the coarse grinding is carried out during grinding to improve the early-stage dispersion efficiency of the pigment, and then the fine grinding is carried out to grind the pigment to a finer particle size, so that the transparency and the chroma reach higher levels.
Compared with the prior art, the nano titanium white paste provided by the invention has the following advantages:
(1) the nano titanium dioxide color paste provided by the invention has good storage stability, and can be stored at 50-40 ℃ for one month alternately with cold and hot temperatures, and the fineness and the hue are not changed.
(2) The weather resistance of the nano titanium white color paste prepared by testing the method of artificially accelerated ageing by a QUV (ultraviolet lamp) and the method of artificially accelerated ageing by a QSUN (xenon lamp) is adopted, and the test result shows that the nano titanium white color paste prepared by the invention has good weather resistance.
(3) The nano titanium white paste pigment provided by the invention has the advantages of fine particle size, high transparency and high chroma.
Detailed Description
The present invention is further described in the following description of the specific embodiments, which is not intended to limit the invention, but various modifications and improvements can be made by those skilled in the art according to the basic idea of the invention, within the scope of the invention, as long as they do not depart from the basic idea of the invention.
The wetting dispersant BYK-180 can be purchased from Shanghai province Shanghai industry materials Co., Ltd; the synergistic dispersant EFKA-5220 is available from Guangzhou Si Tuiyuan chemical Co., Ltd; dispersants are available from Guangzhou Baohua trade, Inc., type: BYK-P104S.
Example 1 nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 40% of surface modified nano titanium dioxide pigment, 10% of butyl acetate, 5% of propylene glycol methyl ether acetate, 4% of composite dispersant, 30% of acrylic resin and 11% of polyester resin; the composite dispersant is a combination of wetting dispersant BYK-180 and synergistic dispersant EFKA-5220, and the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 is 5: 2.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 10 parts of nano titanium dioxide, 0.05 part of dispersing agent, 0.01 part of coupling agent and 180 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment comprises the following steps:
(1) adding a dispersing agent into petroleum ether, stirring and completely dissolving to obtain a dispersing solution;
(2) adding the nano titanium dioxide into the dispersion liquid obtained in the step (1), performing ultrasonic dispersion for 3min, adding a coupling agent, and performing ultrasonic dispersion for 7min to obtain an ultrasonic liquid;
(3) heating the ultrasonic liquid obtained in the step (2) to 85 ℃ in a water bath, keeping the temperature constant, and stirring until petroleum ether is completely volatilized to obtain a material;
(4) and (4) drying and grinding the material obtained in the step (3) to obtain the material.
The preparation method of the nanometer titanium dioxide color paste comprises the following steps:
s1, adding acrylic resin and polyester resin according to the formula ratio, and stirring at the speed of 350r/min for 15min to obtain a material A;
s2, adding butyl acetate and propylene glycol monomethyl ether acetate with the formula ratio into the material A obtained in the step S1, and stirring at the speed of 350r/min for 10min to obtain a material B;
s3, adding the compound dispersant with the formula amount into the material B obtained in the step S2, and stirring at the speed of 350r/min for 3min to obtain a material C;
s4, adding the surface modified nano titanium dioxide pigment with the formula amount into the material C obtained in the step S3, and stirring at the speed of 350r/min for 25min to obtain a material D;
s5, roughly grinding the material D obtained in the step S4 by a sand grinder, wherein the rough grinding conditions are as follows: particle size of zirconia beads: 1.0mm, mill speed: 1380r/min, slurry outlet temperature: 53 ℃, internal pressure of the mill: 0.55MPa to obtain a coarse grinding material;
s6, the coarse grinding material obtained in the step S5 is finely ground by a sand mill under the following fine grinding conditions: particle size of zirconia beads: 0.5mm, mill speed: 1380r/min, slurry outlet temperature: 53 ℃, internal pressure of the mill: 0.55MPa, and the grinding fineness is less than or equal to 7 mu m.
Example 2 nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 5% of propylene glycol methyl ether acetate, 10% of composite dispersant, 30% of acrylic resin and 20% of polyester resin; the composite dispersant is a combination of wetting dispersant BYK-180 and synergistic dispersant EFKA-5220, and the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 is 7: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 15 parts of nano titanium dioxide, 0.08 part of dispersing agent, 0.03 part of coupling agent and 240 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nanometer titanium dioxide color paste comprises the following steps:
s1, adding acrylic resin and polyester resin according to the formula ratio, and stirring at the speed of 450r/min for 25min to obtain a material A;
s2, adding butyl acetate and propylene glycol monomethyl ether acetate with the formula ratio into the material A obtained in the step S1, and stirring at the speed of 450r/min for 15min to obtain a material B;
s3, adding the compound dispersant with the formula amount into the material B obtained in the step S2, and stirring at the speed of 450r/min for 5min to obtain a material C;
s4, adding the surface modified nano titanium dioxide pigment with the formula amount into the material C obtained in the step S3, and stirring at the speed of 450r/min for 35min to obtain a material D;
s5, roughly grinding the material D obtained in the step S4 by a sand grinder, wherein the rough grinding conditions are as follows: particle size of zirconia beads: 1.2mm, mill speed: 1420r/min, slurry outlet temperature: 57 ℃, internal pressure of the mill: 0.65MPa to obtain a coarse grinding material;
s6, the coarse grinding material obtained in the step S5 is finely ground by a sand mill under the following fine grinding conditions: particle size of zirconia beads: 0.6mm, mill speed: 1420r/min, slurry outlet temperature: 57 ℃, internal pressure of the mill: 0.65MPa, and the grinding fineness is less than or equal to 7 mu m.
Example 3 nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the composite dispersant is a combination of wetting dispersant BYK-180 and synergistic dispersant EFKA-5220, and the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nanometer titanium dioxide color paste comprises the following steps:
s1, adding acrylic resin and polyester resin according to the formula ratio, and stirring at the speed of 410r/min for 20min to obtain a material A;
s2, adding butyl acetate and propylene glycol monomethyl ether acetate with formula amounts into the material A obtained in the step S1, and stirring at the speed of 410r/min for 12min to obtain a material B;
s3, adding the compound dispersant with the formula amount into the material B obtained in the step S2, and stirring at the speed of 410r/min for 4min to obtain a material C;
s4, adding the surface modified nano titanium dioxide pigment with the formula amount into the material C obtained in the step S3, and stirring at the speed of 410r/min for 30min to obtain a material D;
s5, roughly grinding the material D obtained in the step S4 by a sand grinder, wherein the rough grinding conditions are as follows: particle size of zirconia beads: 1.0mm, mill speed: 1410r/min, slurry outlet temperature: 56 ℃, mill internal pressure: 0.60 MPa; obtaining a coarse grinding material;
s6, the coarse grinding material obtained in the step S5 is finely ground by a sand mill under the following fine grinding conditions: particle size of zirconia beads: 0.6mm, mill speed: 1410r/min, slurry outlet temperature: 56 ℃, mill internal pressure: 0.60MPa, and the grinding fineness is less than or equal to 7 mu m.
Comparative example 1, nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 1: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from the example 3 is that the mass ratio of the wetting dispersant BYK-180 and the synergistic dispersant EFKA-5220 in the composite dispersant is modified from 5:1 to 1: 1.
comparative example 2, nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 1: 1.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from the example 3 is that the coupling agent in the raw materials used for the surface modified nanometer titanium dioxide pigment is modified from vinyl tri-tert-butyl peroxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7:2 into 1: 1.
Comparative example 3, nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 2: 1.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from the example 3 is that the coupling agent in the raw materials used for the surface modified nanometer titanium dioxide pigment is modified from vinyl tri-tert-butyl peroxy silane and gamma-aminopropyl triethoxy silane according to the mass ratio of 7:2 to 2: 1.
Comparative example 4, nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent is gamma-methacryloxypropyltrimethoxysilane.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from the example 3 is that the coupling agent in the raw material used for the surface modified nano titanium white pigment is gamma-methacryloxypropyltrimethoxysilane.
Comparative example 5 nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from the example 3 is that the nano titanium white paste is prepared without coarse grinding.
Comparative example 6, nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from the example 3 is that the grain diameter of the zirconia beads in the step S6 in the preparation method of the nano titanium white paste is 0.2 mm.
Comparative example 7 nanometer titanium dioxide color paste
The nano titanium white paste comprises the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant and 51.5% of acrylic resin; the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
The surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether; the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyl triethoxysilane according to the mass ratio of 7: 2.
The preparation method of the surface modified nano titanium dioxide pigment is similar to that of the example 1.
The preparation method of the nano titanium dioxide color paste is similar to that of the embodiment 3.
The difference from example 3 is that the mass percentage of the polyester resin was changed from 11.5% to 0, and the mass percentage of the acrylic resin was changed from 40% to 51.5%.
Test example I, fineness test of Nano titanium white paste
1. Test materials: the nanometer titanium dioxide color paste prepared by the following steps of example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, comparative example 4, comparative example 6 and comparative example 7.
2. The test method comprises the following steps: the fineness of the nanometer titanium dioxide color paste is tested by adopting a 25 mu m scraper blade fineness meter.
3. And (3) test results: the test results are shown in table 1.
Table 1: fineness test result of nano titanium dioxide color paste
As can be seen from Table 1, the fineness of the nano titanium white paste prepared by the invention is small, wherein the smallest fineness in the embodiment 3 is the best embodiment of the invention; compared with comparative examples 1, 2, 3, 4, 6 and 7, the fineness of example 3 is smaller, which shows that the composite dispersant composed of wetting dispersant BYK-180 and synergistic dispersant EFKA-5220 according to a certain mass ratio has good dispersion effect on the surface modified nano titanium white pigment, the dispersion efficiency can be improved, and the early-stage dispersion efficiency of the pigment can be improved by carrying out coarse grinding before grinding, and then carrying out fine grinding, so that the pigment can be ground to a finer particle size. Test example II storage stability
1. Test materials: the nanometer titanium white color paste prepared by the following steps of example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, comparative example 4 and comparative example 5.
2. The test method comprises the following steps: the nanometer titanium dioxide color paste prepared by the invention is stored for one month at 50 ℃ to-40 ℃ alternately in a cold and hot way, the change of fineness is tested, and the change of hue is observed.
3. And (3) test results: the test results are shown in table 2.
Table 2: storage stability test results
As can be seen from Table 2, the fineness of the nano titanium dioxide paste prepared by the invention is unchanged after the test, and the observation shows that the hue of the nano titanium dioxide paste prepared by the invention is also unchanged, which indicates that the nano titanium dioxide paste has good storage stability. The storage stability of example 3 of the present invention was better than comparative examples 1, 2, 3, 4 and 5.
Third test example weather resistance test of nanometer titanium dioxide color paste
1. Test materials: the nanometer titanium white color paste prepared in the embodiment 1, the embodiment 2, the embodiment 3, the comparative example 2, the comparative example 3 and the comparative example 4.
2. The test method comprises the following steps: the weather resistance of the prepared nano titanium white paste is tested by adopting a QUV (ultraviolet lamp) artificial accelerated aging method and a QSUN (xenon lamp) artificial accelerated aging method.
3. The test results are shown in table 3.
Table 3: weather resistance test result of nano titanium white paste
As can be seen from Table 3, the color difference of the nano titanium white paste prepared by the invention after QUV artificial accelerated aging for 1000 hours and QSUN artificial accelerated aging for 2000 hours is small, which indicates that the nano titanium white paste prepared by the invention has good weather resistance, wherein the weather resistance of the embodiment 3 is the best embodiment of the invention; the weather resistance of example 3 was more excellent than that of comparative examples 2, 3 and 4.
Claims (4)
1. The nanometer titanium dioxide color paste is characterized by comprising the following components in percentage by mass: 30% of surface modified nano titanium dioxide pigment, 5% of butyl acetate, 8.5% of propylene glycol methyl ether acetate, 5% of composite dispersant, 40% of acrylic resin and 11.5% of polyester resin;
the surface modified nano titanium dioxide pigment is prepared from the following raw materials in parts by mass: 10-15 parts of nano titanium dioxide, 0.05-0.08 part of dispersing agent, 0.01-0.03 part of coupling agent and 240 parts of petroleum ether 180-one;
the coupling agent consists of vinyl tert-butyl hydroperoxide silane and gamma-aminopropyltriethoxysilane according to the mass ratio of 7: 2;
the composite dispersant is a combination of wetting dispersant BYK-180 and synergistic dispersant EFKA-5220, and the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 is 5-7: 1-2;
the preparation method of the nanometer titanium dioxide color paste comprises the following steps:
s1, adding acrylic resin and polyester resin according to the formula ratio, and stirring at the speed of 350-450r/min for 15-25min to obtain a material A;
s2, adding butyl acetate and propylene glycol monomethyl ether acetate with formula amounts into the material A obtained in the step S1, and stirring at the speed of 350-450r/min for 10-15min to obtain a material B;
s3, adding the compound dispersant with the formula amount into the material B obtained in the step S2, and stirring at the speed of 350-450r/min for 3-5min to obtain a material C;
s4, adding the surface modified nano titanium dioxide pigment with the formula amount into the material C obtained in the step S3, and stirring at the speed of 350-450r/min for 25-35min to obtain a material D;
s5, coarsely grinding the material D obtained in the step S4 once by a sand grinder to obtain a coarsely ground material;
s6, fine grinding the coarse ground material obtained in the step S5 by a sand mill, wherein the grinding fineness is less than or equal to 7 mu m, and the coarse ground material is obtained;
the rough grinding conditions of the step S5 are as follows: particle size of zirconia beads: 1.0-1.2mm, mill speed: 1380-: 53-57 ℃, internal pressure of mill: 0.55-0.65 MPa; the step S6 fine grinding conditions are: particle size of zirconia beads: 0.5-0.6mm, mill speed: 1380-: 53-57 ℃, internal pressure of mill: 0.55-0.65 MPa.
2. The nanometer titanium dioxide paste as claimed in claim 1, wherein the surface modified nanometer titanium dioxide pigment is prepared from the following raw materials in parts by weight: 12 parts of nano titanium dioxide, 0.06 part of dispersing agent, 0.02 part of coupling agent and 220 parts of petroleum ether.
3. The nanometer titanium dioxide paste as claimed in claim 1, wherein the mass ratio of the wetting dispersant BYK-180 to the synergistic dispersant EFKA-5220 in the composite dispersant is 5: 1.
4. The nano titanium white paste according to claim 1, wherein the rough grinding conditions in the step S5 are as follows:
particle size of zirconia beads: 1.0mm, mill speed: 1410r/min, slurry outlet temperature: 56 ℃, mill internal pressure: 0.60 MPa; the step S6 fine grinding conditions are: particle size of zirconia beads: 0.6mm, mill speed: 1410r/min, slurry outlet temperature: 56 ℃, mill internal pressure: 0.60 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711331662.7A CN108192251B (en) | 2017-12-13 | 2017-12-13 | Nano titanium dioxide color paste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711331662.7A CN108192251B (en) | 2017-12-13 | 2017-12-13 | Nano titanium dioxide color paste and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108192251A CN108192251A (en) | 2018-06-22 |
| CN108192251B true CN108192251B (en) | 2020-04-14 |
Family
ID=62574109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711331662.7A Active CN108192251B (en) | 2017-12-13 | 2017-12-13 | Nano titanium dioxide color paste and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108192251B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982304B (en) * | 2019-12-06 | 2021-05-11 | 中信钛业股份有限公司 | Preparation method of titanium dioxide pigment with high resistivity |
| CN113064323B (en) * | 2021-02-07 | 2022-04-01 | 纳琳威纳米科技南通有限公司 | Photoresist pigment color paste and preparation method thereof |
| CN116082884A (en) * | 2022-12-26 | 2023-05-09 | 黄山新力油墨科技有限公司 | Gravure composite ink for high-speed printing and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101451039A (en) * | 2007-12-04 | 2009-06-10 | 上海宏达着色剂厂 | Aqueous dispersion colorant |
| CN104693898A (en) * | 2013-12-05 | 2015-06-10 | 大连奥林匹克电子城利辉通讯器材商行 | Method for preparing nano-grade water-based pigment |
| CN107250289A (en) * | 2015-02-27 | 2017-10-13 | 堺化学工业株式会社 | The organic solvent dispersion and its manufacture method of titan oxide particles |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007145285A1 (en) * | 2006-06-16 | 2007-12-21 | Nippon Shokubai Co., Ltd. | Polymer-coated metal oxide microparticle and application thereof |
-
2017
- 2017-12-13 CN CN201711331662.7A patent/CN108192251B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101451039A (en) * | 2007-12-04 | 2009-06-10 | 上海宏达着色剂厂 | Aqueous dispersion colorant |
| CN104693898A (en) * | 2013-12-05 | 2015-06-10 | 大连奥林匹克电子城利辉通讯器材商行 | Method for preparing nano-grade water-based pigment |
| CN107250289A (en) * | 2015-02-27 | 2017-10-13 | 堺化学工业株式会社 | The organic solvent dispersion and its manufacture method of titan oxide particles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108192251A (en) | 2018-06-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108192251B (en) | Nano titanium dioxide color paste and preparation method thereof | |
| DE60213514T2 (en) | Ink jet ink, ink jet ink, aqueous pigment dispersion, and organic and inorganic composite pitches | |
| CN103709833B (en) | Preparation method for polymer coated inorganic pigment paste for color modulation of production line | |
| US20020069790A1 (en) | Composite particles, process for producing the same, and pigment, paint and resin composition using the same | |
| EP2087045B1 (en) | Pigment dispersion | |
| WO2018180936A1 (en) | Coated pigment | |
| CN104119751B (en) | A kind of nano enamel and preparation method thereof for aircraft skin | |
| CN110204978A (en) | A kind of aqueous plastic coating and preparation method thereof and application method | |
| JP5288085B2 (en) | Process for producing organic / inorganic composite particle powder, organic / inorganic composite pigment comprising organic / inorganic composite particle powder, paint and resin composition using the organic / inorganic composite pigment, pigment dispersion containing the organic / inorganic composite pigment, and masterbatch pellet | |
| CN101993640A (en) | Plastic part water-based primer and preparation method thereof | |
| CN108117800B (en) | Extra-black color paste and preparation method thereof | |
| CN109181516B (en) | Water-based weather-resistant scratch-resistant self-cleaning inorganic nano ceramic automobile paint and preparation method thereof | |
| AU2008200377A1 (en) | Hydrophobic metal and metal oxide particles with unique optical properties | |
| CN107793852B (en) | Environment-friendly latex paint taking ceramic polishing waste residues as regenerated filler and preparation method thereof | |
| US20080295738A1 (en) | Pigment dispersion | |
| CN109679411B (en) | Preparation method of titanium dioxide pigment-coated aqueous dispersion | |
| CN106675211B (en) | Water-based highlight antirust carbon black color paste and preparation method and application thereof | |
| CN109943152A (en) | A kind of nanometer transparent iron oxide ink-jet mill base and preparation method thereof | |
| JP6072461B2 (en) | Organic inorganic composite particle powder | |
| CN105885601A (en) | Water-based paint coating and preparation method thereof | |
| CN110256969A (en) | A kind of smalt fine polishing liquid and its preparation method | |
| CN109337440A (en) | A kind of environment-friendly water-based gravure printing ink and preparation method thereof | |
| CN105670485B (en) | A kind of nanometer of Al2O3Modified polyurethane resin coating and preparation method thereof | |
| CN112920664A (en) | Coating for water-based white shading plastic substrate and preparation method thereof | |
| WO2022142749A1 (en) | High-stability fluorescent color paste and preparation method therefor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: The two district 529700 in Guangdong province Jiangmen city Heshan City, the ancient town of labor three industrial zone Applicant after: Yatu high tech materials Co., Ltd Address before: The two district 529700 in Guangdong province Jiangmen city Heshan City, the ancient town of labor three industrial zone Applicant before: YATU ADVANCED MATERIALS Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |