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CN115160825A - Modified yellow pigment and preparation method and application thereof - Google Patents

Modified yellow pigment and preparation method and application thereof Download PDF

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Publication number
CN115160825A
CN115160825A CN202210992862.1A CN202210992862A CN115160825A CN 115160825 A CN115160825 A CN 115160825A CN 202210992862 A CN202210992862 A CN 202210992862A CN 115160825 A CN115160825 A CN 115160825A
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Prior art keywords
yellow pigment
pigment
modified
silica sol
modified yellow
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Inventor
郑帆
盖德成
牛林
徐志新
李金钟
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Asia Cuanon New Materials Chuzhou Co ltd
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Asia Cuanon New Materials Chuzhou Co ltd
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Priority to CN202210992862.1A priority Critical patent/CN115160825A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0081Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • C09C1/0084Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound containing titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041Grinding
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12Treatment with organosilicon compounds
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    • 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/004Reflecting paints; Signal paints
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    • 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62L* (lightness axis)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/90Other properties not specified above

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention provides a modified yellow pigment, a preparation method and application thereof, and relates to the technical field of reflective heat-insulating coatings. The invention solves the technical problem that the existing reflective heat-insulating coating cannot meet the requirement of the GB/T25261-2018 standard on the sunlight reflectance in the lightness interval (L value is in the range of 70-85) when common inorganic iron oxide yellow is used for toning, achieves the technical effects of improving the near-infrared reflectance of the reflective heat-insulating coating and having excellent outdoor weather resistance and light resistance.

Description

Modified yellow pigment and preparation method and application thereof
Technical Field
The invention relates to the technical field of reflective heat-insulating coatings, in particular to a modified yellow pigment and a preparation method and application thereof.
Background
The proportion of building energy consumption in the whole energy consumption is generally between 30 and 40 percent, and the building built in China at present generally has lower energy-saving level, so the building energy saving is the subject of sustainable development of China and even the world in a large society.
In recent years, with rapid economic development and continuous urbanization, urban population is concentrated and heat is not easy to diffuse, so that the temperature of the urban area is 3-5 ℃ higher than that of the suburb, which is called as a heat island effect. Solar radiation causes the temperature of the roof and exterior wall surfaces to increase, and the corresponding indoor temperature to increase. The temperature rise reduces the comfort level of the living environment, is not beneficial to the health of the body, and simultaneously increases the power consumption of refrigeration equipment such as an air conditioner and the like. The data show that for each l deg.c rise in temperature, the corresponding power supply increases by 2%, and the energy spent on cooling equipment such as air conditioners, electric fans, air conditioners, etc., exceeds 20% of the total energy consumed nationwide. Along with the development of low-carbon economy, the building energy conservation draws more and more attention of people.
The traditional heat insulating material is mainly used for improving the porosity, increasing the thermal resistance and reducing the heat conductivity coefficient. The fiber heat-insulating material needs to have a thicker coating layer to increase the convective heat transfer and the radiant heat transfer in the use environment; the inorganic heat-insulating material of section class has the disadvantages of many seams, poor waterproofness, short service life and the like. The reflective heat-insulating coating for the building, as a novel energy-saving material, can effectively reflect, obstruct and radiate the energy of sunlight, obviously reduce the temperature of the outer wall, roof and indoor space of the building, reduce the energy consumption of refrigeration equipment such as an air conditioner and the like under the high-temperature condition, improve the living and working environment, save a large amount of energy, and play an active role in the aspects of energy conservation and reasonable utilization, environment improvement, factory safety accident prevention and the like.
At present, most of reflective thermal insulation coatings for buildings at home and abroad are mainly white emulsion paints and lack colors and artistic modeling, and along with the increasing living standard of people, people have more requirements on the colors and the styles of exterior wall coatings, so that the application and the diversification of the colors are indispensable conditions in a reflective thermal insulation coating system. As the reflective thermal insulation coating for buildings is just emerging at present and has few executable standards, JG/T235-2014 and GB/T25261-2018 are taken as main evaluation bases at present; after the inorganic iron oxide yellow paste/toner is used as a coating for color mixing, when the brightness value L is in a range of 70-85, the sunlight reflection ratio can meet the requirement of the standard JG/T235-2014, but cannot meet the requirement of the new national standard GB/T25261-2018 because the common iron oxide yellow pigment does not have the near infrared reflection capability; the organic yellow paste/toner has small average particle size, so that sunlight can directly penetrate through the pigment under the most conditions, and the organic yellow paste/toner does not have a reflection function.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
It is an object of the present invention to provide a modified yellow pigment having a high near infrared reflectance.
The second purpose of the invention is to provide a preparation method of the modified yellow pigment, which has simple and efficient process.
The invention also aims to provide application of the modified yellow pigment, which has outstanding application effect.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, a modified yellow pigment is a yellow pigment with a silica-coated surface;
the yellow pigment includes at least one of pigment brown 24 and pigment yellow 53.
Further, the particle size distribution D90 of the modified yellow pigment is between 600 and 800nm.
In a second aspect, a method of preparing the modified yellow pigment of any of the above, comprising the steps of:
and treating the yellow pigment by using a silane coupling agent and silica sol to obtain the modified yellow pigment.
Further, the preparation method comprises the following steps:
mixing and dispersing water, a silane coupling agent and the yellow pigment, then adding silica sol, adding acid to adjust the pH value to be neutral, curing, then carrying out solid-liquid separation, and carrying out heat treatment on the obtained solid to obtain the modified yellow pigment.
Further, the preparation method comprises the following steps:
(a) Pre-shearing water, adding a silane coupling agent and the yellow pigment, mixing and dispersing to obtain slurry;
(b) Adding silica sol into the slurry obtained in the step (a), and adding acid to adjust the pH value to be neutral to obtain a mixed solution;
(c) Curing the mixed solution obtained in the step (b), and then carrying out solid-liquid separation to obtain a solid;
(d) And (c) carrying out heat treatment on the solid obtained in the step (c), cooling and then scattering the solid to obtain a scattered product, and grinding the scattered product to obtain the modified yellow pigment.
Further, in the step (a), the mass ratio of water, the silane coupling agent and the yellow pigment is 100:1:10-40 parts of;
preferably, the slurry obtained in step (a) has an average particle size D50 between 300 and 400 nm.
Further, in the step (b), the mass ratio of the silica sol to the silane coupling agent is 40-160:1;
preferably, the silica sol comprises a sodium type silica sol;
preferably, the sodium silica sol has a solids content of 45 to 55%, preferably 50%.
Further, the temperature of the heat treatment in the step (d) is 500-1000 ℃, and the time of the heat treatment is 3-4h.
Further, the grinding in step (d) comprises the steps of:
pre-shearing a mixed solution of alcohol and water, adding a dispersing agent, mixing with the scattered product, dispersing to obtain pre-dispersed product slurry, and then placing the product slurry in a grinding machine to grind until the particle size distribution D90 is 600-800nm to obtain a modified yellow pigment;
preferably, the alcohol comprises propylene glycol;
preferably, the dispersant comprises PL20 dispersant;
preferably, the mass ratio of the mixed solution of alcohol and water, the dispersant and the product after scattering is 20-30:5-10:60-70 parts of;
preferably, the mill comprises a horizontal mill.
In a third aspect, use of a modified yellow pigment of any of the above in a reflective thermal barrier coating.
Compared with the prior art, the invention has at least the following beneficial effects:
the modified yellow pigment provided by the invention is a yellow pigment with a surface coated with silicon dioxide, wherein the yellow pigment comprises at least one of pigment brown 24 and pigment yellow 53. Pigment brown 24 (P.Br.24), also known as red titanium yellow, can be used for the toning of red-phase yellow, because its pigment crystal form is rutile type, so have stronger near-infrared reflecting power; pigment yellow 53 (p.y.53), also known as titanium-nickel yellow, can be used for toning green-phase yellow, and has strong near-infrared reflection capability because the crystal form of the pigment is rutile; the primary particle sizes of the pigment brown 24 and the pigment yellow 53 are small, the particle size of the pigment aggregate after pigmentation is not controllable, and the best reflection efficiency cannot be achieved, and the particle size of the pigment aggregate can be well controlled by coating the surface with silicon dioxide, so that the near infrared reflectance of the formed surface-modified yellow pigment is further improved.
The preparation method of the modified yellow pigment provided by the invention is simple in process and high in efficiency.
The application of the modified yellow pigment provided by the invention can enable the reflective heat-insulating coating to meet the requirement on the sunlight reflectance in GB/T25261-2018 standard, and has an outstanding application effect.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to a first aspect of the present invention, there is provided a modified yellow pigment, which is a silica-coated yellow pigment;
wherein the yellow pigment comprises at least one of pigment brown 24 and pigment yellow 53.
In the invention, the pigment brown 24 (P.Br.24), also called red titanium yellow, can be used for the toning of red yellow, and has stronger near infrared reflection capability because the crystal form of the pigment is rutile; pigment yellow 53 (p.y.53), also known as titanium-nickel yellow, can be used for toning green-phase yellow, and has strong near-infrared reflection capability because the crystal form of the pigment is rutile; the primary particle sizes of the pigment brown 24 and the pigment yellow 53 are small, the particle size of the pigment aggregate after pigmentation is not controllable, and the best reflection efficiency cannot be achieved, and the particle size of the pigment aggregate can be well controlled by coating the surface with silicon dioxide, so that the near infrared reflectance of the formed surface-modified yellow pigment is further improved.
In the present invention, the purpose of the silica coating is to control the particle size of the pigment agglomerates, and the infrared ray can bypass the particles having smaller particles as analyzed from the optical theory, and has the maximum reflectance when the particle size of the particles is about equal to 1/2 of the wavelength of the incident wave.
In a preferred embodiment, the particle size distribution D90 of the modified yellow pigment of the present invention is between 600 and 800nm, for example, 600nm, 650nm, 700nm, 750nm, 800nm, but not limited thereto, and the near infrared reflectance can be further improved.
According to a second aspect of the present invention, there is provided a process for preparing a modified yellow pigment according to any one of the above, comprising the steps of:
and treating the yellow pigment by using a silane coupling agent and silica sol to obtain the modified yellow pigment.
The preparation method of the modified yellow pigment provided by the invention is simple and efficient in process, and can successfully prepare a target product.
In a preferred embodiment, the present invention provides a preparation method comprising the steps of:
mixing and dispersing water, a silane coupling agent and a yellow pigment, then adding silica sol, adding acid to adjust the pH value to be neutral, curing, then carrying out solid-liquid separation, and carrying out heat treatment on the obtained solid to obtain the modified yellow pigment.
The preparation method provided by the invention is simple and efficient in process, and can successfully prepare the target product.
In a preferred embodiment, the present invention provides a preparation method comprising the steps of:
(a) Pre-shearing water, adding a silane coupling agent and a yellow pigment, mixing and dispersing to obtain slurry;
(b) Adding silica sol into the slurry obtained in the step (a), and adding acid to adjust the pH value to be neutral to obtain a mixed solution;
(c) Curing the mixed solution obtained in the step (b), and then carrying out solid-liquid separation to obtain a solid;
(d) And (c) carrying out heat treatment on the solid obtained in the step (c), cooling and then scattering to obtain a scattered product, and grinding to obtain the modified yellow pigment.
In the step (a), the mass ratio of water, the silane coupling agent and the yellow pigment is 100:1:10-40, in a typical but non-limiting mass ratio of, for example, 100:1: 10. 100:1: 15. 100:1: 20. 100, and (2) a step of: 1: 25. 100:1: 30. 100, and (2) a step of: 1: 35. 100:1:40, which is more favorable for the modification effect of the yellow pigments (pigment brown 24 and pigment yellow 53); the average particle diameter D50 of the slurry obtained in step (a) is between 300nm and 400nm, for example, 300nm, 310nm, 320nm, 330nm, 340nm, 350nm, 360nm, 370nm, 380nm, 390nm and 400nm, but not limited thereto, which is more beneficial to the subsequent modification process and improves the modification effect.
In the step (b), the mass ratio of the silica sol to the silane coupling agent is 40-160:1, typically but not limited to, in a mass ratio of, for example, 40: 1. 50: 1. 60: 1. 70: 1. 80: 1. 90: 1. 100, and (2) a step of: 1. 110: 1. 120: 1. 130: 1. 140: 1. 150: 1. 160:1, the modification effect of pigment brown 24 and pigment yellow 53 is improved; wherein, the silica sol includes but is not limited to sodium type silica sol, which is more beneficial to improving the modification effect of pigment brown 24 and pigment yellow 53; the solid content of the sodium-type silica sol is 45 to 55%, and may be, for example, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, but is not limited thereto, and may be more preferably 50%.
In step (c), the aging time is 5-6h, and typical but not limiting times are 5h and 6h, which are more beneficial to achieve the coating of silica and improve the surface modification effect of the pigment.
In the step (d), the temperature of the heat treatment is 500-1000 ℃, the typical but non-limiting temperature is 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃,1000 ℃, the time of the heat treatment is 3-4h, the typical but non-limiting time is 3h, 3.5h, 4h, and the coating of the silicon dioxide is more favorably realized, and the surface modification effect of the pigment is improved.
In a preferred embodiment, the grinding in step (d) comprises the steps of:
the mixed solution of alcohol and water is firstly pre-sheared, then the dispersant and the scattered product are added to be mixed and dispersed to obtain pre-dispersed product slurry, and then the pre-dispersed product slurry is placed in a grinding machine to be ground until the particle size distribution D90 is between 600 and 800nm, such as 600nm, 650nm, 700nm, 750nm and 800nm, but not limited to, the preparation of the modified yellow pigment is obtained.
It is to be understood that the specific form of the modified yellow pigment preparation obtained by grinding and particle size control in the present invention is not particularly limited, and the modified yellow pigment preparation may be, for example, a pigment-form preparation or a slurry-form preparation, but is not limited thereto.
Among them, the mass ratio of alcohol to water in the mixed solution of alcohol and water is not particularly limited, and may preferably be 1:1, but not limited thereto; the alcohol is not particularly limited, and may be, for example, propylene glycol, but is not limited thereto; the dispersant is not particularly limited, and may be, for example, PL20 dispersant, but is not limited thereto.
In a preferred embodiment, the mass ratio of the mixed solution of alcohol and water, the dispersant and the product after being broken up is 20-30:5-10:60-70, typically but not limited to, in a mass ratio of, for example, 20:10: 70. 25:5: 70. 30:5: 65. 30:10:60, the grinding of the subsequent grinder is facilitated, full grinding is realized, the grinding effect is improved, and a high-quality target product is obtained.
In the present invention, the grinding mill used for grinding includes, but is not limited to, a horizontal type grinding mill, and it is more advantageous to enhance the grinding effect to obtain a preparation of the modified yellow pigment having a target particle size.
A typical preparation method of a modified yellow pigment comprises the following steps:
s1, preparing 100 parts of deionized water in advance, pre-shearing by using a high-speed dispersion machine, slowly adding 1 part of silane coupling agent in a starting dispersion state (500-800 r/min), slowly adding 10-40 parts of pigment (pigment brown 24 or pigment yellow 53), and dispersing at 1500-2000r/min until the average particle size D50 is 300-400nm to obtain slurry;
s2, reducing the shearing speed of the high-speed dispersion machine to 500-800r/min, slowly adding 40-160 parts of silica sol, and adding acid while stirring to adjust the pH value to be neutral to obtain a mixed solution;
s3, continuing to stir the mixed solution obtained in the step S2 for 5-6 hours, curing, filtering, and washing with water to obtain a filter cake;
s4: drying the filter cake, heating at 500-1000 deg.C for 3-4 hr, cooling, and dispersing with jet mill to obtain inorganic composite modified pigment with brown pigment 24 or yellow pigment 53 as core and silica coated surface, and grinding;
s5, grinding:
preparing a mixed solution of 10-15 parts of propylene glycol and 10-15 parts of water in advance, pre-shearing by using a high-speed dispersion machine, slowly adding 5-10 parts of a dispersing agent into 20-30 parts of the mixed solution in a starting dispersion state (500-800 r/min), dispersing for 5min at 1000-1500r/min, then slowly adding 60-70 parts of the inorganic composite modified pigment obtained in the step S4, and dispersing for 15min at 3000r/min to obtain a pre-dispersed product slurry;
and (3) feeding the pre-dispersed product slurry into a horizontal grinder for circular grinding, monitoring the particle size condition all the time, and stopping grinding when the particle size distribution D90 is between 600 and 800nm to obtain a preparation of the modified yellow pigment.
The preparation method provided by the invention has simple and efficient process, can successfully prepare the modified yellow pigment preparation which takes the pigment brown 24 or the pigment yellow 53 as the core and is coated with silicon dioxide on the surface, and the obtained product has higher excellent rate and better and stable quality.
According to a third aspect of the present invention, there is provided a use of a preparation of the modified yellow pigment of any one of the above in a reflective thermal barrier coating.
The application of the modified yellow pigment preparation provided by the invention can enable the reflective heat-insulating coating to meet the requirement on the sunlight reflectance in GB/T25261-2018 standard, and has an outstanding application effect.
The invention is further illustrated by the following examples. The materials in the examples are prepared according to known methods or are directly commercially available, unless otherwise specified.
Example 1
Example 1 provides a modified yellow pigment preparation, specifically a modified yellow pigment preparation having pigment brown 24 (p.br.24) as a core and silica coated on the surface, and having a particle size distribution D90 of 600nm to 800nm.
The preparation of the modified yellow pigment of this example, comprising the steps of:
1. preparing 100 parts of deionized water in advance, pre-shearing by using a high-speed dispersion machine, slowly adding 1 part of silane coupling agent (Mei chart 174) under the condition of starting dispersion (500-800 r/min), slowly adding 10-40 parts of pigment brown 24 (P.Br.24), and dispersing at 1500-2000r/min until the average particle size D50 of the slurry is about 300-400 nm;
2. reducing the shearing speed of a dispersion machine to 500-800r/min, slowly adding 40-160 parts of silica sol (Na type, about 50 percent of solid content), adding acid while stirring, and adjusting the pH value to be neutral;
3. continuously stirring for 5-6 hours, curing, filtering, and washing the filtered filter cake with deionized water;
4. drying the filter cake, heating at 500-1000 deg.C for 3-4 hr, cooling, and grinding with air flow mill to obtain inorganic composite modified pigment with pigment brown 24 as core and coated with silicon dioxide;
5. preparing a mixed solution of 10-15 parts of propylene glycol and 10-15 parts of water in advance, pre-shearing by using a high-speed dispersion machine, slowly adding 5-10 parts of PL20 (Craine) dispersing agent into 20-30 parts of the mixed solution in a starting dispersion state (500-800 r/min), dispersing for 5min at 1000-1500r/min, slowly adding 60-70 parts of the inorganic composite modified pigment obtained in the step 4, dispersing for 15min at 3000r/min, then sending into a horizontal grinding machine (relaxation-resistant LabStart) for circulating grinding, monitoring the particle size condition at any time, and stopping grinding when the particle size distribution D90 is about 600-800nm to obtain a preparation of the modified yellow pigment.
Example 2
Example 2 provides a modified yellow pigment preparation, specifically a modified yellow pigment preparation having a pigment yellow 53 (p.y.53) as a core and silica coated on the surface, and having a particle size distribution D90 of 600nm to 800nm.
The preparation of the modified yellow pigment of this example was prepared by the same method as in example 1 except that pigment yellow 53 (p.y.53) was used in place of pigment brown 24 (p.br.24) of example 1, and the remaining steps and parameters were the same as in example 1.
Comparative example 1
A method of preparing a preparation of pigment brown 24, comprising the steps of:
preparing a mixed solution of 10-15 parts of propylene glycol and 10-15 parts of water in advance, pre-shearing by using a high-speed dispersion machine, slowly adding 5-10 parts of PL20 (Craine) dispersing agent into 20-30 parts of the mixed solution in an open dispersion state (500-800 r/min), dispersing for 5min at 1000-1500r/min, then slowly adding 60-70 parts of pigment brown 24 (P.Br.24), dispersing for 15min at 3000r/min, and then sending into a horizontal grinding machine (relaxation-resistant LabStart) for circulating grinding for 60-120min to finally obtain a preparation of the pigment brown 24 with the particle size distribution D90 of 100-200 nm.
Comparative example 2
A method of preparing a preparation of pigment yellow 53, comprising the steps of:
preparing a mixed solution of 10-15 parts of propylene glycol and 10-15 parts of water in advance, pre-shearing by using a high-speed dispersion machine, slowly adding 5-10 parts of PL20 (Craine) dispersing agent into 20-30 parts of the mixed solution in an open dispersion state (500-800 r/min), dispersing for 5min at 1000-1500r/min, then slowly adding 60-70 parts of pigment yellow 53 (P.Y.53) and dispersing for 15min at 3000r/min, and then sending into a horizontal grinding machine (relaxation-resistant LabStart) to circularly grind for 60-120min to finally obtain a preparation of the pigment yellow 53 with the particle size distribution D90 of 100-200 nm.
Comparative example 3
Colanyl Oxide Yellow R132-CN (inorganic common color paste).
Comparative example 4
Colamyl Yellow 3R 100-CN (organic common color paste).
Test example 1
The preparations of the modified yellow pigments provided in example 1 and example 2 and the products provided in comparative examples 1 to 4 were respectively color-mixed with the Asia BE reflective thermal insulation coating \ BGOM 452 \/18L/24 KG \ white to obtain flat-coating finish paint which is respectively marked as test group 1, test group 2 and comparative test groups 1 to 4, and the L value, the solar light reflectance ratio, the near infrared reflectance ratio, the hemispherical emissivity and the thermal insulation temperature difference of the flat-coating finish paint are tested, and the results are shown in Table 1;
wherein, the testing method of the L value is to use a spectrophotometer to test, GB/T3181-2008, and 3.14 is defined;
the testing method of the solar reflectance ratio is carried out according to the specification of 6.4 in JG/T235-2014;
the testing method of the near infrared reflectance is carried out according to the specification of 6.4 in JG/T235-2014;
the testing method of the hemispherical emissivity is carried out according to the specification of 6.5 in JG/T235-2014;
the testing method of the heat insulation temperature difference is carried out according to the method in GB/T25261-2018 appendix B.
TABLE 1
Figure BDA0003804436590000111
Figure BDA0003804436590000121
The modified yellow pigment preparations provided in examples 1 and 2 and the products provided in comparative examples 1 to 4 were respectively color-matched with the Asia BE reflective thermal insulation coating \ BGOM 452\18L/24KG \ to obtain flat-coating top coats which were respectively marked as test group 1, test group 2 and comparative test groups 1 to 4, and the L value, solar light reflectance, near-infrared reflectance, hemispherical emissivity and thermal insulation temperature difference were measured, and the specific test methods were the same as above, and the results are shown in Table 2.
TABLE 2
Figure BDA0003804436590000122
Figure BDA0003804436590000131
The modified yellow pigment preparations provided in examples 1 and 2 and the products provided in comparative examples 1 to 4 were respectively mixed with a paint for an external wall of a suji painted wall, i.e., 18L/24KG white, to obtain flat-coated finishes, which were respectively identified as test groups 1, 2 and comparative test groups 1 to 4, and tested for L value, solar reflectance, near-infrared reflectance, hemispherical emissivity and thermal insulation temperature difference, the specific test methods are the same as above, and the results are shown in table 3.
TABLE 3
Figure BDA0003804436590000132
The modified yellow pigment preparations provided in examples 1 and 2 and the products provided in comparative examples 1 to 4 were respectively color-mixed with the paint-D type \18L/24KG \ to obtain flat-coating finish paints, which were respectively identified as test groups 1, 2 and comparative test groups 1 to 4, and the L value, solar reflectance, near-infrared reflectance, hemispherical emissivity and thermal insulation temperature difference were measured, and the specific test methods are the same as above, and the results are shown in Table 4.
TABLE 4
Figure BDA0003804436590000141
From the data, the reflection performance of the flat paint obtained by using the reflective thermal insulation coating and the modified yellow pigment provided by the embodiment of the invention meets the requirement of GB/T25261-2018; meanwhile, the reflection performance of the flat paint obtained by using the common coating and the modified yellow pigment provided by the embodiment of the invention is clamped at the standard boundary, so that the reflection performance of the common coating is improved to a certain extent; the reflection performance deviation of the flat-coating finish paint is obtained by using the reflective heat-insulating coating and the common inorganic yellow color paste; although the reflection performance of part of the flat-coating finish paint is excellent, the actual reflection performance (heat insulation temperature difference term) is poor because the particle size of the organic pigment is small, sunlight is mostly transmitted, and the excellence of reflection data is mostly caused by the good performance of the reflection heat insulation paint and the good reflection capability of the substrate.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A modified yellow pigment is characterized in that the modified yellow pigment is a yellow pigment with a surface coated with silicon dioxide;
the yellow pigment includes at least one of pigment brown 24 and pigment yellow 53.
2. The modified yellow pigment of claim 1, wherein the particle size distribution D90 of the modified yellow pigment is between 600 and 800nm.
3. A method for preparing the modified yellow pigment of claim 1 or 2, comprising the steps of:
and treating the yellow pigment by using a silane coupling agent and silica sol to obtain the modified yellow pigment.
4. The method of manufacturing according to claim 3, comprising the steps of:
mixing and dispersing water, a silane coupling agent and the yellow pigment, then adding silica sol, adding acid to adjust the pH value to be neutral, curing, then carrying out solid-liquid separation, and carrying out heat treatment on the obtained solid to obtain the modified yellow pigment.
5. The method of manufacturing according to claim 4, comprising the steps of:
(a) Pre-shearing water, adding a silane coupling agent and the yellow pigment, mixing and dispersing to obtain slurry;
(b) Adding silica sol into the slurry obtained in the step (a), and adding acid to adjust the pH value to be neutral to obtain a mixed solution;
(c) Curing the mixed solution obtained in the step (b), and then carrying out solid-liquid separation to obtain a solid;
(d) And (c) carrying out heat treatment on the solid obtained in the step (c), cooling and then scattering the solid to obtain a scattered product, and grinding the scattered product to obtain the modified yellow pigment.
6. The production method according to claim 5, wherein in the step (a), the mass ratio of water, the silane coupling agent and the yellow pigment is 100:1:10-40;
preferably, the slurry obtained in step (a) has an average particle size D50 between 300 and 400 nm.
7. The production method according to claim 5, wherein in the step (b), the mass ratio of the silica sol to the silane coupling agent is 40 to 160:1;
preferably, the silica sol comprises a sodium type silica sol;
preferably, the sodium silica sol has a solids content of 45 to 55%, preferably 50%.
8. The method according to any one of claims 5 to 7, wherein the temperature of the heat treatment in the step (d) is 500 to 1000 ℃ and the time of the heat treatment is 3 to 4 hours.
9. The method according to any one of claims 5 to 7, wherein the grinding in step (d) comprises the steps of:
pre-shearing a mixed solution of alcohol and water, adding a dispersing agent, mixing with the scattered product, dispersing to obtain pre-dispersed product slurry, and then placing the product slurry into a grinding machine to be ground until the particle size distribution D90 is 600-800nm to obtain the modified yellow pigment;
preferably, the alcohol comprises propylene glycol;
preferably, the dispersant comprises PL20 dispersant;
preferably, the mass ratio of the mixed solution of alcohol and water, the dispersant and the product after scattering is 20-30:5-10:60-70 parts of;
preferably, the mill comprises a horizontal mill.
10. Use of the modified yellow pigment of claim 1 or 2 in a reflective thermal barrier coating.
CN202210992862.1A 2022-08-18 2022-08-18 Modified yellow pigment and preparation method and application thereof Pending CN115160825A (en)

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