CN115572503A - Bonding-free pearlescent pigment for electrostatic powder coating and preparation method thereof - Google Patents

Bonding-free pearlescent pigment for electrostatic powder coating and preparation method thereof Download PDF

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CN115572503A
CN115572503A CN202211186477.4A CN202211186477A CN115572503A CN 115572503 A CN115572503 A CN 115572503A CN 202211186477 A CN202211186477 A CN 202211186477A CN 115572503 A CN115572503 A CN 115572503A
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pearlescent pigment
coating
modified
reactor
bonding
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吴昌梓
吕鹏鹏
林晨
吴昊
吴俊�
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Ruicai Technology Co ltd
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Ruicai Technology Co ltd
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    • 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/36Pearl essence, e.g. coatings containing platelet-like pigments for pearl lustre
    • 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
    • C09C1/0015Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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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
    • C09D5/03Powdery paints
    • C09D5/032Powdery paints characterised by a special effect of the produced film, e.g. wrinkle, pearlescence, matt finish
    • 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • C09D5/033Powdery paints characterised by the additives
    • C09D5/035Coloring agents, e.g. pigments
    • 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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    • 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
    • C09C2220/00Methods of preparing the interference pigments
    • C09C2220/20PVD, CVD methods or coating in a gas-phase using a fluidized bed

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Abstract

The invention discloses a bonding-free pearlescent pigment for electrostatic powder coating and a preparation method thereof, and particularly relates to the technical field of pearlescent pigment production.

Description

Bonding-free pearlescent pigment for electrostatic powder coating and preparation method thereof
Technical Field
The invention relates to the technical field of production of pearlescent pigments, in particular to a bonding-free pearlescent pigment for electrostatic powder coating and a preparation method thereof.
Background
The pearlescent pigment is an optical effect pigment, has the glittering effect of a metal pigment, can generate the soft color of natural pearls, can generate multi-level reflection when being irradiated by sunlight, and presents soft and dazzling or colorful luster and color by the interaction of reflected light.
The mica titanium pearlescent pigment is the pearlescent pigment which is most widely researched and has the most mature technology, and due to the fact that the refractive indexes of titanium dioxide and a mica substrate are different, a good pearlescent effect, a color effect and a visual angle flashing effect are generated through the multiple reflection and interference of light, along with the development of society and economy, people pursue the beauty and color at a higher level, and the industrial development of the pearlescent pigment is very rapid.
The powder coating is a solid powder synthetic resin coating composed of solid resin, pigment, filler, auxiliary agent and the like, compared with common solvent-based coatings and water-based coatings, the dispersion medium of the powder coating is not solvent and water but air, the powder coating is called 4E type coating, has the advantages of high productivity (efficiency), excellent coating performance (excellence), ecological environment protection (ecology) and economy (economy), and the powder coating is rapidly developed as a new technology of the coating industry in recent decades. With the national higher and higher requirements on environmental protection, the change of paint into powder is an inevitable big trend.
Due to the characteristics of pearlescent pigments and powder coatings, it is difficult to prepare composite powder coatings with high pearlescent pigment content using conventional processes because of: the fusion mixing extrusion and high-speed crushing adopted by the traditional powder coating preparation process can damage the structure of the pearlescent pigment and cause that the pearlescent effect cannot be shown, therefore, the pearlescent pigment must be added after the powder coating is prepared, but the charging performance of the mica titanium pearlescent pigment is very poor, the problems of low powdering rate and easy gun blockage are easily caused in the electrostatic spraying process, and finally the problems of uneven distribution of the pearlescent pigment on the surface of a coating film, unstable appearance of the coating film and the like are caused.
The research and development method for preparing the pearlescent powder coating mainly comprises the following steps:
(1) And (3) dry mixing process: the process has the characteristics of simple process and simple equipment, but the pearly-lustre pigment particles after dry mixing cannot be adhered with the powder coating particles, so the electrostatic spraying effect is poor, and patents represented by CN103160181A and CN111617721A exist.
(2) Bonding method: the process comprises a special mixing procedure for solving the problem of adhesion between the powder coating and the pearlescent pigment, so that the pearlescent powder coating prepared by the bonding method has more stable performance. The bonding process specifically comprises the steps of preheating the powder coating to the softening point of the powder coating, and then adding the pearlescent pigment to adhere the pearlescent pigment and the powder coating particles together, so that two particles cannot be separated in electrostatic spraying, and the spraying effect is stable, and the technique is the mainstream technique for preparing pearlescent powder coatings at present and represents patents such as CN105273583B, CN108102506A, CN108841299A, CN111560209A and the like.
However, because the orientation of the pearlescent particles adhered to the surface of each particle of the powder coating is different, and the pearlescent effect of the pearlescent pigment is related to the flaky plane direction of the pearlescent pigment, the electrostatic spraying effect of the pearlescent powder coating prepared by the bonding process cannot achieve the optimal gloss effect of the pearlescent pigment, and in addition, the bonding process also has the problem that too much pearlescent pigment cannot be bonded, and is not suitable for preparing the powder coating with high pearlescent content.
(3) Other processes comprise: the process for preparing the pearlescent powder coating by hot-melting and mixing the powder coating and the pearlescent pigment (CN 108112257B, CN112724798A and CN 112724804A) and the process for spraying after mixing the pearlescent powder and the powder coating (CN 101302366B).
The process mainly focuses on improving the effect of mixing/bonding two kinds of powder in the mixing process of the pearlescent pigment and the powder coating, because the pearlescent characteristic of the pearlescent pigment is related to the direction of a flaky plane of the pearlescent pigment, the process cannot give full play to the optimal gloss effect of the pearlescent pigment, powder surface modification is carried out on the pearlescent pigment, the problems of the electrostatic spraying process are improved, theoretically, better application effects can be obtained, and patents CN111518419A, CN107400383B, CN107400394B, CN113248944A and CN105860593B propose that the surface treatment is carried out on the pearlescent pigment by adopting a liquid-phase surface coating modification process, the prepared modified pearlescent pigment is directly used for the powder coating.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a bonding-free pearlescent pigment for electrostatic powder coating and a preparation method thereof, and the technical problems to be solved by the invention are as follows: the preparation method of the pearlescent pigment in the prior art is difficult to solve the problems when the pearlescent pigment is used for electrostatic spraying, and the prepared pearlescent pigment has the problem of poor luster effect.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a exempt from to bind pearl pigment for electrostatic powder coating, exempt from to bind pearl pigment including modified pearl pigment body and cladding in the modified pearl pigment body surface's nanometer silica modified layer, modified pearl pigment includes modified pearl pigment body and cladding in the coating of the tin oxide and the titanium dioxide on pearl pigment body surface.
As a further scheme of the invention: the pearlescent pigment body comprises one or more of natural mica substrate pearlescent pigment, synthetic mica substrate pearlescent pigment, silica substrate pearlescent pigment and alumina substrate pearlescent pigment.
The particle size of the pearlescent pigment is 5-125 μm, preferably, the particle size of the pearlescent pigment is 10-60 μm.
The diameter-thickness ratio of the pearlescent pigment is more than or equal to 50.
As a further scheme of the invention: the thickness of the nano silicon dioxide modified layer is 1-30 nm, and preferably, the thickness of the nano silicon dioxide modified layer is 5-10 nm.
The coating rate of the nano silicon dioxide modified layer is 0.1-10%, and preferably, the coating rate of the nano silicon dioxide modified layer is 1-3%.
The coating layers of the tin oxide and the titanium dioxide comprise three tin oxide coating layers and three titanium dioxide coating layers, and the three tin oxide coating layers and the three titanium dioxide coating layers are alternately arranged.
The coating rate of the tin oxide coating layer is 1-3%, preferably, the coating rate of the tin oxide coating layer is 2%, the coating rate of the titanium dioxide coating layer is 10-50%, preferably, the coating rate of the titanium dioxide coating layer is 20-45%.
A preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, the pearlescent pigment body is used as a base material and placed in a reactor, control parameters are adjusted to enable the pearlescent pigment body powder to be in a continuous motion state, tin oxide is evenly sprayed into the reactor through an atomizing nozzle, and the reaction is continued for a period of time to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into the reactor through an atomizing nozzle after coating is finished, continuously reacting for a period of time to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material as a base material in the reactor, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at high temperature and calcining at ultrahigh temperature to obtain the modified pearlescent pigment body.
And S3, setting the reactor again, heating to a certain temperature, keeping a constant temperature state, putting the modified pearlescent pigment body powder into the reactor, and adjusting the control parameters to enable the modified pearlescent pigment body powder to be in a continuous motion state in the reactor.
And S4, uniformly spraying the precursor into a reactor through an atomizing nozzle, fully contacting the precursor with the modified pearlescent pigment body powder, reacting for a certain reaction time, and taking out the modified bonding-free pearlescent pigment after the reactor is cooled.
As a further scheme of the invention: the precursor is one or a mixture of more of tetraethoxysilane, silica sol and silane coupling agent.
As a further scheme of the invention: the reactor is one of a fluidized bed, a vibrating bed and a rotary furnace.
The operating gas for the reactor is a mixture of one or more of nitrogen, argon and air.
The operating gas velocity of the fluidized bed is 0.05-0.5 m/s.
The vibration knocking frequency of the vibration bed is 60-300 times/min.
As a further scheme of the invention: the rotation speed of the rotary furnace is 5-60 r/min.
The high-temperature drying temperature is 120-130 ℃.
The high-temperature calcination temperature is 800-900 ℃.
As a further scheme of the invention: the modification chemical reaction temperature is 200-700 ℃, preferably 300-500 ℃, and 300-500 ℃.
The duration time of the modification chemical reaction is 1-30 min, and preferably, the duration time of the modification chemical reaction is 5-15 min.
The invention has the beneficial effects that:
1. according to the invention, the nano silicon dioxide is modified by in-situ deposition, the content is controllable, the nano silicon dioxide can be uniformly and completely coated on the surface of the modified pearlescent pigment body, the powdering rate and the spraying effect of the pearlescent pigment used in the electrostatic spraying process of the powder coating are improved, the tin oxide and the titanium dioxide are coated on the surface of the pearlescent pigment body, various magic hues and gloss are created by selectively reflecting, refracting and transmitting various color rays with different wavelengths in natural light, the gloss, brightness and saturation of the surface of the pearlescent pigment body can be greatly improved, the pearlescent pigment can be directly used in the powder coating application, the flaky pearlescent pigment can be formed into a film by electrostatic spraying, the flaky orientation is consistent with the film, the pearlescent effect of the pearlescent pigment is maximized, and the problem that the pearlescent effect is influenced by different bonding orientations of the pearlescent pigment in the existing bonding process is solved.
2. The content of the modified pearlescent pigment added into the powder coating is not controlled, the addition amount of the pearlescent pigment can be adjusted at will according to the coating effect, and the problem that the pearlescent pigment cannot be bonded too much in the existing bonding process is solved.
3. The pearlescent pigment is subjected to surface coating treatment by adopting a vapor deposition technology, the modification process is simple, the economy is good, the environment is protected, and the problems of poor batch stability and fussy waste liquid treatment existing in the conventional liquid phase coating process are solved.
Drawings
FIG. 1 is a microscopic schematic view of a bonding-free pearlescent pigment provided by the present invention;
FIG. 2 is a schematic flow chart of the preparation of the bonding-free pearlescent pigment of the present invention;
FIG. 3 is a schematic flow chart of the bulk preparation of the modified pearlescent pigment of the present invention;
FIG. 4 is a schematic flow chart of the preparation of the nano-silica modified layer according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1:
as shown in fig. 1, the bonding-free pearlescent pigment for electrostatic powder coating comprises a modified pearlescent pigment body and a nano-silica modified layer coated on the surface of the modified pearlescent pigment body, wherein the modified pearlescent pigment comprises the modified pearlescent pigment body and a coating layer of tin oxide and titanium dioxide coated on the surface of the pearlescent pigment body.
The pearlescent pigment body is a mixture of natural mica substrate pearlescent pigment, synthetic mica substrate pearlescent pigment, silica substrate pearlescent pigment and alumina substrate pearlescent pigment.
The particle size of the pearlescent pigment was 15 μm.
The diameter-thickness ratio of the pearlescent pigment is more than or equal to 50.
The coating layers of the tin oxide and the titanium dioxide comprise three layers of tin oxide coating layers and three layers of titanium dioxide coating layers, and the three layers of tin oxide coating layers and the three layers of titanium dioxide coating layers are alternately arranged.
As shown in fig. 2 to 4, a method for preparing a bonding-free pearlescent pigment for electrostatic powder coating includes the following steps:
s1, the pearlescent pigment body is used as a base material and placed in a reactor, control parameters are adjusted to enable the pearlescent pigment body powder to be in a continuous motion state, tin oxide is evenly sprayed into the reactor through an atomizing nozzle, and the reaction is continued for a period of time to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into the reactor through an atomizing nozzle after coating, continuously reacting for a period of time to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material as a base material in the reactor, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at high temperature and calcining at ultrahigh temperature to obtain the modified pearlescent pigment body.
And S3, setting the reactor again, heating to a certain temperature, maintaining the constant temperature state, putting the modified pearlescent pigment body powder into the reactor, and adjusting the control parameters to enable the modified pearlescent pigment body powder to be in a continuous motion state in the reactor.
And S4, uniformly spraying the precursor into the reactor through an atomizing nozzle, fully contacting the precursor with the modified pearlescent pigment body powder, reacting for a certain reaction time, and taking out the modified bonding-free pearlescent pigment after the reactor is cooled.
The precursor is tetraethoxysilane.
The reactor is a fluidized bed.
The operating gas for the reactor was argon.
The operating gas velocity of the fluidized bed was 0.3m/s.
The temperature for high-temperature drying is 126 ℃.
The temperature of the high-temperature calcination was 850 ℃.
The modification chemical reaction temperature is 350 ℃ and the modification chemical reaction temperature is 360 ℃.
The duration of the modification chemical reaction is 15min.
The prepared bonding-free pearlescent pigment is found by analysis and characterization, the coating rate of the nano silicon dioxide modified layer is 3%, the thickness of the nano silicon dioxide modified layer is 5nm, the coating rate of the tin oxide coating layer is 2%, and the coating rate of the titanium dioxide coating layer is 40%, and the obtained bonding-free pearlescent pigment can create various magic hues and glosses by means of selective reflection, refraction and transmission of various colors of light with different wavelengths in natural light, so that the glossiness, the brightness and the saturation of the surface of the pearlescent pigment body can be greatly improved.
Example 2:
a preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, selecting natural mica substrate pearlescent pigment with the particle size of 5 microns and the diameter-thickness ratio of more than or equal to 50 as a substrate, placing the substrate in a fluidized bed reactor at 150 ℃, taking nitrogen as operating gas of the fluidized bed reactor, adjusting operating parameters to enable pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the fluidized bed reactor through an atomizing nozzle, and continuously reacting for 15min to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into the fluidized bed reactor through an atomizing nozzle after coating, continuously reacting for 15min to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material in the fluidized bed reactor by taking the material as a base material, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at the high temperature of 130 ℃ and calcining at the ultrahigh temperature of 850 ℃ to obtain the modified pearlescent pigment body.
And S3, setting the fluidized bed reactor again, heating to 200 ℃, maintaining the constant temperature state, putting the modified pearlescent pigment body powder into the fluidized bed reactor, taking nitrogen as the operating gas of the fluidized bed reactor, and adjusting the operation parameters to enable the pearlescent pigment body powder to be in a continuous motion state, wherein the operating gas speed is 0.05 m/S.
And S4, uniformly spraying the precursor ethyl orthosilicate into the fluidized bed reactor through an atomizing nozzle, fully contacting with the pearlescent pigment body powder, reacting for 1min for a certain reaction time, cooling the fluidized bed reactor, and taking out the modified bonding-free pearlescent pigment.
Analysis and characterization show that the thickness of the nano silicon dioxide modified layer is 1nm, the coating rate is 0.1%, the coating rate of the tin oxide coating layer is 2%, and the coating rate of the titanium dioxide coating layer is 40%, and the obtained bonding-free pearlescent pigment can selectively reflect, refract and transmit various light rays with different wavelengths in natural light to create various magic hues and glosses, so that the glossiness, the brightness and the saturation of the surface of the pearlescent pigment body can be greatly improved.
Example 3:
a preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, selecting natural mica substrate pearlescent pigment with the particle size of 125 microns and the diameter-thickness ratio of more than or equal to 60 as a substrate, placing the substrate in a vibrating bed reactor at 360 ℃, using argon as operating gas of the vibrating bed reactor, wherein the operating gas speed is 0.06m/S, the vibration knocking frequency of the vibrating bed reactor is 60 times/min, adjusting operating parameters to enable the pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the vibrating bed reactor through an atomizing nozzle, and continuously reacting for 15min to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body to form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into the vibrating bed reactor through an atomizing nozzle after coating, continuously reacting for 15min to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material in the vibrating bed reactor by taking the material as a base material, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at the high temperature of 130 ℃ and calcining at the ultrahigh temperature of 850 ℃ to obtain the modified pearlescent pigment body.
And S3, setting the vibrating bed reactor again, heating to 700 ℃, keeping the constant temperature state, putting the modified pearlescent pigment body powder into the vibrating bed reactor, taking argon as operating gas of the vibrating bed reactor, and adjusting the operation parameters to enable the pearlescent pigment body powder to be in a continuous motion state, wherein the operating gas speed is 0.05 m/S.
And S4, uniformly spraying the precursor silica sol into the vibrating bed reactor through an atomizing nozzle, fully contacting with the pearlescent pigment body powder, reacting for 30min, and taking out the modified bonding-free pearlescent pigment after cooling the vibrating bed reactor.
The prepared bonding-free pearlescent pigment is analyzed and characterized, and the thickness of the nano silicon dioxide modified layer is 30nm, the coating rate is 10%, the coating rate of the tin oxide coating layer is 3%, and the coating rate of the titanium dioxide coating layer is 45%.
Example 4:
a preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, selecting natural mica substrate pearlescent pigment with the particle size of 25 microns and the diameter-thickness ratio of more than or equal to 70 as a substrate, placing the substrate in a fluidized bed reactor at 280 ℃, taking air as operating gas of the fluidized bed reactor, adjusting operating parameters to enable pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the fluidized bed reactor through an atomizing nozzle, and continuously reacting for 13min to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into the fluidized bed reactor through an atomizing nozzle after coating, continuously reacting for 15min to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material in the fluidized bed reactor by taking the material as a base material, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at the high temperature of 125 ℃ and calcining at the ultrahigh temperature of 860 ℃ to obtain the modified pearlescent pigment body.
And S3, setting the fluidized bed reactor again, heating to 600 ℃, maintaining the constant temperature state, putting the modified pearlescent pigment body powder into the fluidized bed reactor, taking air as operating gas of the fluidized bed reactor, and adjusting the operation parameters to enable the pearlescent pigment body powder to be in a continuous motion state, wherein the operating gas speed is 0.5m/S.
And S4, uniformly spraying the precursor coupling agent into the fluidized bed reactor through an atomizing nozzle, fully contacting the precursor coupling agent with the pearlescent pigment body powder, reacting for 15min, and taking out the modified bonding-free pearlescent pigment after the fluidized bed reactor is cooled.
Analysis and characterization show that the prepared bonding-free pearlescent pigment has the thickness of a nano silicon dioxide modified layer of 12nm, the coating rate of 3%, the coating rate of a tin oxide coating layer of 2.5% and the coating rate of a titanium dioxide coating layer of 38%.
Example 5:
a preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, selecting natural mica substrate pearlescent pigment with the particle size of 60 microns and the diameter-thickness ratio of more than or equal to 100 as a substrate, placing the substrate in a vibrating bed reactor at 130 ℃, wherein the vibrating knocking frequency of the vibrating bed reactor is 300 times/min, argon is used as operating gas of the vibrating bed reactor, the operating gas speed is 0.1m/S, adjusting operating parameters to enable the pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the vibrating bed reactor through an atomizing nozzle, and continuously reacting for 18min to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body to form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into the vibrating bed reactor through an atomizing nozzle after coating is finished, continuously reacting for 15min to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body to form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material as a base material in the vibrating bed reactor, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at the high temperature of 120 ℃ and calcining at the ultrahigh temperature of 830 ℃ to obtain the modified pearlescent pigment body.
And S3, setting the vibrating bed reactor again, heating to 400 ℃, keeping the constant temperature state, putting the modified pearlescent pigment body powder into the vibrating bed reactor, taking argon as operating gas of the vibrating bed reactor, and adjusting the control parameters to enable the pearlescent pigment body powder to be in a continuous motion state, wherein the operating gas speed is 0.1 m/S.
And S4, uniformly spraying the precursor silica sol into a vibrating bed reactor through an atomizing nozzle, fully contacting the precursor silica sol with the pearlescent pigment body powder, reacting for 20min, and taking out the modified bonding-free pearlescent pigment after the vibrating bed reactor is cooled.
Analysis and characterization show that the thickness of the nano silicon dioxide modified layer is 15nm, the coating rate is 4%, the coating rate of the tin oxide coating layer is 2.9%, and the coating rate of the titanium dioxide coating layer is 42%.
Example 6:
a preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, selecting natural mica substrate pearlescent pigment with the particle size of 20 microns and the diameter-thickness ratio of more than or equal to 50 as a substrate, placing the substrate in a rotary furnace reactor at the temperature of 126 ℃, controlling the rotation speed of the rotary furnace reactor to be 5r/min, using air as operating gas of the rotary furnace reactor, controlling the operating parameters to enable the pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the rotary furnace reactor through an atomizing nozzle, and continuously reacting for 26min to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into a rotary furnace reactor through an atomizing nozzle after coating, continuously reacting for 20min to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material in the rotary furnace reactor by using the material as a base material, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying the material at a high temperature of 128 ℃ and calcining the material at an ultrahigh temperature of 870 ℃ to obtain the modified pearlescent pigment body.
And S3, setting the rotary furnace reactor again, heating to 450 ℃, maintaining the constant temperature state, putting the modified pearlescent pigment body powder into the rotary furnace reactor, taking air as operating gas of the rotary furnace reactor, controlling the operating gas speed to be 0.3m/S, and adjusting the control parameters to enable the pearlescent pigment body powder to be in a continuous motion state.
And S4, uniformly spraying ethyl orthosilicate into the rotary furnace reactor through an atomizing nozzle, fully contacting the ethyl orthosilicate with the pearlescent pigment body powder, reacting for 30min, cooling the rotary furnace reactor, and taking out the modified bonding-free pearlescent pigment.
The prepared bonding-free pearlescent pigment is analyzed and characterized, and the thickness of the nano silicon dioxide modified layer is 5nm, the coating rate is 1%, the coating rate of the tin oxide coating layer is 1.2%, and the coating rate of the titanium dioxide coating layer is 36%.
Example 7:
a preparation method of a bonding-free pearlescent pigment for electrostatic powder coating comprises the following steps:
s1, selecting natural mica substrate pearlescent pigment with the particle size of 10 microns and the diameter-thickness ratio of more than or equal to 100 as a substrate, placing the substrate in a rotary furnace reactor at 200 ℃, controlling the rotation speed of the rotary furnace reactor to be 60r/min, using air as operating gas of the rotary furnace reactor, controlling the operating gas speed to be 0.4m/S, adjusting the operating parameters to enable the pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the rotary furnace reactor through an atomizing nozzle, and continuously reacting for 3min to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer.
And S2, uniformly spraying titanium dioxide into a rotary furnace reactor through an atomizing nozzle after coating, continuously reacting for 8min to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material in the rotary furnace reactor by using the material as a base material, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at the high temperature of 120 ℃ and calcining at the ultrahigh temperature of 820 ℃ to obtain the modified pearlescent pigment body.
And S3, setting the rotary furnace reactor again, heating to 450 ℃, keeping the constant temperature state, placing the modified pearlescent pigment body powder into the rotary furnace reactor, taking air as operating gas of the rotary furnace reactor, and adjusting the control parameters to enable the pearlescent pigment body powder to be in a continuous motion state, wherein the operating gas speed is 0.4 m/S.
And S4, uniformly spraying tetraethoxysilane into the rotary furnace reactor through an atomizing nozzle, fully contacting the tetraethoxysilane with the pearlescent pigment body powder, reacting for 5min, and taking out the modified bonding-free pearlescent pigment after the rotary furnace reactor is cooled.
The prepared bonding-free pearlescent pigment is analyzed and characterized, and the thickness of the nano silicon dioxide modified layer is 3nm, the coating rate is 0.8%, the coating rate of the tin oxide coating layer is 1.1%, and the coating rate of the titanium dioxide coating layer is 10%.
In conclusion, the modified bonding-free pearlescent pigment prepared by the preparation method of the bonding-free pearlescent pigment for electrostatic powder coating can greatly improve the glossiness, brightness and saturation of the surface of the pearlescent pigment body, can be directly used for powder coating application, can be formed into a film by electrostatic spraying, has the same orientation as the film, can maximize the pearlescent effect of the pearlescent pigment, can be uniformly and completely coated on the surface of the modified pearlescent pigment body, and improves the powdering rate and spraying effect of the pearlescent pigment in the electrostatic spraying process of the powder coating.
The nano silicon dioxide is modified by in-situ deposition, the content is controllable, the nano silicon dioxide can be uniformly and completely coated on the surface of the modified pearlescent pigment body, the powdering rate and the spraying effect of the pearlescent pigment used in the electrostatic spraying process of powder coating are improved, various magic hues and gloss are created by carrying out selective reflection, refraction and transmission on various color light rays with different wavelengths in natural light by coating tin oxide and titanium dioxide on the surface of the pearlescent pigment body, the gloss, brightness and saturation of the surface of the pearlescent pigment body can be greatly improved, and the problem that the gloss effect is influenced by different bonding orientations of the pearlescent pigment in the conventional bonding process is solved.
Meanwhile, the content of the modified pearlescent pigment added into the powder coating is not controlled, the addition amount of the pearlescent pigment can be adjusted at will according to the coating effect, the problem that the pearlescent pigment cannot be bonded too much in the existing bonding process is solved, the surface coating treatment is carried out on the pearlescent pigment by adopting a vapor deposition technology, the modification process is simple, the economy is good, the environment is protected, and the problems of poor batch stability and fussy waste liquid treatment in the existing liquid phase coating process are solved.
The points to be finally explained are: although the present invention has been described in detail with reference to the general description and the specific embodiments, on the basis of the present invention, the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting 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 the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A bonding-free pearlescent pigment for electrostatic powder coating is characterized in that: the bonding-free pearlescent pigment comprises a modified pearlescent pigment body and a nano silicon dioxide modified layer coated on the surface of the modified pearlescent pigment body, and the modified pearlescent pigment comprises the modified pearlescent pigment body and a coating layer coated on the surface of the pearlescent pigment body and containing tin oxide and titanium dioxide.
2. A bonding-free pearlescent pigment for electrostatic powder coatings according to claim 1, characterized in that: the pearlescent pigment body comprises one or a mixture of natural mica substrate pearlescent pigment, synthetic mica substrate pearlescent pigment, silicon dioxide substrate pearlescent pigment and alumina substrate pearlescent pigment;
the particle size of the pearlescent pigment is 5-125 μm;
the diameter-thickness ratio of the pearlescent pigment is more than or equal to 50.
3. A bonding-free pearlescent pigment for electrostatic powder coatings according to claim 1, characterized in that: the thickness of the nano silicon dioxide modified layer is 1-30 nm;
the coating rate of the nano silicon dioxide modified layer is 0.1-10%;
the coating layers of the tin oxide and the titanium dioxide comprise three tin oxide coating layers and three titanium dioxide coating layers, and the three tin oxide coating layers and the three titanium dioxide coating layers are alternately arranged;
the coating rate of the tin oxide coating layer is 1-3%, and the coating rate of the titanium dioxide coating layer is 10-50%.
4. A method for preparing a bonding-free pearlescent pigment for electrostatic powder coating according to any one of claims 1-3, comprising the steps of:
s1, placing a pearlescent pigment body serving as a base material in a reactor, adjusting control parameters to enable the pearlescent pigment body powder to be in a continuous motion state, uniformly spraying tin oxide into the reactor through an atomizing nozzle, and continuously reacting for a period of time to enable the tin oxide to be fully contacted with the surface of the pearlescent pigment body and form a tin oxide coating layer;
s2, uniformly spraying titanium dioxide into a reactor through an atomizing nozzle after coating, continuously reacting for a period of time to enable the titanium dioxide to be fully contacted with the surface of the pearlescent pigment body and form a titanium dioxide coating layer, washing the obtained material to be clean, placing the material as a base material in the reactor, repeating the steps until three tin oxide coating layers and three titanium dioxide coating layers are formed on the surface of the pearlescent pigment body, washing the material to be clean again, and then drying at high temperature and calcining at ultrahigh temperature to obtain a modified pearlescent pigment body;
s3, setting the reactor again, heating to a certain temperature, maintaining the constant temperature state, putting the modified pearlescent pigment body powder into the reactor, and adjusting the control parameters to enable the modified pearlescent pigment body powder to be in a continuous motion state in the reactor;
and S4, uniformly spraying the precursor into a reactor through an atomizing nozzle, fully contacting the precursor with the modified pearlescent pigment body powder, reacting for a certain reaction time, and taking out the modified bonding-free pearlescent pigment after the reactor is cooled.
5. The bonding-free pearlescent pigment for electrostatic powder coating and the preparation method thereof according to claim 4, characterized in that: the precursor is one or a mixture of more of tetraethoxysilane, silica sol and silane coupling agent.
6. The bonding-free pearlescent pigment for electrostatic powder coating and the preparation method thereof according to claim 4, characterized in that: the reactor is one of a fluidized bed, a vibrating bed and a rotary furnace;
the operation gas of the reactor is one or more of nitrogen, argon and air;
the operating gas velocity of the fluidized bed is 0.05-0.5 m/s;
the vibration knocking frequency of the vibration bed is 60-300 times/min.
7. The bonding-free pearlescent pigment for electrostatic powder coating and the preparation method thereof according to claim 4, characterized in that: the rotation speed of the rotary furnace is 5-60 r/min;
the temperature for high-temperature drying is 120-130 ℃;
the high-temperature calcination temperature is 800-900 ℃.
8. The bonding-free pearlescent pigment for electrostatic powder coating and the preparation method thereof according to claim 4, characterized in that: the temperature of the modification chemical reaction is 200-700 ℃, and the temperature of the modification chemical reaction is 300-500 ℃;
the duration of the modification chemical reaction is 1-30 min.
CN202211186477.4A 2022-09-27 2022-09-27 Bonding-free pearlescent pigment for electrostatic powder coating and preparation method thereof Pending CN115572503A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116445011A (en) * 2023-04-10 2023-07-18 瑞彩科技股份有限公司 Bonding-free pearlescent pigment for electrostatic powder coating and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116445011A (en) * 2023-04-10 2023-07-18 瑞彩科技股份有限公司 Bonding-free pearlescent pigment for electrostatic powder coating and preparation method thereof

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