CN115353753A - Infrared reflection cobalt green pigment and preparation process thereof - Google Patents
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Abstract
The invention belongs to the technical field of reflective pigment coating, and particularly relates to an infrared reflective cobalt green pigment and a preparation process thereof. The product developed by the invention comprises a 1# cobalt green pigment, wherein the 1# cobalt green pigment is composed of hollow glass beads and a cobalt green pigment layer loaded on the surfaces of the hollow glass beads; the 2# cobalt green pigment is composed of graphene oxide and cobalt green pigment layers loaded between the graphene oxide layers; during preparation, mixing the mixed solution with polyethylene glycol, adding a sodium carbonate solution and hollow glass beads, carrying out hydrothermal reaction, filtering, washing and drying, carrying out high-temperature calcination, cooling and discharging to obtain a No. 1 cobalt green pigment; and mixing the mixed solution with the nano styrene-acrylic emulsion, adding graphene oxide, performing ultrasonic dispersion uniformly, adding a sodium carbonate solution, performing hydrothermal reaction, performing suction filtration, washing and drying, calcining at high temperature under the protection of inert gas, cooling, and discharging to obtain the 2# cobalt green pigment.
Description
Technical Field
The invention belongs to the technical field of reflective pigments. More particularly, relates to an infrared reflection cobalt green pigment and a preparation process thereof.
Background
Cobalt green is a pigment with a distinct yellow-light green color and a vivid hue. Compared with other green pigments, the red pigment has better heat resistance, light resistance, acid resistance, alkali resistance and high infrared reflectivity, and is nontoxic. Therefore, in some application fields requiring super durability, particularly in the fields of high color retention, gloss retention and chalking resistance, it is often necessary to use such pigments. According to the structure and color development mechanism of the cobalt green pigment, other metal ions with similar atomic radii can be doped in the preparation of the cobalt green pigment to change CO 2+ The coordination state of the cobalt green pigment can change the hue of the cobalt green pigment, so that a series of modified cobalt green pigments can be formed, the application performance of the cobalt green pigment is improved, and the application field of the cobalt green pigment is expanded.
The conventional preparation method of cobalt pigments is a solid phase method. However, the solid-phase reaction method has high energy consumption, the reaction speed is influenced by diffusion kinetics, the physicochemical reaction is not easy to be fully carried out, the prepared pigment has uneven particle size distribution, the color and the chemical stability of the pigment are poor, and the application performance of the pigment has certain defects. The liquid-phase coprecipitation method is to mix the reactants evenly in the liquid phase, the reactants can react fully, the prepared pigment has small granularity and high purity, the calcination temperature is lower than that of the solid-phase reaction and is easy to control, and the high-temperature stability and the chemical stability are good.
Disclosure of Invention
The invention aims to solve the technical problem that the existing cobalt green pigment can only reflect or refract light by the pigment per se in the actual use process, so that the defect and the defect that the performance bottleneck of the material per se is difficult to further break through are overcome, and the infrared reflection cobalt green pigment and the preparation process thereof are provided.
The invention aims to provide an infrared reflection cobalt green pigment.
The invention also aims to provide a preparation process of the infrared reflection cobalt green pigment.
The above purpose of the invention is realized by the following technical scheme:
an infrared-reflective cobalt green pigment comprising:
the 1# cobalt green pigment is composed of hollow glass beads and a cobalt green pigment layer loaded on the surfaces of the hollow glass beads;
the 2# cobalt green pigment is composed of graphene oxide and cobalt green pigment layers loaded between the graphene oxide layers;
the D50 of the hollow glass bead is 10-15 mu m;
the D50 of the graphene oxide is 1-3 μm;
the mass ratio of the No. 1 cobalt green pigment to the No. 2 cobalt green pigment is 1:3-1:5.
further, the particle size distribution range of the hollow glass beads is 5-20 μm, and the particle size distribution range of the graphene oxide is 0.5-4 μm.
According to the technical scheme, the hollow glass beads with spherical structures are selected, the cobalt green pigment is loaded on the surfaces of the hollow glass beads to serve as the No. 1 cobalt green pigment, and the graphene oxide with a layered structure is utilized to load the cobalt green pigment between the layers of the hollow glass beads to serve as the No. 2 cobalt green pigment;
the 1# cobalt green pigment can utilize the reflection and refraction effects of the spherical glass beads and the interface between the spherical glass beads and the cobalt green pigment adsorbed on the surface of the spherical glass beads to strengthen the reflection and refraction effects of the pigment; meanwhile, the particle size of the spherical glass beads is larger than that of the layered graphene oxide, and the density of the spherical glass beads is larger, so that a part of graphene oxide can be clamped at the interfaces of different glass beads, and a part of graphene oxide is distributed on the surface of the whole coating.
Further, the cobalt green pigment layer is a continuous cobalt green pigment layer.
Furthermore, spherical porous carbon is distributed at intervals in the 2# cobalt green pigment layer.
A preparation process of an infrared reflection cobalt green pigment comprises the following specific preparation steps:
preparing raw materials:
according to the molar ratio of the cobalt, the zinc and the chromium being 0.5-1.0:0.1-0.3:1.5-2.0, preparing a cobalt sulfate solution, a zinc sulfate solution and a chromium nitrate solution, and uniformly mixing the cobalt sulfate solution, the zinc sulfate solution and the chromium nitrate solution to obtain a mixed solution;
preparation of 1# cobalt green pigment:
mixing the mixed solution with polyethylene glycol according to a mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding 30-50% by mass of a sodium carbonate solution with the mass fraction of 10-20% and hollow glass beads with the mass fraction of 1.0-1.5 times that of the mixture, carrying out hydrothermal reaction, filtering, washing and drying, carrying out high-temperature calcination, cooling and discharging to obtain the No. 1 cobalt green pigment;
preparation of No. 2 cobalt green pigment:
mixing the mixed solution with the nano styrene-acrylic emulsion according to a mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide accounting for 60-80% of the mass of the mixed solution, performing ultrasonic dispersion uniformly, adding a sodium carbonate solution accounting for 30-50% of the mass of the mixed solution and accounting for 10-20% of the mass of the mixed solution, performing hydrothermal reaction, performing suction filtration, washing and drying, calcining at high temperature under the protection of inert gas, cooling, and discharging to obtain a 2# cobalt green pigment;
and mixing the obtained 1# cobalt green pigment and 2# cobalt green pigment according to a mass ratio of 1:3-1:5, uniformly mixing to obtain the product.
Above-mentioned technical scheme is through in 2# cobalt green pigment preparation process, add nanometer styrene-acrylic emulsion, nanometer styrene-acrylic emulsion can adsorb the fixed precursor crystal that deposits and form, and effectively fix it between the oxidation graphite alkene layer after the dispersion, form continuous pigment layer, the high temperature effect of in-process is calcined in the cooperation again, styrene-acrylic emulsion microballon carbonization forms spherical hollow carbon gradually, thus, can effectively enrich the porosity in the continuous pigment layer, when reducing 2# cobalt green pigment's density, through the existence in this hole, make and form the interface between the pigment granule of difference, the infrared reflection effect on its surperficial continuous pigment layer has effectively been promoted.
Further, the polyethylene glycol is selected from any one of PEG-200, PEG-400 or PEG-600.
Further, the solid content of the nano styrene-acrylic emulsion is 30-35%.
Further, the high-temperature calcination is as follows: heating to 1250-1350 ℃ at the speed of 3-8 ℃/min, and then carrying out heat preservation and calcination for 30-45min.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
Preparing raw materials:
according to the molar ratio of cobalt, zinc and chromium of 0.5:0.1:1.5, preparing a cobalt sulfate solution with the mass fraction of 10%, a zinc sulfate solution with the mass fraction of 10% and a chromium nitrate solution with the mass fraction of 15%, mixing, and stirring and mixing for 40min by using a stirrer at the stirring rotating speed of 400r/min to obtain a mixed solution;
preparation of 1# cobalt green pigment:
and (3) mixing the mixed solution with polyethylene glycol according to a mass ratio of 5:1, mixing and pouring the mixture into a reaction kettle, adding a sodium carbonate solution with the mass fraction of 10 percent and hollow glass beads with the mass fraction of 1.0 time of the mixture, wherein the mass fraction of the sodium carbonate solution is 30 percent of the mass of the mixture, carrying out hydrothermal reaction for 3 hours at the temperature of 120 ℃ and the stirring speed of 400r/min, filtering, collecting a filter cake, washing the filter cake with deionized water until the washing liquid is neutral, transferring the washed filter cake into a drying oven, drying the filter cake to constant weight at the temperature of 100 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating the dried filter cake to 1250 ℃ at the speed of 3 ℃/min, carrying out heat preservation and calcination for 30min, cooling the dried filter cake to room temperature along with the furnace, and discharging to obtain the 1# cobalt green pigment;
wherein the particle size distribution range of the hollow glass beads is 5-20 μm, and the D50 is 10 μm;
the polyethylene glycol is selected from PEG-200;
preparation of # 2 cobalt green pigment:
mixing the mixed solution with a nano styrene-acrylic emulsion with a solid content of 30% according to a mass ratio of 5:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide accounting for 60% of the mass of the mixed solution, carrying out constant-temperature ultrasonic dispersion for 40min at the temperature of 45 ℃ and the ultrasonic frequency of 80kHz, adding a sodium carbonate solution accounting for 30% of the mass of the mixed solution and accounting for 10% of the mass of the mixed solution, carrying out hydrothermal reaction for 3h at the temperature of 120 ℃ and the stirring speed of 400r/min, carrying out suction filtration, collecting a filter cake, washing the filter cake with deionized water until the washing liquid is neutral, transferring the washed filter cake into a drying oven, drying to constant weight at the temperature of 100 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating to 1250 ℃ at the speed of 3 ℃/min under the condition of argon atmosphere, carrying out heat preservation and calcination for 30min, cooling to room temperature along with the furnace, and discharging to obtain a 2# cobalt green pigment;
wherein the particle size distribution range of the graphene oxide is 0.5-4 μm, and the D50 is 1 μm;
and mixing the obtained 1# cobalt green pigment and 2# cobalt green pigment according to a mass ratio of 1:3, mixing, stirring and mixing for 3 hours at the rotating speed of 300r/min by using a stirrer, and discharging to obtain the product.
Example 2
Preparing raw materials:
according to the molar ratio of cobalt, zinc and chromium being 0.8:0.2:1.8, preparing a 12% cobalt sulfate solution, a 12% zinc sulfate solution and an 18% chromium nitrate solution, mixing, and stirring and mixing for 50min by using a stirrer at a stirring speed of 600r/min to obtain a mixed solution;
preparation of 1# cobalt green pigment:
and (3) mixing the mixed solution with polyethylene glycol according to the mass ratio of 8:1, mixing and pouring the mixture into a reaction kettle, adding a sodium carbonate solution with the mass fraction of 15 percent and hollow glass beads with the mass fraction of 1.2 times that of the mixture solution, wherein the mass fraction of the sodium carbonate solution is 40 percent of the mass of the mixture solution, carrying out hydrothermal reaction for 4 hours at the temperature of 125 ℃ and the stirring speed of 500r/min, filtering, collecting a filter cake, washing the filter cake with deionized water until the washing liquid is neutral, transferring the washed filter cake into a drying oven, drying the filter cake to constant weight at the temperature of 105 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating the dried filter cake to 1300 ℃ at the speed of 6 ℃/min, carrying out heat preservation and calcination for 40min, cooling the dried filter cake to room temperature, and discharging to obtain a 1# cobalt green pigment;
wherein the particle size distribution range of the hollow glass beads is 8-20 μm, and the D50 is 12 μm;
the polyethylene glycol is selected from PEG-400;
preparation of # 2 cobalt green pigment:
mixing the mixed solution with a nano styrene-acrylic emulsion with the solid content of 32% according to a mass ratio of 8:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide accounting for 70% of the mass of the mixture, carrying out constant-temperature ultrasonic dispersion for 50min at the temperature of 50 ℃ and the ultrasonic frequency of 90kHz, adding a sodium carbonate solution accounting for 40% of the mass of the mixture and accounting for 15% of the mass of the mixture, carrying out hydrothermal reaction for 4h at the temperature of 125 ℃ and the stirring speed of 500r/min, carrying out suction filtration, collecting a filter cake, washing the filter cake with deionized water until the washing liquid is neutral, transferring the washed filter cake into a drying oven, drying to constant weight at the temperature of 105 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating to 1300 ℃ at the speed of 6 ℃/min under the condition of argon atmosphere, carrying out heat preservation and calcination for 40min, cooling to room temperature along with the furnace, and discharging to obtain a 2# cobalt green pigment;
wherein the particle size distribution range of the graphene oxide is 1-4 μm, and the D50 is 1.5 μm;
and mixing the obtained 1# cobalt green pigment and 2# cobalt green pigment according to a mass ratio of 1:4, mixing, stirring and mixing for 4 hours at the rotating speed of 400r/min by using a stirrer, and discharging to obtain the product.
Example 3
Preparing raw materials:
according to the molar ratio of cobalt, zinc and chromium being 1.0:0.3:2.0, preparing a cobalt sulfate solution with the mass fraction of 15%, a zinc sulfate solution with the mass fraction of 15% and a chromium nitrate solution with the mass fraction of 20%, mixing, and stirring and mixing for 60min by using a stirrer under the condition that the stirring speed is 800r/min to obtain a mixed solution;
preparation of 1# cobalt green pigment:
mixing the mixed solution with polyethylene glycol according to a mass ratio of 10:1, mixing and pouring the mixture into a reaction kettle, adding a sodium carbonate solution with the mass fraction of 20 percent and hollow glass beads with the mass fraction of 1.5 times of the mass of the mixture solution, wherein the mass fraction of the sodium carbonate solution is 50 percent of the mass of the mixture solution, carrying out hydrothermal reaction for 5 hours at the temperature of 130 ℃ and the stirring speed of 600r/min, filtering, collecting a filter cake, washing the filter cake with deionized water until the washing liquid is neutral, transferring the washed filter cake into a drying oven, drying the filter cake to constant weight at the temperature of 110 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating the dried filter cake to 1350 ℃ at the speed of 8 ℃/min, carrying out heat preservation and calcination for 45min, cooling the dried filter cake to room temperature, and discharging to obtain the 1# cobalt green pigment;
wherein the particle size distribution range of the hollow glass beads is 10-20 μm, and the D50 is 15 μm;
the polyethylene glycol is selected from PEG-600;
preparation of # 2 cobalt green pigment:
mixing the mixed solution with a nano styrene-acrylic emulsion with a solid content of 35% according to a mass ratio of 10:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide accounting for 80% of the mass of the mixture, then carrying out constant-temperature ultrasonic dispersion for 60min at the temperature of 55 ℃ and the ultrasonic frequency of 100kHz, adding a sodium carbonate solution accounting for 50% of the mass of the mixture and accounting for 20% of the mass of the mixture, carrying out hydrothermal reaction for 5h at the temperature of 130 ℃ and the stirring speed of 600r/min, carrying out suction filtration, collecting a filter cake, washing the filter cake with deionized water until the washing liquid is neutral, transferring the washed filter cake into a drying oven, drying to constant weight at the temperature of 110 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating to 1350 ℃ at the speed of 8 ℃/min under the condition of argon atmosphere, carrying out heat preservation and calcination for 45min, cooling to room temperature along with the furnace, and discharging to obtain a 2# cobalt green pigment;
wherein the particle size distribution range of the graphene oxide is 2-4 μm, and the D50 is 3 μm;
and mixing the obtained 1# cobalt green pigment and 2# cobalt green pigment according to a mass ratio of 1:5, mixing, stirring and mixing for 5 hours at the rotating speed of 500r/min by using a stirrer, and discharging to obtain the product.
Example 4
This example differs from example 1 in that: the nano styrene-acrylic emulsion is not added, and other conditions are kept unchanged.
Comparative example 1
This comparative example differs from example 1 in that: the graphene oxide is replaced by hollow glass microspheres with the same mass, the particle size distribution range of 5-20 mu m and the D50 of 10 mu m, and the rest conditions are kept unchanged.
Comparative example 2
This comparative example differs from example 1 in that: the graphene oxide with the same mass, the particle size distribution range of 0.5-4 mu m and the D50 of 1 mu m is adopted to replace the hollow glass microspheres, and the other conditions are kept unchanged.
Comparative example 3
This comparative example differs from example 1 in that: graphene oxide with the particle size distribution range of 5-20 μm and the D50 of 10 μm in equal mass is adopted to replace the graphene oxide with the particle size distribution range of 0.5-4 μm and the D50 of 1 μm, and the rest conditions are kept unchanged.
Comparative example 4
This comparative example differs from example 1 in that: the hollow glass beads with the same mass, the particle size distribution range of 0.5-4 mu m and the D50 of 1 mu m are adopted to replace the hollow glass beads with the particle size distribution range of 5-20 mu m and the D50 of 10 mu m, and the rest conditions are kept unchanged.
The products obtained in examples 1 to 4 and comparative examples 1 to 4 were subjected to performance tests, and the specific test methods and test results are as follows:
according to the mass ratio of 25:75 mixing the above products of each example or comparative example with the organic silicon resin SC-8-768 respectively, and adding a curing agent matched with the organic silicon resin; wherein, the organic silicon resin and the matched curing agent thereof are produced by Shenzhen shengzhen electronic material Limited company; after stirring and mixing evenly, coating on the surface of the polymethyl methacrylate resin sheet, controlling the thickness of a coating film to be 2mm, and after the coating film is dried and cured, carrying out the following performance test;
the heat reflection performance of the coating sample is tested by adopting a Lamda950 (produced by PE company) ultraviolet-visible-near infrared spectrophotometer, the heat reflection performance (reflectance ratio) of the product at 500nm waveband, 1000nm waveband and 1500nm waveband is respectively tested and recorded, and the specific test result is shown in Table 1;
table 1: product performance test results
| 500nm wave band | 1000nm wave band | 1500nm wave band | |
| Example 1 | 0.48 | 0.83 | 0.29 |
| Example 2 | 0.49 | 0.84 | 0.31 |
| Example 3 | 0.49 | 0.84 | 0.31 |
| Example 4 | 0.46 | 0.82 | 0.31 |
| Comparative example 1 | 0.40 | 0.76 | 0.24 |
| Comparative example 2 | 0.39 | 0.75 | 0.24 |
| Comparative example 3 | 0.38 | 0.75 | 0.22 |
| Comparative example 4 | 0.38 | 0.74 | 022 |
The test results in table 1 show that the product obtained by the invention can play a good reflection role in different wave bands, and has wide application scenes.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. An infrared-reflective cobalt green pigment, comprising:
the 1# cobalt green pigment is composed of hollow glass beads and a cobalt green pigment layer loaded on the surfaces of the hollow glass beads;
the 2# cobalt green pigment is composed of graphene oxide and cobalt green pigment layers loaded between the graphene oxide layers;
the D50 of the hollow glass beads is 10-15 μm;
the D50 of the graphene oxide is 1-3 μm;
the mass ratio of the No. 1 cobalt green pigment to the No. 2 cobalt green pigment is 1:3-1:5.
2. the infrared-reflective cobalt green pigment of claim 1, wherein the hollow glass microspheres have a particle size distribution ranging from 5 to 20 μm, and the graphene oxide has a particle size distribution ranging from 0.5 to 4 μm.
3. The infrared-reflective cobalt green pigment of claim 1, wherein the cobalt green pigment layer is a continuous cobalt green pigment layer.
4. The infrared-reflective cobalt green pigment as claimed in claim 3, wherein spherical porous carbon is distributed at intervals in the 2# cobalt green pigment layer.
5. A process for preparing an infrared-reflective cobalt green pigment according to any one of claims 1 to 4, comprising the specific steps of:
preparing raw materials:
according to the molar ratio of the cobalt, the zinc and the chromium being 0.5-1.0:0.1-0.3:1.5-2.0, preparing a cobalt sulfate solution, a zinc sulfate solution and a chromium nitrate solution, and uniformly mixing the cobalt sulfate solution, the zinc sulfate solution and the chromium nitrate solution to obtain a mixed solution;
preparation of 1# cobalt green pigment:
and (3) mixing the mixed solution with polyethylene glycol according to a mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding 30-50% by mass of a sodium carbonate solution with the mass fraction of 10-20% and hollow glass beads with the mass fraction of 1.0-1.5 times that of the mixture, carrying out hydrothermal reaction, filtering, washing and drying, carrying out high-temperature calcination, cooling and discharging to obtain the No. 1 cobalt green pigment;
preparation of # 2 cobalt green pigment:
mixing the mixed solution with the nano styrene-acrylic emulsion according to a mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide accounting for 60-80% of the mass of the mixed solution, performing ultrasonic dispersion uniformly, adding a sodium carbonate solution accounting for 30-50% of the mass of the mixed solution and accounting for 10-20% of the mass of the mixed solution, performing hydrothermal reaction, performing suction filtration, washing and drying, calcining at high temperature under the protection of inert gas, cooling, and discharging to obtain a 2# cobalt green pigment;
and mixing the obtained 1# cobalt green pigment and 2# cobalt green pigment according to the mass ratio of 1:3-1:5, uniformly mixing to obtain the product.
6. The process for preparing an infrared-reflective cobalt green pigment according to claim 5, wherein the polyethylene glycol is selected from any one of PEG-200, PEG-400 or PEG-600.
7. The preparation process of the infrared reflection cobalt green pigment according to claim 5, wherein the solid content of the nano styrene-acrylic emulsion is 30-35%.
8. The process of claim 5, wherein the high temperature calcination is: heating to 1250-1350 ℃ at the speed of 3-8 ℃/min, and then carrying out heat preservation and calcination for 30-45min.
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| CN116218315A (en) * | 2023-04-10 | 2023-06-06 | 常州烯聚新材料科技有限公司 | Long-acting visible-near infrared graphene-based black high-reflectivity coating and preparation method thereof |
| CN116218315B (en) * | 2023-04-10 | 2024-02-06 | 常州烯聚新材料科技有限公司 | Long-acting visible-near infrared graphene-based black high-reflectivity coating and preparation method thereof |
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