CN115353753B - Infrared reflection cobalt green pigment and preparation process thereof - Google Patents
Infrared reflection cobalt green pigment and preparation process thereof Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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 No. 1 cobalt green pigment, wherein the No. 1 cobalt green pigment consists of hollow glass beads and a cobalt green pigment layer loaded on the surfaces of the hollow glass beads; the 2# cobalt green pigment consists of graphene oxide and a cobalt green pigment layer supported between graphene oxide layers; during preparation, mixing the mixed solution with polyethylene glycol, adding sodium carbonate solution and hollow glass beads, performing hydrothermal reaction, filtering, washing, drying, calcining at high temperature, cooling, and discharging to obtain 1# cobalt green; mixing the mixed solution with the nano styrene-acrylic emulsion, adding graphene oxide, uniformly dispersing by ultrasonic, adding sodium carbonate solution, performing a hydrothermal reaction, performing suction filtration, washing and drying, calcining at a 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, to an infrared reflection cobalt green pigment and a preparation process thereof.
Background
Cobalt green is a pigment with unique yellow-green color and vivid hue. Compared with other green pigments, the 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 fields of high color retention, gloss retention, and chalk resistance, the use of such pigments is often required. From the structure and color development mechanism of cobalt green pigment, other metal ions with similar atomic radius can be doped in the preparation of cobalt green pigment to change CO 2+ The coordination state of the cobalt green pigment is changed, so that a series of modified cobalt green pigments can be formed, the application performance of the cobalt green pigments is improved, and the application field of the cobalt green pigments is expanded.
The traditional preparation method of the cobalt pigment is a solid phase method. However, the solid phase reaction method has high energy consumption, the reaction speed is affected by diffusion kinetics, the physical and chemical reactions are not easy to fully proceed, the prepared pigment has uneven particle size distribution, the pigment has poor color and chemical stability, and certain defects exist in the application performance. The liquid phase coprecipitation method is to uniformly mix reactants under a liquid phase, the reactants can fully react, and the prepared pigment has small granularity, high purity, low calcining temperature and easy control compared with solid phase reaction, and has excellent high-temperature stability and chemical stability.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings that the existing cobalt green pigment only singly depends on reflection or refraction of the pigment to light in the actual use process, so that the performance bottleneck of the material is difficult to break through further, and provides an infrared reflection cobalt green pigment and a preparation process thereof.
The invention aims to provide an infrared reflection cobalt green pigment.
The invention further aims to provide a preparation process of the infrared reflection cobalt green pigment.
The above object of the present invention is achieved by the following technical scheme:
an infrared reflective cobalt green pigment comprising:
the 1# cobalt green pigment consists of hollow glass beads and a cobalt green pigment layer loaded on the surfaces of the hollow glass beads;
the 2# cobalt green pigment consists of graphene oxide and a cobalt green pigment layer supported between graphene oxide layers;
the D50 of the hollow glass beads is 10-15 mu m;
the D50 of the graphene oxide is 1-3 mu m;
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 mu m, and the particle size distribution range of the graphene oxide is 0.5-4 mu m.
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 be used as a No. 1 cobalt green pigment, and the cobalt green pigment is loaded between layers of the hollow glass beads to be used as a No. 2 cobalt green pigment by utilizing the graphene oxide with the layered structure;
the 1# cobalt green pigment can strengthen the reflection and refraction effects of the pigment by utilizing the reflection and refraction effects of the spherical glass beads and the interfaces between the spherical glass beads and the cobalt green pigment adsorbed on the surfaces of the spherical glass beads; meanwhile, the particle size of the spherical glass beads is larger than that of 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 the other part of graphene oxide is distributed on the surface of the whole coating, so that the interfaces of different glass beads of the coating are used for constructing light reflection and refraction interfaces, and meanwhile, interfaces with different reflection and refraction effects are constructed on the surface layer and the bottom layer, and the reflection effect of the product on infrared light is enhanced through rich interface effects.
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.
The preparation process of the infrared reflection cobalt green pigment comprises the following specific preparation steps:
raw material preparation:
the mole ratio of the cobalt, the zinc and the chromium is 0.5-1.0:0.1-0.3:1.5 to 2.0, preparing a cobalt sulfate solution, a zinc sulfate solution and a chromium nitrate solution, and uniformly mixing the three solutions to obtain a mixed solution;
preparation of # 1 cobalt green pigment:
mixing the mixed solution and polyethylene glycol according to the mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding a sodium carbonate solution with the mass fraction of 10-20% of the mass of the mixed solution and hollow glass beads with the mass of 1.0-1.5 times of the mass of the mixed solution, carrying out hydrothermal reaction, filtering, washing and drying, calcining at a high temperature, cooling, and discharging to obtain a No. 1 cobalt green pigment;
preparation of # 2 cobalt green pigment:
mixing the mixed solution and the nano styrene-acrylic emulsion according to the mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide with the mass of 60-80% of the mixed solution, uniformly dispersing by ultrasonic, adding sodium carbonate solution with the mass of 10-20% of the mixed solution with the mass of 30-50% of the mixed solution, carrying out a hydrothermal reaction, carrying out suction filtration, washing and drying, calcining at a high temperature under the protection of inert gas, cooling, and discharging to obtain a No. 2 cobalt green pigment;
the obtained 1# cobalt green pigment and the obtained 2# cobalt green pigment are mixed according to the mass ratio of 1:3-1:5, uniformly mixing to obtain the product.
According to the technical scheme, the nano styrene-acrylic emulsion is added in the preparation process of the No. 2 cobalt green pigment, the nano styrene-acrylic emulsion can adsorb and fix precursor crystals formed by precipitation, the precursor crystals are effectively fixed between dispersed graphene oxide layers to form a continuous pigment layer, and then the spherical hollow carbon is formed by gradually carbonizing styrene-acrylic emulsion microspheres under the high-temperature effect in the calcination process, so that the porosity in the continuous pigment layer can be effectively enriched, the density of the No. 2 cobalt green pigment is reduced, and meanwhile, interfaces are formed among different pigment particles through the existence of the pores, so that the infrared light reflection effect of the continuous pigment layer on the surface of the precursor crystals is effectively improved.
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: heating at a speed of 3-8 ℃/min to 1250-1350 ℃, and then preserving heat and calcining for 30-45min.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Reagents and materials used in the following examples are commercially available unless otherwise specified.
Example 1
Raw material preparation:
the mole ratio of the cobalt, the zinc and the chromium is 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 under the condition that the stirring speed is 400r/min by using a stirrer to obtain a mixed solution;
preparation of # 1 cobalt green pigment:
mixing the mixed solution and polyethylene glycol according to the 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% and hollow glass beads with the mass of 1.0 times of the mass of the mixture, carrying out hydrothermal reaction for 3 hours at the temperature of 120 ℃ under the condition of the stirring rotation 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 baking 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 to room temperature along with the furnace, and discharging to obtain a No. 1 cobalt green pigment;
wherein the particle size distribution range of the hollow glass beads is 5-20 mu m, and the D50 is 10 mu m;
the polyethylene glycol is selected from PEG-200;
preparation of # 2 cobalt green pigment:
mixing the mixed solution and the nano styrene-acrylic emulsion with the solid content of 30 percent according to the mass ratio of 5:1 mixing and pouring the mixture into a reaction kettle, adding graphene oxide with 60% of the mass of the mixed solution, then carrying out constant-temperature ultrasonic dispersion for 40min under the condition that the temperature is 45 ℃ and the ultrasonic frequency is 80kHz, adding sodium carbonate solution with 30% of the mass of the mixed solution and the mass fraction of 10%, carrying out hydrothermal reaction for 3h under the condition that the temperature is 120 ℃ and the stirring speed is 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 the filter cake to constant weight under the condition that the temperature is 100 ℃ to obtain a dried filter cake, transferring the obtained dried filter cake into a muffle furnace, heating and heating the dried filter cake 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 No. 2 cobalt green pigment;
wherein the particle size distribution range of the graphene oxide is 0.5-4 mu m, and D50 is 1 mu m;
the obtained 1# cobalt green pigment and the obtained 2# cobalt green pigment are mixed according to the 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
Raw material preparation:
the mole ratio of cobalt, zinc and chromium is 0.8:0.2:1.8, preparing a cobalt sulfate solution with the mass fraction of 12%, a zinc sulfate solution with the mass fraction of 12% and a chromium nitrate solution with the mass fraction of 18%, mixing, and stirring and mixing for 50min under the condition that the stirring speed is 600r/min by using a stirrer to obtain a mixed solution;
preparation of # 1 cobalt green pigment:
mixing the mixed solution and 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% and hollow glass beads with the mass fraction of 1.2 times of the mixed solution, carrying out hydrothermal reaction for 4 hours at the temperature of 125 ℃ and the stirring rotation speed of 500r/min, filtering, collecting a filter cake, washing the filter cake with deionized water until the washing solution is neutral, transferring the washed filter cake into a baking oven, drying at the temperature of 105 ℃ until the constant weight is obtained, transferring the obtained dry filter cake into a muffle furnace, heating the obtained dry filter cake to 1300 ℃ at the speed of 6 ℃/min, carrying out heat preservation calcination for 40min, cooling to room temperature along with the furnace, and discharging to obtain a No. 1 cobalt green pigment;
wherein the particle size distribution range of the hollow glass beads is 8-20 mu m, and the D50 is 12 mu m;
the polyethylene glycol is selected from PEG-400;
preparation of # 2 cobalt green pigment:
mixing the mixed solution and the nano styrene-acrylic emulsion with the solid content of 32 percent according to the mass ratio of 8:1 mixing and pouring the mixture into a reaction kettle, adding graphene oxide with the mass of 70% of the mixed solution, then carrying out constant-temperature ultrasonic dispersion for 50min at the temperature of 50 ℃ and the ultrasonic frequency of 90kHz, adding sodium carbonate solution with the mass fraction of 15% of the mixed solution, carrying out hydrothermal reaction for 4 hours at the temperature of 125 ℃ and the stirring rotating 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 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 and heating the dried filter cake to 1300 ℃ at the speed of 6 ℃/min under the atmosphere of argon, carrying out heat preservation and calcination for 40min, cooling to room temperature along with the furnace, and discharging to obtain a No. 2 cobalt green pigment;
wherein the particle size distribution range of the graphene oxide is 1-4 mu m, and the D50 is 1.5 mu m;
the obtained 1# cobalt green pigment and the obtained 2# cobalt green pigment are mixed according to the 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
Raw material preparation:
the mole ratio of the cobalt, the zinc and the chromium is 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 under the condition that the stirring speed is 800r/min by using a stirrer to obtain a mixed solution;
preparation of # 1 cobalt green pigment:
mixing the mixed solution and polyethylene glycol according to the 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% and hollow glass beads with the mass of 1.5 times of the mass of the mixed solution, carrying out hydrothermal reaction for 5 hours at the temperature of 130 ℃ under the condition of the stirring rotating 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 baking 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 calcination for 45min, cooling to room temperature along with the furnace, and discharging to obtain a No. 1 cobalt green pigment;
wherein the particle size distribution range of the hollow glass beads is 10-20 mu m, and the D50 is 15 mu m;
the polyethylene glycol is selected from PEG-600;
preparation of # 2 cobalt green pigment:
mixing the mixed solution and the nano styrene-acrylic emulsion with the solid content of 35 percent according to the mass ratio of 10:1 mixing and pouring the mixture into a reaction kettle, adding graphene oxide with 80% of the mass of the mixed solution, then carrying out constant-temperature ultrasonic dispersion for 60min at the temperature of 55 ℃ and the ultrasonic frequency of 100kHz, adding sodium carbonate solution with 50% of the mass of the mixed solution and the mass fraction of 20%, carrying out hydrothermal reaction for 5h at the temperature of 130 ℃ and the stirring rotating 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 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 and heating the dried filter cake to 1350 ℃ at the speed of 8 ℃/min under the argon atmosphere, carrying out heat preservation calcination for 45min, cooling to room temperature along with the furnace, and discharging to obtain a No. 2 cobalt green pigment;
wherein the particle size distribution range of the graphene oxide is 2-4 mu m, and the D50 is 3 mu m;
the obtained 1# cobalt green pigment and the obtained 2# cobalt green pigment are mixed according to the 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
The difference between this embodiment and embodiment 1 is that: no nano styrene-acrylic emulsion is added, and the rest conditions are kept unchanged.
Comparative example 1
The difference between this comparative example and example 1 is that: the hollow glass beads with the equal mass and the particle size distribution range of 5-20 mu m and the D50 of 10 mu m are adopted to replace graphene oxide, and the rest conditions are kept unchanged.
Comparative example 2
The difference between this comparative example and example 1 is that: the hollow glass micro-beads are replaced by graphene oxide with the equal mass and the particle size distribution range of 0.5-4 mu m and the D50 of 1 mu m, and the rest conditions are kept unchanged.
Comparative example 3
The difference between this comparative example and example 1 is that: the graphene oxide with the equal mass and particle size distribution range of 5-20 mu m and the D50 of 10 mu m is adopted to replace the graphene oxide with the particle size distribution range of 0.5-4 mu m and the D50 of 1 mu m, and the rest conditions are kept unchanged.
Comparative example 4
The difference between this comparative example and example 1 is that: the hollow glass beads with the equal mass and 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 specific test methods and test results are as follows:
the mass ratio is 25:75, respectively mixing the products of the examples or the comparative examples with the silicone resins SC-8-768, and adding a curing agent matched with the silicone resins; wherein the organic silicon resin and the matched curing agent are produced by Shenzhen liter-based electronic materials Co., ltd; after stirring and mixing uniformly, coating the mixture on the surface of a polymethyl methacrylate resin sheet, controlling the thickness of a coating film to be 2mm, and carrying out the following performance test after the coating film is dried and solidified;
the thermal reflection performance of the coating samples was tested by using a Lamda950 (manufactured by PE company) ultraviolet-visible-near infrared spectrophotometer, and the thermal reflection performance (reflectance) of the products in 500nm band, 1000nm band and 1500nm band were respectively tested and recorded, and the specific test results are shown in Table 1;
table 1: product performance test results
| 500nm band | 1000nm band | 1500nm 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 |
As shown by the test results in the table 1, the product obtained by the invention can play a good role in reflection in different wave bands, and has wide application scenes.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (8)
1. An infrared reflective cobalt green pigment comprising:
the 1# cobalt green pigment consists of hollow glass beads and a cobalt green pigment layer loaded on the surfaces of the hollow glass beads;
the 2# cobalt green pigment consists of graphene oxide and a cobalt green pigment layer supported between graphene oxide layers;
the D50 of the hollow glass beads is 10-15 mu m;
the D50 of the graphene oxide is 1-3 mu m;
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 according to 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. An infrared reflective cobalt green pigment according to claim 1, wherein the cobalt green pigment layer is a continuous cobalt green pigment layer.
4. An infrared reflecting cobalt green pigment according to claim 3, wherein spherical porous carbon is spaced apart in the layer of cobalt green pigment comprising # 2.
5. A process for the preparation of an infrared reflective cobalt green pigment as claimed in any one of claims 1 to 4, wherein the specific preparation steps comprise:
raw material preparation:
the mole ratio of the cobalt, the zinc and the chromium is 0.5-1.0:0.1-0.3:1.5 to 2.0, preparing a cobalt sulfate solution, a zinc sulfate solution and a chromium nitrate solution, and uniformly mixing the three solutions to obtain a mixed solution;
preparation of # 1 cobalt green pigment:
mixing the mixed solution and polyethylene glycol according to the mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding a sodium carbonate solution with the mass fraction of 10-20% of the mass of the mixed solution and hollow glass beads with the mass of 1.0-1.5 times of the mass of the mixed solution, carrying out hydrothermal reaction, filtering, washing and drying, calcining at a high temperature, cooling, and discharging to obtain a No. 1 cobalt green pigment;
preparation of # 2 cobalt green pigment:
mixing the mixed solution and the nano styrene-acrylic emulsion according to the mass ratio of 5:1-10:1, mixing and pouring the mixture into a reaction kettle, adding graphene oxide with the mass of 60-80% of the mixed solution, uniformly dispersing by ultrasonic, adding sodium carbonate solution with the mass of 10-20% of the mixed solution with the mass of 30-50% of the mixed solution, carrying out a hydrothermal reaction, carrying out suction filtration, washing and drying, calcining at a high temperature under the protection of inert gas, cooling, and discharging to obtain a No. 2 cobalt green pigment;
the obtained 1# cobalt green pigment and the obtained 2# cobalt green pigment are mixed 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 said polyethylene glycol is selected from any one of PEG-200, PEG-400 or PEG-600.
7. The process for preparing an infrared reflective cobalt green pigment according to claim 5, wherein the nano styrene-acrylic emulsion has a solid content of 30-35%.
8. The process for preparing an infrared reflective cobalt green pigment according to claim 5, wherein the high temperature calcination is: heating at a speed of 3-8 ℃/min to 1250-1350 ℃, and then preserving heat and calcining for 30-45min.
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| CN109678222A (en) * | 2019-01-25 | 2019-04-26 | 浙江理工大学 | A kind of colored pigment and its preparation method and application with photo-catalysis function |
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