CN114250007A - Vanadium-containing color-changing coating and preparation method thereof - Google Patents
Vanadium-containing color-changing coating and preparation method thereof Download PDFInfo
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- CN114250007A CN114250007A CN202111393825.0A CN202111393825A CN114250007A CN 114250007 A CN114250007 A CN 114250007A CN 202111393825 A CN202111393825 A CN 202111393825A CN 114250007 A CN114250007 A CN 114250007A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/26—Thermosensitive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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Abstract
The invention relates to the field of chemical industry, and discloses a vanadium-containing color-changing coating and a preparation method thereof. The method comprises the following steps: (1) mixing vanadium pentoxide and an acetic acid aqueous solution for reaction, and then filtering to obtain a first filtrate; (2) mixing the first filtrate with cholesterol and triglyceride for reaction, and then filtering to obtain a second filtrate; (3) adding aluminum silicate into the second filtrate, stirring and reacting to obtain vanadium-containing color-changing coating; in the step (1), the solid-to-liquid ratio of the vanadium pentoxide to the acetic acid aqueous solution is 100-300 g/L. The vanadium-containing color-changing coating prepared by the method is an excellent high-temperature color-developing coating, and the color deepens along with the rise of the temperature, and the highest temperature can reach 500 ℃. Has the characteristics of simple preparation process, bright color at high temperature, normal-temperature recovery color and repeated use.
Description
Technical Field
The invention relates to the field of chemical industry, and particularly relates to a vanadium-containing color-changing coating and a preparation method thereof.
Background
Vanadium is a substance with multiple valence states, and is characterized by its diversified color and rich color due to its multiple valence states, wherein pentavalent vanadium is light yellow under alkaline condition, red under acidic condition, quadrivalent vanadium is blue under acidic condition, trivalent state is black, and valence state is gray, and combines with different atoms to display different colors, such as VF4Green, VF3Yellow-green, VCl4Red, magenta. VO is thus2Is an excellent coating per se.
Patent application CN113105765A discloses an intelligent thermal insulation composite coating with high visible light transmittance, which comprises a first anti-reflection coating, a vanadium dioxide coating, a tungsten bronze coating and a second anti-reflection coating. Also discloses a preparation method of the intelligent heat-insulating composite coating with high visible light transmittance. The composite coating can be directly acted on service glass, has high visible light transmittance which can reach 75 percent, has the performances of high visible light transmittance, low-temperature infrared light barrier rate of more than 50 percent, high-temperature infrared light barrier rate of more than 60 percent and infrared light regulation rate of more than 10 percent, can play a role in heat insulation at the temperature of more than 10 ℃ when being applied to the surface of the glass, and can meet the requirements of light transmission and heat insulation of building glass, traffic glass and the like. Vanadium dioxide is used directly as a coating in this patent application. However, at present, no report is found about the preparation of high-temperature color-changing coating by directly using vanadium as a raw material.
Disclosure of Invention
The invention aims to solve the problems of few high-temperature color-changing coatings, narrow color-changing range and the like in the prior art, and provides a vanadium-containing color-changing coating and a preparation method thereof.
In order to achieve the above object, the present invention provides a method for preparing a vanadium-containing color-changing paint, comprising the steps of:
(1) mixing vanadium pentoxide and an acetic acid aqueous solution for reaction, and then filtering to obtain a first filtrate;
(2) mixing the first filtrate with cholesterol and triglyceride for reaction, and then filtering to obtain a second filtrate;
(3) adding aluminum silicate into the second filtrate, stirring and reacting to obtain vanadium-containing color-changing coating;
in the step (1), the solid-to-liquid ratio of the vanadium pentoxide to the acetic acid aqueous solution is 100-300 g/L.
Preferably, in step (1), the pH value of the aqueous acetic acid solution is 1.5-3.
Preferably, in the step (1), the reaction temperature is 60-80 ℃ and the reaction time is 60-180 min.
Preferably, in the step (2), the solid-to-liquid ratio of the cholesterol to the first filtrate is 0.5-3 g/L.
Preferably, in step (2), the volume ratio of triglyceride to first filtrate is 0.5-1: 1000.
Preferably, in the step (2), the reaction temperature is 40-60 ℃ and the reaction time is 60-120 min.
Preferably, in the step (3), the solid-to-liquid ratio of the aluminum silicate to the second filtrate is 3-50 g/L.
Preferably, in the step (3), the stirring reaction time is 30-60min, and the stirring reaction temperature is 10-35 ℃.
Preferably, in step (1), the purity of the vanadium pentoxide is greater than or equal to 98.5 wt.%.
The second aspect of the invention provides the vanadium-containing color-changing coating prepared by the method.
The vanadium-containing color-changing coating prepared by the method is an excellent high-temperature color-developing coating, and the color deepens along with the rise of the temperature, and the highest temperature can reach 500 ℃. Has the characteristics of simple preparation process, bright color at high temperature, normal-temperature recovery color and repeated use.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of a vanadium-containing color-changing coating, which comprises the following steps:
(1) mixing vanadium pentoxide and an acetic acid aqueous solution for reaction, and then filtering to obtain a first filtrate;
(2) mixing the first filtrate with cholesterol and triglyceride for reaction, and then filtering to obtain a second filtrate;
(3) adding aluminum silicate into the second filtrate, stirring and reacting to obtain vanadium-containing color-changing coating;
in the step (1), the solid-to-liquid ratio of the vanadium pentoxide to the acetic acid aqueous solution is 100-300 g/L.
In a preferred embodiment, the solid-to-liquid ratio of the vanadium pentoxide to the aqueous acetic acid solution in step (1) may be 100g/L, 150g/L, 200g/L, 250g/L or 300 g/L.
In a preferred embodiment, in step (1), the pH of the aqueous acetic acid solution is 1.5 to 3.
In a preferred embodiment, in step (1), the reaction temperature is 60-80 ℃ and the reaction time is 60-180 min. Specifically, the reaction temperature can be 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃; the reaction time may be 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180 min.
In a preferred embodiment, in step (2), the solid-to-liquid ratio of cholesterol to first filtrate is 0.5 to 3 g/L. Specifically, the solid-to-liquid ratio may be 0.5g/L, 1g/L, 1.5g/L, 2g/L, 2.5g/L, or 3 g/L.
In a preferred embodiment, in step (2), the volume ratio of triglyceride to first filtrate is 0.5-1: 1000.
In a preferred embodiment, in step (2), the reaction temperature is 40-60 ℃ and the reaction time is 60-120 min. Specifically, the reaction temperature can be 40 ℃, 45 ℃, 50 ℃, 55 ℃ or 60 ℃; the reaction time may be 60min, 70min, 80min, 90min, 100min, 110min, or 120 min.
In a preferred embodiment, in step (3), the solid-to-liquid ratio of the aluminum silicate to the second filtrate is 3 to 50 g/L. Specifically, the solid-to-liquid ratio may be 3g/L, 5g/L, 10g/L, 15g/L, 20g/L, 25g/L, 30g/L, 35g/L, 40g/L, 45g/L, or 50 g/L.
In a preferred embodiment, in the step (3), the stirring reaction time is 30 to 60min, and the stirring reaction temperature is 10 to 35 ℃. Specifically, the reaction time can be 30min, 35min, 40min, 45min, 50min, 55min or 60 min; the reaction temperature may be 10 deg.C, 15 deg.C, 20 deg.C, 25 deg.C, 30 deg.C or 35 deg.C.
In a preferred embodiment, in step (1), the purity of the vanadium pentoxide is greater than or equal to 98.5% by weight.
The second aspect of the invention provides the vanadium-containing color-changing coating prepared by the method.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
Example 1
(1) Mixing 40g of vanadium pentoxide (with a purity of 98.5%) and 0.2L of an aqueous acetic acid solution (pH 1.5) to react at 60 ℃ for 60min, and then filtering to obtain 0.2L of a first filtrate;
(2) mixing 0.2L of the first filtrate with 0.1g of cholesterol and 0.1mL of triglyceride for reaction at 40 ℃ for 60min, and then filtering to obtain 200.1mL of second filtrate;
(3) and adding 0.603g of aluminum silicate into 200.1mL of the second filtrate, stirring at room temperature (25 ℃) and reacting for 30min to obtain the vanadium-containing color-changing coating.
Example 2
(1) Mixing 200g of vanadium pentoxide (with the purity of 99%) and 1L of acetic acid aqueous solution (with the pH value of 2) for reaction at the temperature of 70 ℃ for 120min, and then filtering to obtain 995mL of first filtrate;
(2) mixing 995mL of the first filtrate with 2g of cholesterol and 0.8mL of triglyceride for reaction at 50 ℃ for 100min, and then filtering to obtain 995.6mL of a second filtrate;
(3) and adding 30g of aluminum silicate into 995.6mL of second filtrate, and stirring at room temperature (25 ℃) to react for 40min to obtain the vanadium-containing color-changing coating.
Example 3
(1) Mixing 300g of vanadium pentoxide (with the purity of 99.5%) and 1.5L of acetic acid aqueous solution (with the pH value of 3) for reaction, reacting at the temperature of 80 ℃ for 180min, and then filtering to obtain 1470mL of first filtrate;
(2) mixing 1470mL of first filtrate, 4.41g of cholesterol and 1.47mL of triglyceride for reaction at 60 ℃ for 120min, and then filtering to obtain 1464mL of second filtrate;
(3) and adding 73.2g of aluminum silicate into 1464mL of second filtrate, and stirring at room temperature (25 ℃) to react for 60min to obtain the vanadium-containing color-changing coating.
Comparative example 1
(1) Mixing 35g of vanadium pentoxide (with a purity of 98.5%) and 0.2L of an aqueous acetic acid solution (with a pH of 1.5) to react at a reaction temperature of 60 ℃ for 60min, and then filtering to obtain 0.2L of a first filtrate;
(2) mixing 0.2L of the first filtrate with 0.08g of cholesterol and 0.08mL of triglyceride for reaction at 40 ℃ for 60min, and then filtering to obtain 200mL of second filtrate;
(3) and adding 0.50g of aluminum silicate into 200mL of second filtrate, stirring at room temperature (25 ℃) and reacting for 30min to obtain the vanadium-containing color-changing coating.
Comparative example 2
(1) Mixing 65g of vanadium pentoxide (with a purity of 98.5%) and 0.2L of an aqueous acetic acid solution (pH 1.5) to react at 60 ℃ for 60min, and then filtering to obtain 0.195L of a first filtrate;
(2) mixing 0.195L of the first filtrate with 0.6g of cholesterol and 0.25mL of triglyceride for reaction at 40 ℃ for 60min, and then filtering to obtain 192mL of second filtrate;
(3) and adding 12g of aluminum silicate into 192mL of second filtrate, stirring at room temperature (25 ℃) and reacting for 30min to obtain the vanadium-containing color-changing coating.
Test example
The coatings obtained in the examples and comparative examples were applied to the surface of a porcelain cell and placed in a muffle furnace set at a temperature schedule of: the mixture is put into the porcelain cell from room temperature at the temperature of 10 ℃/1min (the temperature is raised by 10 ℃ for 1 min), the color change of the surface coating coated on the porcelain cell is observed, and the color change temperature range is determined. The results are shown in Table 1.
TABLE 1
As can be seen from the data in Table 1, the method of the present invention can prepare high temperature color-changing coatings with wide color-changing range.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The preparation method of the vanadium-containing color-changing coating is characterized by comprising the following steps:
(1) mixing vanadium pentoxide and an acetic acid aqueous solution for reaction, and then filtering to obtain a first filtrate;
(2) mixing the first filtrate with cholesterol and triglyceride for reaction, and then filtering to obtain a second filtrate;
(3) adding aluminum silicate into the second filtrate, stirring and reacting to obtain vanadium-containing color-changing coating;
in the step (1), the solid-to-liquid ratio of the vanadium pentoxide to the acetic acid aqueous solution is 100-300 g/L.
2. The method for preparing vanadium-containing color-changing paint according to claim 1, wherein in the step (1), the pH value of the acetic acid aqueous solution is 1.5-3.
3. The method for preparing the vanadium-containing color-changing paint according to claim 1, wherein in the step (1), the reaction temperature is 60-80 ℃ and the reaction time is 60-180 min.
4. The method for preparing vanadium-containing allochromatic paint according to claim 1, wherein in the step (2), the solid-to-liquid ratio of cholesterol to the first filtrate is 0.5-3 g/L.
5. The method for preparing vanadium-containing color-changing paint according to claim 1 or 4, wherein in the step (2), the volume ratio of the triglyceride to the first filtrate is 0.5-1: 1000.
6. The method for preparing the vanadium-containing color-changing paint according to claim 1, wherein in the step (2), the reaction temperature is 40-60 ℃ and the reaction time is 60-120 min.
7. The method for preparing vanadium-containing allochromatic paint as claimed in claim 1, wherein in the step (3), the solid-to-liquid ratio of the aluminum silicate to the second filtrate is 3-50 g/L.
8. The method for preparing vanadium-containing allochroic paint according to claim 1, wherein in the step (3), the stirring reaction time is 30-60min, and the stirring reaction temperature is 10-35 ℃.
9. The method for preparing the vanadium-containing color-changing paint according to claim 1, wherein in the step (1), the purity of the vanadium pentoxide is more than or equal to 98.5 wt%.
10. The vanadium-containing color-changing paint prepared by the method of any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111393825.0A CN114250007A (en) | 2021-11-23 | 2021-11-23 | Vanadium-containing color-changing coating and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111393825.0A CN114250007A (en) | 2021-11-23 | 2021-11-23 | Vanadium-containing color-changing coating and preparation method thereof |
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| CN202111393825.0A Pending CN114250007A (en) | 2021-11-23 | 2021-11-23 | Vanadium-containing color-changing coating and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106634065A (en) * | 2016-09-28 | 2017-05-10 | 浙江大学自贡创新中心 | Intelligent inorganic thermal insulation coating containing two components |
| CN109399710A (en) * | 2018-10-26 | 2019-03-01 | 西安理工大学 | Witch culture temperature induced color changing VO2Nano material and its preparation method and application |
| CN110923814A (en) * | 2019-11-25 | 2020-03-27 | 北京理工大学重庆创新中心 | Preparation method of nano vanadium dioxide film |
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2021
- 2021-11-23 CN CN202111393825.0A patent/CN114250007A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106634065A (en) * | 2016-09-28 | 2017-05-10 | 浙江大学自贡创新中心 | Intelligent inorganic thermal insulation coating containing two components |
| CN109399710A (en) * | 2018-10-26 | 2019-03-01 | 西安理工大学 | Witch culture temperature induced color changing VO2Nano material and its preparation method and application |
| CN110923814A (en) * | 2019-11-25 | 2020-03-27 | 北京理工大学重庆创新中心 | Preparation method of nano vanadium dioxide film |
Non-Patent Citations (1)
| Title |
|---|
| 张小强: ""钨、铕掺杂及退火对温致变色二氧化钒性能影响的研究"", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 * |
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Application publication date: 20220329 |