CN113185837A - Thermochromic material, preparation method thereof and thermochromic product - Google Patents
Thermochromic material, preparation method thereof and thermochromic product Download PDFInfo
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- CN113185837A CN113185837A CN202110384908.7A CN202110384908A CN113185837A CN 113185837 A CN113185837 A CN 113185837A CN 202110384908 A CN202110384908 A CN 202110384908A CN 113185837 A CN113185837 A CN 113185837A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The application provides a thermochromic material, a preparation method thereof and a thermochromic product. The thermochromic product comprises the thermochromic material. The thermochromic product prepared from the thermochromic material provided by the application has the advantages of higher ultraviolet resistance service life, broken use limitation, no limitation to silica gel products, wider application field and longer service life.
Description
Technical Field
The present invention relates to but is not limited to a color-changing product, and particularly relates to but is not limited to a temperature-sensitive color-changing material, a preparation method thereof and a temperature-sensitive color-changing product.
Background
The existing color-changing products on the market, such as color-changing silica gel water cups, color-changing plastics and the like, mostly adopt temperature-sensitive color-changing powder to be directly added into a product raw material system, the illumination-resistant color-changing effect is very poor, the use environment is limited, the service life of the product is short, the effect of independently adding an ultraviolet absorbent and a light shielding agent in the system is not obvious, and the market demand is difficult to meet; only the ultraviolet absorbent is added into the raw material system, so that the uvioresistant performance of the raw material system is improved, but the protection effect on the temperature-sensitive color-changing powder is not obvious, and the temperature-sensitive color-changing powder can still be damaged by ultraviolet rays. At present, most of the color changing principles of the temperature-sensitive color changing powder on the market are electron transfer processes of organic compounds, the color changing powder is sensitive to ultraviolet rays, and the ultraviolet resistance of the transparent shell is difficult to promote, the cost is high, so that the application scene of a color changing product is greatly influenced by the environment.
Disclosure of Invention
The following is a summary of the subject matter described in detail herein. This summary is not intended to limit the scope of the present application.
According to the technical scheme, the temperature-sensitive color-changing powder is modified by the high-adsorption modified mesoporous silica microspheres, so that the aging of ultraviolet rays to the temperature-sensitive color-changing powder can be effectively prevented, the service life of a temperature-sensitive color-changing product is prolonged, and the use scene is widened;
the base material in the technical scheme of the application can be silica gel, thermoplastic materials (PP, ABS and the like), thermosetting materials (epoxy resin, silicone resin and the like).
The application provides a temperature-sensitive color-changing material which comprises a temperature-sensitive color-changing powder, an antioxidant, an ultraviolet absorbent, silica microspheres and silicone oil.
In one embodiment provided herein, the mass ratio of the temperature sensitive toner, the antioxidant, the ultraviolet absorber, and the silica microspheres to the silicone oil is (0.05 to 1): (0.1 to 1): (0.05 to 1.5): (0.05 to 0.8): (1 to 8).
In one embodiment provided herein, the thermochromic powder is added to the substrate in an amount of 0.05phr to 1phr, the antioxidant is added to the substrate in an amount of 0.1phr to 1phr, the ultraviolet absorber is added to the substrate in an amount of 0.05phr to 1.5phr, the silica microspheres are added to the substrate in an amount of 0.05phr to 0.8phr, and the silicone oil is added to the substrate in an amount of 1phr to 8 phr.
In one embodiment provided herein, the antioxidant is selected from any one or more of antioxidant 168, antioxidant 1010, and antioxidant 626;
in one embodiment provided herein, the ultraviolet absorber is selected from any one or more of UVP-327, UVP-531, UVP-327, and UV-9;
in one embodiment provided herein, the silicone oil is selected from any one or more of a dimethyl silicone oil, a vinyl silicone oil, and an amino silicone oil.
In one embodiment provided herein, the temperature sensitive toner has a particle size of 1 μm to 15 μm;
in one embodiment provided herein, the temperature-sensitive toner is a temperature-sensitive toner with a core-shell structure, and a thickness of a transparent shell in the core-shell structure is 100nm to 400 nm;
in one embodiment provided herein, the temperature sensitive color-changing powder has a color-changing temperature of 35 ℃ to 45 ℃;
in one embodiment provided by the present application, the thermochromic powder is subjected to surface modification treatment; optionally, the modifier selected for the surface modification treatment is any one or more of an amino silane coupling agent, a trialkoxy silane coupling agent and a dialkoxy coupling agent; optionally, the surface modification treatment comprises the following steps: uniformly mixing the surface of the thermochromic powder with the modifier, wherein the modifier is a modifier solution with the concentration of 0.5 wt.% to 1.0 wt.%, and then drying the modified thermochromic powder at the drying temperature of 60 ℃ to 90 ℃ for 20min to 60 min.
In one embodiment provided by the present application, the thermochromic powder core may be one of triarylmethane phthalide type, indoline phthalide type, fluorane type, phenothiazine type reversible thermochromic pigments;
in one embodiment provided herein, the modifier solution may be used in an amount that the surface of the thermochromic powder is slightly wet.
In one embodiment provided herein, the silica microspheres are mesoporous silica microspheres;
in one embodiment provided herein, the silica microspheres are hollow silica microspheres;
in one embodiment provided herein, the silica microspheres have a particle size of 80nm to 300 nm;
in one embodiment provided herein, the silica microspheres are further subjected to a surface modification treatment, wherein the surface modification treatment comprises uniformly mixing a portion of the ultraviolet absorber with the silica microspheres. The mesoporous hollow silica and the mesoporous silica have better ultraviolet resistance effect, wherein the mesoporous hollow silica has better effect than the mesoporous silica, better light shielding effect and more obvious color development.
In one embodiment provided herein, the surface modification treatment comprises the steps of:
uniformly mixing a mixture obtained by mixing the ultraviolet absorbent and a solvent with the silicon dioxide microspheres, and finishing surface modification treatment after the solvent is volatilized;
in one embodiment provided herein, the uniformly mixing comprises ultrasonically dispersing for 20min to 40min under vacuum conditions of 5 ℃ to 20 ℃;
in one embodiment provided herein, the volatilizing comprises continuing the ultrasonic dispersion and raising the temperature to 40 ℃ to 60 ℃ after the mixing is uniform, and drying at 80 ℃ to 100 ℃ for 1h to 2h after the solvent is substantially volatilized.
In another aspect, the present application provides a method for preparing the thermochromic material, including the following steps:
1) uniformly mixing the temperature-sensitive color-changing powder with the silicon dioxide microspheres to obtain a mixture 1;
2) and uniformly mixing the mixture 1 with the ultraviolet absorbent, the antioxidant and the silicone oil to obtain the thermochromic material.
In another aspect, the present application provides the above thermochromic product, which includes a substrate and the above thermochromic material; the substrate is selected from any one or more of silica gel, thermoplastic materials and thermosetting materials;
in one embodiment provided herein, the thermochromic article is prepared by injection molding or compression molding.
In one embodiment provided herein, the silica gel is selected from one or more of liquid silica gel and solid silica gel.
In one embodiment provided herein, the injection molding temperature is from 100 ℃ to 150 ℃ and the injection molding cycle is from 60s to 250 s;
in one embodiment provided by the application, the temperature of the injection-molded product is reduced in water at 10-40 ℃ to obtain the color-changing product.
The technical scheme provided by the application has the advantages of higher ultraviolet resistance service life, broken use limitation, application without limitation to silica gel products, wider application field and longer service life.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. Other advantages of the present application may be realized and attained by the invention in its aspects as described in the specification.
Drawings
The accompanying drawings are included to provide an understanding of the present disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the examples serve to explain the principles of the disclosure and not to limit the disclosure.
FIG. 1 is a schematic diagram showing the comparison between the color-changed product obtained in example 1 and a conventional product on the market, wherein the upper diagram in FIG. 1 is a photograph of the product just prepared, and the lower diagram is a photograph of the product after xenon lamp aging resistance test, as can be seen, the color of the product on the market is seriously faded, and the product provided by the application is basically fadeless.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, embodiments of the present application are described in detail below. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
Example 1
In the embodiment, the base material silica gel is liquid silica gel which is purchased from Japan Shifting company under the brand number KE-2090-50A/B;
the ultraviolet absorbent is UV-9, which is purchased from Guangzhou Honghai new material auxiliary agent company;
the antioxidant is antioxidant 168;
the silicone oil is dimethyl silicone oil, which is purchased from Xiamen Hanxu silicon material company and has a 500cps mark;
the temperature-sensitive color-changing powder is of a core-shell structure, the shell is made of melamine resin, and the content is reversible color-changing organic matter, and is purchased from Chongyu scientific and technological company; the color changing temperature of the temperature sensing color changing material is 43 ℃; the average particle size of the temperature-sensitive color-changing powder is 8 mu m; the thickness of the shell is 150 nm.
The temperature-sensitive color-changing powder is subjected to surface modification treatment, and the selected surface modifier is an aminosilane coupling agent purchased from excelsior chemical company; the surface modification treatment step comprises uniformly spraying the silane coupling agent with the concentration of 0.6 wt.% on the surface of the temperature-sensitive color-changing powder, uniformly mixing, and drying the modified temperature-sensitive color-changing powder at 60 ℃ for 30 min; preparing temperature-sensitive color-changing powder with modified surface;
the silica microspheres are hollow silica microspheres which are purchased from Ongxing novel carbon material Hezhou Co., Ltd, 60676-86-0; the average particle size of the silicon dioxide microspheres is 150 nm;
the product A prepared by using the thermochromic material has the following preparation process:
1) dissolving 0.3 part of UV-9 in 100 parts of ethanol, ultrasonically dissolving uniformly, adding the hollow silica microspheres into a mixed solution, uniformly mixing, vacuumizing at the low temperature of 10 ℃ and ultrasonically dispersing for 30min, taking out from a vacuum device, continuously performing ultrasonic dispersion, simultaneously heating to average 50 ℃, accelerating ethanol volatilization, after the ethanol is basically volatilized, placing the treated silica microspheres in an oven for drying treatment at the temperature of 80 ℃ for 1h to completely volatilize the ethanol, and preparing modified silica microspheres;
2) 0.3 part of thermochromic powder after surface treatment is uniformly mixed with 0.4 part of modified silica microspheres prepared in the step 1), so that the silica microspheres with smaller particle sizes are uniformly adsorbed on the surface of the thermochromic powder by virtue of high specific surface area adsorption capacity, and bonding is formed between the thermochromic powder and the silica surface through Si-O bonds on the surface of the thermochromic powder, so that the particles of the silica microspheres can be bonded on the surface of the thermochromic powder in a non-continuous manner;
3) dissolving the mixture obtained in the step 2) with an ultraviolet absorbent UV-9(0.3 part) and an antioxidant (0.2 part) in silicone oil (3 parts), and uniformly mixing the mixture and silica gel (A/B gel);
4) and (3) injection molding the mixture obtained in the step 3), wherein the injection molding temperature is 110 ℃, and the injection molding period is 60s, and in addition, the product obtained after injection molding is cooled in cold water, the temperature of the cold water is 30 ℃, and the target product is obtained after cooling.
Example 2
This example differs from example 1 only in that mesoporous silica, which is available from Nanjing Keyed Biotechnology Ltd under the trade designation JK-04-004 and has an average particle size of 100nm, is used instead of mesoporous hollow silica;
the other raw materials and their preparation process in this example 2 are exactly the same as in example 1.
Example 3
The difference between this example and example 1 is only the difference in the amount of each raw material, and the source and preparation process of the raw materials are exactly the same as those of example 1.
Example 4
The difference between the embodiment and the embodiment 1 is only that the used color-changing powder is a temperature-sensitive color-changing powder with a core-shell structure, the material of the shell is melamine resin, and the content is reversible color-changing organic matter, which is purchased from advanced science and technology limited of Jinhua city; the color changing temperature of the temperature sensing color changing material is 40 ℃; the average particle size of the temperature-sensitive color-changing powder is 10 mu m; the thickness of the shell is 250 nm.
Comparative example 1
This comparative example differs from example 1 only in that no silica microspheres are involved. Other raw material sources and preparation processes are completely the same as those of the example 1.
Comparative example 2
The present comparative example differs from the examples only in that no modified temperature-sensitive toner is involved.
The amounts of the raw materials used in the examples and comparative examples of the present application are shown in Table 1.
Table 1: raw material amounts of examples and comparative examples
The products prepared in the examples and comparative examples were identical in size and shape, and the test results are shown in table 2, part 2 xenon arc lamps according to the chinese national standard GB/T16422.2 plastic laboratory light source exposure test method were tested.
Table 2: performance testing of examples and comparative examples
| Test results | Color change effect | Xenon lamp aging resistance | Color difference value Delta E |
| Example 1 | Good taste | Normal color change | 0.21 |
| Example 2 | Is preferably used | Normal color change | 0.33 |
| Example 3 | Good taste | Normal color change | 0.20 |
| Example 4 | Good taste | Normal color change | 0.31 |
| Comparative example 1 | Good taste | Fading and no discoloration | 8.27 |
| Comparative example 2 | Is free of | Fading and no discoloration | 0.25 |
Although the embodiments disclosed in the present application are described above, the descriptions are only for the convenience of understanding the present application, and are not intended to limit the present application. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the disclosure as defined by the appended claims.
Claims (10)
1. The thermochromic material comprises thermochromic powder, an antioxidant, an ultraviolet absorbent, silica microspheres and silicone oil.
2. The thermochromic material according to claim 1, wherein the weight ratio of the thermochromic powder, the antioxidant, the ultraviolet absorber, and the silica microspheres to the silicone oil is (0.05 to 1): (0.1 to 1): (0.05 to 1.5): (0.05 to 0.8): (1 to 8).
3. The thermochromic material of claim 1, wherein the antioxidant is selected from any one or more of antioxidant 168, antioxidant 1010, and antioxidant 626;
optionally, the ultraviolet absorber is selected from any one or more of UVP-327, UVP-531, UVP-327 and UV-9;
optionally, the silicone oil is selected from any one or more of dimethyl silicone oil, vinyl silicone oil and amino silicone oil.
4. The thermochromic material according to any one of claims 1 to 3, wherein the particle diameter of the thermochromic powder is 1 μm to 15 μm; optionally, the temperature-sensitive color-changing powder is a core-shell structure, and the thickness of a transparent shell in the core-shell structure is 100nm to 400 nm;
optionally, the temperature-sensitive color-changing powder has a color-changing temperature of 35 ℃ to 45 ℃;
optionally, the temperature-sensitive color-changing powder is subjected to surface modification treatment; optionally, the modifier selected for the surface modification treatment is any one or more of an amino silane coupling agent, a trialkoxy silane coupling agent and a dialkoxy coupling agent; optionally, the surface modification treatment comprises the following steps: uniformly mixing the surface of the thermochromic powder with the modifier, wherein the modifier is a modifier solution with the concentration of 0.5 wt.% to 1.0 wt.%, and then drying the modified thermochromic powder at the drying temperature of 60 ℃ to 90 ℃ for 20min to 60 min.
5. The thermochromic material according to any one of claims 1 to 3, wherein the silica microspheres are mesoporous silica microspheres; optionally, the silica microspheres are hollow silica microspheres;
optionally, the silica microspheres have a particle size of 80nm to 300 nm; optionally, the silica microspheres are further subjected to surface modification treatment, and the surface modification treatment comprises uniformly mixing a part of the ultraviolet absorbent with the silica microspheres.
6. The thermochromic material of claim 5, wherein the surface modification treatment comprises:
uniformly mixing a mixture obtained by mixing the ultraviolet absorbent and a solvent with the silicon dioxide microspheres, and finishing surface modification treatment after the solvent is volatilized;
optionally, the uniformly mixing comprises ultrasonically dispersing for 20min to 40min under vacuum conditions of 5 ℃ to 20 ℃;
optionally, the volatilizing operation comprises continuing ultrasonic dispersion after the mixing is uniform and heating to 40 ℃ to 60 ℃, and drying for 1h to 2h at 80 ℃ to 100 ℃ after the solvent is substantially volatilized.
7. The method of producing the thermochromic material according to any one of claims 1 to 5, comprising the steps of:
1) uniformly mixing the temperature-sensitive color-changing powder with the silicon dioxide microspheres to obtain a mixture 1;
2) and uniformly mixing the mixture 1 with the ultraviolet absorbent, the antioxidant and the silicone oil to obtain the thermochromic material.
8. A thermochromic article comprising a substrate and the thermochromic material of any one of claims 1 to 5; the substrate is selected from any one or more of silica gel, thermoplastic materials and thermosetting materials; optionally, the silica gel is selected from one or more of liquid silica gel and solid silica gel.
9. The thermochromic article according to claim 8, wherein the thermochromic article is prepared by injection molding or compression molding.
10. The thermochromic article of claim 9, wherein the injection molding temperature is from 100 ℃ to 150 ℃ and the injection molding cycle is from 60s to 250 s;
optionally, cooling in water of 10-40 ℃ after injection molding, and cooling to obtain the color-changing product.
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Cited By (3)
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| CN114672169A (en) * | 2022-03-22 | 2022-06-28 | 湖南航天三丰科工有限公司 | Temperature-sensitive color-changing agent and preparation method and application thereof |
| CN115349745A (en) * | 2022-09-26 | 2022-11-18 | 蚌埠学院 | Preparation method of temperature-sensitive color-changing cup |
| CN115683382A (en) * | 2022-10-28 | 2023-02-03 | 江南大学 | Intelligent color-changing fabric based on heartbeat emotion recognition and preparation method thereof |
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Cited By (4)
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| CN115683382A (en) * | 2022-10-28 | 2023-02-03 | 江南大学 | Intelligent color-changing fabric based on heartbeat emotion recognition and preparation method thereof |
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