CN115466611A - Thermochromic particle and preparation method thereof, thermochromic coating and application thereof - Google Patents
Thermochromic particle and preparation method thereof, thermochromic coating and application thereof Download PDFInfo
- Publication number
- CN115466611A CN115466611A CN202211255213.XA CN202211255213A CN115466611A CN 115466611 A CN115466611 A CN 115466611A CN 202211255213 A CN202211255213 A CN 202211255213A CN 115466611 A CN115466611 A CN 115466611A
- Authority
- CN
- China
- Prior art keywords
- thermochromic
- phase mixture
- water
- oil
- urea
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002245 particle Substances 0.000 title claims abstract description 59
- 239000011248 coating agent Substances 0.000 title claims abstract description 40
- 238000000576 coating method Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 35
- 229920001807 Urea-formaldehyde Polymers 0.000 claims abstract description 32
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000002270 dispersing agent Substances 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 18
- 239000000839 emulsion Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000012071 phase Substances 0.000 claims description 66
- 238000000034 method Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 16
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 15
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical group CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 14
- 230000008859 change Effects 0.000 claims description 12
- LIZLYZVAYZQVPG-UHFFFAOYSA-N (3-bromo-2-fluorophenyl)methanol Chemical compound OCC1=CC=CC(Br)=C1F LIZLYZVAYZQVPG-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 239000008098 formaldehyde solution Substances 0.000 claims description 7
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 6
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 7
- 230000001681 protective effect Effects 0.000 abstract description 7
- 239000011258 core-shell material Substances 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 6
- 230000032683 aging Effects 0.000 abstract description 4
- 239000012065 filter cake Substances 0.000 description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000012153 distilled water Substances 0.000 description 9
- 239000012752 auxiliary agent Substances 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- AOMUHOFOVNGZAN-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)dodecanamide Chemical compound CCCCCCCCCCCC(=O)N(CCO)CCO AOMUHOFOVNGZAN-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1088—Heterocyclic compounds characterised by ligands containing oxygen as the only heteroatom
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to a thermochromic particle and a preparation method thereof, and a thermochromic coating and application thereof. The preparation method comprises the steps of mixing the thermochromic material with fatty alcohol, adding the oily solvent and the oil-soluble dispersing agent to obtain an oil phase mixture, forming the thermochromic core-shell structure with the thermochromic material as an inner core and the fatty alcohol as a wall material in the oil phase mixture, stirring and mixing the oil phase mixture and the water phase mixture containing the urea-formaldehyde prepolymer and the water-soluble dispersing agent, and reacting the obtained emulsion under a certain condition to enable the urea-formaldehyde polymer to form a protective film on the surface of the thermochromic core-shell structure. The thermochromic particles are prepared into a coating and coated on the power equipment, so that whether the power equipment has serious heating condition or not can be visually and dynamically monitored in real time without manual detection operation. The urea-formaldehyde polymer forms a layer of protective film on the surface of the thermochromic particles, so that the ultraviolet aging resistance is improved, and the water resistance and oil resistance of the thermochromic material are improved.
Description
Technical Field
The invention relates to the field of temperature monitoring, in particular to thermochromic particles and a preparation method thereof, a thermochromic coating and application thereof.
Background
During the operation of the power system, thermal failure of the power equipment is very likely to occur due to the influence of various factors. Thermal faults may occur at different parts of various power equipment, such as cable joints, bus contacts, switch contacts, transformers, high-voltage switches, bushings, disconnectors, zinc oxide arresters, and the like. Thermal failures of such equipment can endanger the personal safety of the personnel and equipment safety of the substation staff, and also cause economic losses. Therefore, it is necessary to check the power equipment on a daily basis and to find the heat generation of the power equipment.
The traditional heating condition inspection mode mainly depends on detecting workers to use the thermal infrared imager to regularly inspect equipment, and early warning is carried out when abnormal temperature is found. However, the method of using the infrared thermal imager for inspection can only detect the instantaneous temperature of the device, and cannot perform dynamic monitoring in real time. In the measurement process, time intervals, measurement positions, and test angles vary from person to person, and it is difficult to achieve standardized operations, and there are human factors that lead to erroneous detection and lack of measurement.
Disclosure of Invention
Based on the above, it is necessary to provide a thermochromic particle, a preparation method thereof, a thermochromic coating and an application thereof, so as to solve the problems that the dynamic monitoring cannot be realized and the standardized operation is difficult to realize by using a thermal infrared imager for inspection.
One of the objects of the present invention is to provide a method for preparing thermochromic particles, wherein the scheme is as follows:
a method of preparing thermochromic particles comprising the steps of:
mixing a thermochromic material with fatty alcohol, adding an oily solvent and an oil-soluble dispersing agent, heating, and stirring for dissolving to obtain an oil-phase mixture;
obtaining an aqueous solution of a urea formaldehyde prepolymer, adding a water-soluble dispersant, and stirring until the water-soluble dispersant is dissolved to obtain a water-phase mixture;
stirring and mixing the oil phase mixture and the water phase mixture at 55-65 ℃ for 0.5h to obtain emulsion;
adjusting the pH value of the emulsion to 7.5-8.0, and reacting at 55-65 ℃ for 1-1.5 h to obtain a suspension;
and filtering, washing and drying the suspension to obtain the thermochromic particles.
In one embodiment, the thermochromic material is a mixture of crystal violet lactone and bisphenol a.
In one embodiment, the thermochromic material has a color change temperature of 65 ℃ to 70 ℃.
In one embodiment, the fatty alcohol is selected from at least one of dodecanol, tetradecanol, hexadecanol, octadecanol.
In one embodiment, the oily solvent is butanone.
In one embodiment, the thermochromic material is 20-30% by weight of the oil phase mixture, the fatty alcohol is 10-15% by weight of the oil phase mixture, and the urea formaldehyde prepolymer is 70-75% by weight of the water phase mixture.
In one embodiment, the mass ratio of the oil phase mixture to the water phase mixture is (1.3-1.7) to 1.
In one embodiment, the preparation method of the urea formaldehyde prepolymer comprises the following steps:
dissolving urea in formaldehyde solution, regulating pH value to 7.5-8.0, and reacting at 55-65 deg.c for 1-1.5 hr.
Another object of the present invention is to provide a thermochromic particle, which is formulated as follows:
thermochromic particles prepared by the preparation method of any one of the embodiments.
Still another object of the present invention is to provide a thermochromic coating material, which has the following scheme:
a thermochromic paint includes a dispersion solvent and the color-changing particles dispersed in the dispersion solvent.
It is a further object of the present invention to provide the use of said thermochromic coating for early warning of heating failures in electrical equipment.
Compared with the existing scheme, the preparation method of the thermochromic particles has the following beneficial effects:
the preparation method of the thermochromic particles comprises the steps of mixing a thermochromic material with fatty alcohol, adding an oily solvent and an oil-soluble dispersing agent to obtain an oil phase mixture, forming a thermochromic core-shell structure with the thermochromic material as an inner core and the fatty alcohol as a wall material in the oil phase mixture, stirring and mixing the oil phase mixture and a water phase mixture containing a urea-formaldehyde prepolymer and a water-soluble dispersing agent, and reacting the obtained emulsion under a certain condition to enable the urea-formaldehyde polymer to form a protective film on the surface of the thermochromic core-shell structure.
The thermochromic particles prepared by the preparation method can generate a color change phenomenon after being heated to a certain temperature, and are prepared into a coating to form the thermochromic coating which is coated on power equipment, so that the large-area coverage of the power equipment can be realized, the thermochromic coating can be deployed in an inaccessible area and a concealed area of an infrared thermal imager, a worker can visually and dynamically monitor whether the power equipment has serious heating conditions or not in real time, manual detection operation is not needed, the interference of human factors on detection accuracy is reduced, and early warning information is transmitted in time. Compared with the method of directly adding the thermochromic material into the coating, the preparation method enables the urea-formaldehyde polymer to form a layer of protective film on the surface of the thermochromic particle, can greatly improve the ultraviolet aging resistance, improves the water resistance and oil resistance of the thermochromic material, and can be applied to electronic equipment working outdoors for a long time.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following more detailed description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The preparation method of the thermochromic particles provided by one embodiment of the invention comprises the following steps of:
step S1, mixing the thermochromic material with fatty alcohol, adding an oily solvent and an oil-soluble dispersing agent, heating, stirring and dissolving to obtain an oil phase mixture.
In one example, the thermochromic material is a mixture of crystal violet lactone and bisphenol a. In one example, the mass ratio of crystal violet lactone to bisphenol A is 1: (15-25). In some specific examples, the ratio of crystal violet lactone to bisphenol A is 1: 15, 1: 17, 1: 18, 1: 19, 1: 20, 1: 21, 1: 22, 1: 23, 1: 24, 1: 25 by mass.
The thermochromic material has the advantages of high sensitivity, strong timeliness and quick color development, and is favorable for realizing encapsulation.
It is understood that in other examples, the thermochromic material is not limited to crystal violet lactone and bisphenol a, and may be selected according to the desired color change temperature.
In one example, the thermochromic material has a color change temperature of 65-70 ℃ and is suitable for heating early warning of power equipment. Further, in one example, the thermochromic material has a color change temperature of 67 ℃ to 69 ℃. In some specific examples, the thermochromic material has a color change temperature of 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, etc.
In one example, the fatty alcohol is selected from at least one of dodecanol, tetradecanol, hexadecanol, octadecanol.
In one example, the fatty alcohol is stearyl alcohol.
In one example, the oily solvent is butanone.
The oil-soluble dispersant can be oil-soluble dispersant commonly used in the field, such as cellulose acetate butyrate.
In one example, the thermochromic material is 20% to 30% of the oil phase mixture by weight. Further, in one example, the weight fraction of the thermochromic material in the oil phase mixture is 23% to 28%. In some specific examples, the thermochromic material is present in the oil phase mixture at 22%, 24%, 26%, 28%, 29%, 30%, etc. by mass.
In one example, the fatty alcohol is present in the oil phase mixture at a mass fraction of 10% to 15%. Further, in one example, the mass fraction of the fatty alcohol in the oil phase mixture is 12% to 11%. In some particular examples, the fatty alcohol is present in the oil phase mixture at 10%, 11%, 12%, 13%, 11%, 15%, etc. by mass.
And S2, obtaining an aqueous solution of the urea-formaldehyde prepolymer, adding a water-soluble dispersant, and stirring until the water-soluble dispersant is dissolved to obtain a water-phase mixture.
In one example, the mass fraction of the urea formaldehyde prepolymer in the aqueous phase mixture is 70% to 75%. Further, in one example, the mass fraction of the urea-formaldehyde prepolymer in the aqueous phase mixture is 71% to 74%. In some particular examples, the mass fraction of urea formaldehyde prepolymer in the aqueous phase mixture is 70%, 71%, 72%, 73%, 74%, 75%, etc.
The water-soluble dispersant can be selected from water-soluble dispersants commonly used in the art, such as sodium dodecyl benzene sulfonate, lauroyl diethanol amine, and the like.
In one example, a method of preparing a urea formaldehyde prepolymer includes the steps of:
dissolving urea in formaldehyde solution, regulating pH value to 7.5-8.0, and reacting at 55-65 deg.c for 1-1.5 hr.
The prepared urea-formaldehyde polymer can form a layer of protective film on the surface of the thermochromic particles, can greatly improve the ultraviolet aging resistance, simultaneously improves the water resistance and the oil resistance of the thermochromic material, and can be applied to electronic equipment working outdoors all the year round.
In one example, in the above method for preparing the urea formaldehyde prepolymer, the pH of the reaction liquid is adjusted to 7.7 to 7.9. In some specific examples, the pH of the reaction solution is adjusted to 7.5, 7.6, 7.7, 7.8, 7.9, 8.0, and the like.
In one example, in the above method for preparing the urea formaldehyde prepolymer, the reaction temperature is 58 ℃ to 62 ℃. In some specific examples, the reaction temperature is 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃ and the like.
In one example, in the preparation method of the urea formaldehyde prepolymer, the reaction time is 1.2 h-1.4 h. In some specific examples, the reaction time is 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, and the like.
And step S3, stirring and mixing the oil phase mixture and the water phase mixture at the temperature of 55-65 ℃ to obtain emulsion.
In one example, in step S3, the temperature condition for the agitation and mixing is 58 to 62 ℃. In some specific examples, the temperature conditions for the stirring and mixing in step S3 are 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃ and the like.
In one example, in step S3, the stirring and mixing time is 0.5h to 2h. Further, in one example, in step S3, the stirring and mixing time is 1 to 2 hours. In some specific examples, in step S3, the time for stirring and mixing is 0.5h, 1h, 1.5h, 2h, and the like.
In one example, in step S3, the mass ratio of the oil phase mixture to the water phase mixture is (1.3-1.7): 1. Further, in one example, in step S3, the mass ratio of the oil phase mixture to the water phase mixture is (1.4-1.6): 1. In some specific examples, in step S3, the mass ratio of the oil phase mixture to the water phase mixture is 1.3: 1, 1.4: 1, 1.5: 1, 1.6: 1, 1.7: 1, and the like.
And S4, adjusting the pH value of the emulsion to 7.5-8.0, and reacting for 1-1.5 h at the temperature of 55-65 ℃ to obtain a suspension.
In one example, in step S4, the pH of the reaction solution is adjusted to 7.7 to 7.9. In some specific examples, in step S4, the pH of the reaction solution is adjusted to 7.5, 7.6, 7.7, 7.8, 7.9, 8.0, and the like.
In one example, in step S4, the temperature of the reaction is from 58 ℃ to 62 ℃. In some specific examples, in step S4, the temperature of the reaction is 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃ and the like.
In one example, in step S4, the reaction time is 1.2h to 1.4h. In some specific examples, in step S4, the reaction time is 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, and the like.
The acid used in step S4 may be, for example, acetic acid.
And S5, filtering, washing and drying the suspension to obtain the thermochromic particles.
The filter cake of the suspension filtration can be washed by ethanol and distilled water. The filtration and washing can be alternately performed for a plurality of times. The drying method is, for example, air drying, and vacuum drying at 30 deg.C for 24 hr.
In one example, the thermochromic particles are prepared to have a particle size of 40 μm to 80 μm. Further, in one example, the thermochromic particles are prepared to have a particle size of 50 μm to 70 μm. In some specific examples, the thermochromic particles are prepared to have a particle size of 40 μm to 70 μm, 40 μm to 60 μm, 40 μm to 50 μm, 50 μm to 80 μm, 50 μm to 70 μm, 50 μm to 60 μm, 60 μm to 80 μm, 60 μm to 70 μm, 70 μm to 80 μm, and the like.
The preparation method of the thermochromic particles comprises the steps of mixing a thermochromic material with fatty alcohol, adding an oily solvent and an oil-soluble dispersing agent to obtain an oil phase mixture, forming a thermochromic core-shell structure with the thermochromic material as an inner core and the fatty alcohol as a wall material in the oil phase mixture, stirring and mixing the oil phase mixture and a water phase mixture containing a urea-formaldehyde prepolymer and a water-soluble dispersing agent, and reacting the obtained emulsion under a certain condition to enable the urea-formaldehyde polymer to form a protective film on the surface of the thermochromic core-shell structure.
The thermochromic particles prepared by the preparation method can generate a color change phenomenon after being heated to a certain temperature, and are prepared into a coating to form the thermochromic coating which is coated on power equipment, so that the large-area coverage of the power equipment can be realized, the thermochromic coating can be deployed in an inaccessible area and a concealed area of an infrared thermal imager, a worker can visually and dynamically monitor whether the power equipment has serious heating conditions or not in real time, manual detection operation is not needed, the interference of human factors on detection accuracy is reduced, and early warning information is transmitted in time. Compared with the method of directly adding the thermochromic material into the coating, the preparation method enables the urea-formaldehyde polymer to form a layer of protective film on the surface of the thermochromic particles, can greatly improve the ultraviolet aging resistance and simultaneously improve the water resistance and oil resistance of the thermochromic material, and can be applied to electronic equipment working outdoors all the year round.
Further, the present invention also provides a thermochromic particle prepared by any one of the above-exemplified methods for preparing a thermochromic particle.
Further, the present invention also provides a thermochromic coating material including a dispersion solvent and the thermochromic particles of any of the above examples, the thermochromic particles being dispersed in the dispersion solvent.
The thermochromic coating described above contains the thermochromic particles of any of the examples described above, and thus can obtain corresponding advantageous effects. In one example, the thermochromic particles are present in the thermochromic coating in an amount of 20% to 25% by weight. Further, in one example, the thermochromic particles are present in the thermochromic coating in a mass fraction of 22% to 24%. In some specific examples, the thermochromic particles are present in the thermochromic coating at 20%, 21%, 22%, 23%, 24%, 25%, etc. by mass.
In one example, the dispersion solvent is selected from at least one of benzene, toluene, xylene, and ethyl acetate.
In one example, a method of preparing a thermochromic coating includes the steps of: adding the thermochromic particles into the dispersion solvent, and uniformly stirring.
The following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples, and it should be understood that the scope of the present invention is summarized by the appended claims, and a person skilled in the art should realize that certain changes made to the embodiments of the present invention, in light of the inventive concept, are intended to be covered by the spirit and scope of the claims of the present invention.
Example 1
The embodiment provides a preparation method of thermochromic particles, which comprises the following steps:
step 1, mixing 20g of crystal violet lactone, 400g of bisphenol A and 200g of octadecanol, adding the mixture into 1000g of butanone, adding 300g of oil-soluble dispersing agent, heating to 60 ℃, and stirring until the mixture is dissolved to obtain an oil phase mixture.
And 2, dissolving 18g of urea in 200ml of formaldehyde solution, adding 0.1mol/L NaOH aqueous solution to adjust the pH value to 8.0, slowly heating to 60 ℃, and carrying out heat preservation reaction for 1.2 hours to obtain the urea-formaldehyde prepolymer. Diluting the obtained urea formaldehyde prepolymer with a proper amount of distilled water, adding 270g of water-soluble dispersing agent, and stirring to dissolve the water-soluble auxiliary agent to obtain a water-phase mixture.
And 3, adding the oil phase mixture into the water phase mixture under the stirring state, and mixing at 60 ℃, wherein the mass ratio of the water phase mixture to the oil phase mixture is 60: 40, so as to obtain an emulsion.
And 4, adding acetic acid into the emulsion, adjusting the pH value to 7.8, and reacting at 60 ℃ for 1.5 hours to obtain a suspension.
And 5, filtering the suspension to obtain a filter cake, washing the filter cake with ethanol and distilled water for several times in sequence, naturally drying the filter cake, and drying the filter cake in vacuum at 30 ℃ for 24 hours without drying the filter cake too much to obtain the thermochromic particles.
Example 2
The embodiment provides a preparation method of thermochromic particles, which comprises the following steps:
step 1, mixing 20g of crystal violet lactone, 350g of bisphenol A and 200g of octadecanol, adding the mixture into 1000g of butanone, adding 300g of oil-soluble dispersing agent, heating to 60 ℃, and stirring until the mixture is dissolved to obtain an oil phase mixture.
And 2, dissolving 18g of urea in 200ml of formaldehyde solution, adding 0.1mol/L of NaOH aqueous solution to adjust the pH value to 8.0, slowly heating to 60 ℃, and carrying out heat preservation reaction for 1.2h to obtain the urea formaldehyde prepolymer. Diluting the obtained urea formaldehyde prepolymer with a proper amount of distilled water, adding 270g of water-soluble dispersing agent, and stirring to dissolve the water-soluble auxiliary agent to obtain a water-phase mixture.
And 3, adding the oil phase mixture into the water phase mixture under the stirring state, and mixing at 60 ℃, wherein the mass ratio of the water phase mixture to the oil phase mixture is 60: 40, so as to obtain an emulsion.
And 4, adding acetic acid into the emulsion, adjusting the pH value to 7.5, and reacting at 65 ℃ for 1h to obtain a suspension.
And 5, filtering the suspension to obtain a filter cake, washing the filter cake with ethanol and distilled water for several times in sequence, naturally drying the filter cake, and drying the filter cake in vacuum at the temperature of 30 ℃ for 24 hours without drying the filter cake too much to obtain the thermochromic particles.
Example 3
The embodiment provides a preparation method of thermochromic particles, which comprises the following steps:
step 1, mixing 20g of crystal violet lactone, 450g of bisphenol A and 200g of octadecanol, adding the mixture into 1000g of butanone, adding 300g of oil-soluble dispersing agent, heating to 60 ℃, and stirring until the mixture is dissolved to obtain an oil phase mixture.
And 2, dissolving 18g of urea in 200ml of formaldehyde solution, adding 0.1mol/L of NaOH aqueous solution to adjust the pH value to 8.0, slowly heating to 60 ℃, and carrying out heat preservation reaction for 1.2h to obtain the urea formaldehyde prepolymer. Diluting the obtained urea formaldehyde prepolymer with a proper amount of distilled water, adding 270g of water-soluble dispersing agent, and stirring to dissolve the water-soluble auxiliary agent to obtain a water-phase mixture.
And 3, adding the oil phase mixture into the water phase mixture under the stirring state, and mixing at 60 ℃, wherein the mass ratio of the water phase mixture to the oil phase mixture is 50: 50, so as to obtain an emulsion.
And 4, adding acetic acid into the emulsion, adjusting the pH value to 7.8, and reacting at 55 ℃ for 1.5h to obtain a suspension.
And 5, filtering the suspension to obtain a filter cake, washing the filter cake with ethanol and distilled water for several times in sequence, naturally drying the filter cake, and drying the filter cake in vacuum at the temperature of 30 ℃ for 24 hours without drying the filter cake too much to obtain the thermochromic particles.
Example 4
The embodiment provides a preparation method of thermochromic particles, which comprises the following steps:
step 1, mixing 20g of crystal violet lactone, 400g of bisphenol A and 300g of octadecanol, adding the mixture into 1000g of butanone, adding 300g of oil-soluble dispersing agent, heating to 60 ℃, and stirring until the mixture is dissolved to obtain an oil phase mixture.
And 2, dissolving 18g of urea in 200ml of formaldehyde solution, adding 0.1mol/L of NaOH aqueous solution to adjust the pH value to 8.0, slowly heating to 60 ℃, and carrying out heat preservation reaction for 1.2h to obtain the urea formaldehyde prepolymer. Diluting the obtained urea formaldehyde prepolymer with a proper amount of distilled water, adding 270g of water-soluble dispersing agent, and stirring to dissolve the water-soluble auxiliary agent to obtain a water-phase mixture.
And 3, adding the oil phase mixture into the water phase mixture under the stirring state, and mixing at 60 ℃, wherein the mass ratio of the water phase mixture to the oil phase mixture is 50: 50, so as to obtain an emulsion.
And 4, adding acetic acid into the emulsion, adjusting the pH value to 7.5, and reacting at 60 ℃ for 1.5 hours to obtain a suspension.
And 5, filtering the suspension to obtain a filter cake, washing the filter cake with ethanol and distilled water for several times in sequence, naturally drying the filter cake, and drying the filter cake in vacuum at the temperature of 30 ℃ for 24 hours without drying the filter cake too much to obtain the thermochromic particles.
Example 5
The embodiment provides a preparation method of a thermochromic coating, which comprises the following steps:
the thermochromic particles prepared in example 1 were dispersed in toluene to obtain a thermochromic coating, and the mass fraction of the thermochromic particles in the thermochromic coating was 20%.
The thermochromic coating of this example had a color change temperature of 66 ℃.
Example 6
The embodiment provides a preparation method of a thermochromic coating, which comprises the following steps:
the thermochromic particles prepared in example 2 were dispersed in toluene to obtain a thermochromic coating, and the mass fraction of the thermochromic particles in the thermochromic coating was 20%.
The thermochromic coating of this example had a color change temperature range of 65 ℃.
Example 7
The embodiment provides a preparation method of a thermochromic coating, which comprises the following steps:
the thermochromic particles prepared in example 3 were dispersed in toluene to obtain a thermochromic coating, and the mass fraction of the thermochromic particles in the thermochromic coating was 25%.
The thermochromic coating of this example had a color change temperature of 66 ℃.
Example 8
The embodiment provides a preparation method of a thermochromic coating, which comprises the following steps:
the thermochromic particles prepared in example 4 were dispersed in toluene to obtain a thermochromic coating, and the mass fraction of the thermochromic particles in the thermochromic coating was 25%.
The thermochromic coating of this example had a color change temperature of 66 ℃.
Example 9
When a certain local distribution network power equipment has a thermal fault, the on-site rush repair proves that the fixed hardware fitting of the A-phase equipment wire clamp on the wire inlet side of the distribution network transformer is corroded and loosened, so that the contact resistance is increased and the heating is caused, and the bolt is replaced and then the bolt is fixed and recovered to be normal. The accident shows the defect of regular infrared temperature measurement, and all-weather early warning cannot be realized.
The thermochromic coating prepared in the embodiment 5 is coated on the newly-configured bolt, and in later-stage operation and maintenance, an inspector can effectively prevent related faults by observing whether the bolt changes color or not.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the patent of the invention is subject to the appended claims, and the description can be used for explaining the contents of the claims.
Claims (10)
1. A method for preparing thermochromic particles is characterized by comprising the following steps:
mixing a thermochromic material with fatty alcohol, adding an oily solvent and an oil-soluble dispersing agent, heating, and stirring for dissolving to obtain an oil-phase mixture;
obtaining an aqueous solution of a urea formaldehyde prepolymer, adding a water-soluble dispersant, and stirring until the water-soluble dispersant is dissolved to obtain a water-phase mixture;
stirring and mixing the oil phase mixture and the water phase mixture at 55-65 ℃ to obtain emulsion;
adjusting the pH value of the emulsion to 7.5-8.0, and reacting at 55-65 ℃ for 1-1.5 h to obtain a suspension;
and filtering, washing and drying the suspension to obtain the thermochromic particles.
2. The method of claim 1, wherein the thermochromic material is a mixture of crystal violet lactone and bisphenol a.
3. The method of claim 1, wherein the thermochromic material has a color change temperature of 65 ℃ to 70 ℃.
4. The method of claim 1, wherein the method of preparation satisfies one or more of the following characteristics:
the fatty alcohol is at least one of dodecanol, tetradecanol, hexadecanol and octadecanol;
the oily solvent is butanone.
5. The method according to any one of claims 1 to 4, wherein the thermochromic material is present in the oil phase mixture at a mass fraction of 20% to 30%, the fatty alcohol is present in the oil phase mixture at a mass fraction of 10% to 15%, and the urea-formaldehyde prepolymer is present in the aqueous phase mixture at a mass fraction of 70% to 75%.
6. The method according to claim 5, wherein the mass ratio of the oil-phase mixture to the water-phase mixture is (1.3-1.7) to 1.
7. The method of any one of claims 1 to 4, 6, wherein the method of preparing the urea formaldehyde prepolymer comprises the steps of:
dissolving urea in formaldehyde solution, regulating pH value to 7.5-8.0, and reacting at 55-65 deg.c for 1-1.5 hr.
8. Thermochromic particles, which are obtained by the production method according to any one of claims 1 to 7.
9. A thermochromic paint, comprising a dispersion solvent and the color-changing particles according to claim 8, wherein the color-changing particles are dispersed in the dispersion solvent.
10. Use of the thermochromic coating according to claim 9 for warning of heating faults in electrical equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211255213.XA CN115466611A (en) | 2022-10-13 | 2022-10-13 | Thermochromic particle and preparation method thereof, thermochromic coating and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211255213.XA CN115466611A (en) | 2022-10-13 | 2022-10-13 | Thermochromic particle and preparation method thereof, thermochromic coating and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115466611A true CN115466611A (en) | 2022-12-13 |
Family
ID=84336422
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211255213.XA Pending CN115466611A (en) | 2022-10-13 | 2022-10-13 | Thermochromic particle and preparation method thereof, thermochromic coating and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115466611A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170041A (en) * | 2015-07-13 | 2015-12-23 | 西安理工大学 | Reversible thermochromic microcapsule pigment preparation method |
| CN110964498A (en) * | 2019-12-13 | 2020-04-07 | 天津优米优科技有限公司 | Thermochromic capsule and preparation method thereof |
| CN112473580A (en) * | 2020-12-21 | 2021-03-12 | 天津工业大学 | Preparation method of thermochromic capsules |
| CN112835279A (en) * | 2019-11-25 | 2021-05-25 | 广东乐普泰新材料科技有限公司 | Preparation method of thermochromic anti-counterfeiting ink powder |
| US20220145106A1 (en) * | 2019-04-02 | 2022-05-12 | Wuhan Institutes Of Advanced Technology, Chinese Academy Of Sciences | Microcapsule Type Thermochromic Pigment and Preparation Method and Use Thereof, Thermochromic Ink and Use Thereof |
-
2022
- 2022-10-13 CN CN202211255213.XA patent/CN115466611A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170041A (en) * | 2015-07-13 | 2015-12-23 | 西安理工大学 | Reversible thermochromic microcapsule pigment preparation method |
| US20220145106A1 (en) * | 2019-04-02 | 2022-05-12 | Wuhan Institutes Of Advanced Technology, Chinese Academy Of Sciences | Microcapsule Type Thermochromic Pigment and Preparation Method and Use Thereof, Thermochromic Ink and Use Thereof |
| CN112835279A (en) * | 2019-11-25 | 2021-05-25 | 广东乐普泰新材料科技有限公司 | Preparation method of thermochromic anti-counterfeiting ink powder |
| CN110964498A (en) * | 2019-12-13 | 2020-04-07 | 天津优米优科技有限公司 | Thermochromic capsule and preparation method thereof |
| CN112473580A (en) * | 2020-12-21 | 2021-03-12 | 天津工业大学 | Preparation method of thermochromic capsules |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108169615B (en) | Optical CT-based phase failure detection method for starting standby transformer | |
| CN106324321A (en) | Monitoring method and monitoring device for resistive current of zinc oxide lightning arrester | |
| CN106990304A (en) | Power capacitor running status on-line monitoring method based on capacitance | |
| CN112198390B (en) | Real-time evaluation method and system for health state of capacitor bank | |
| CN106324415B (en) | Double-winding synchronous wind-driven generator interturn short-circuit failure diagnosing method and monitoring method | |
| CN103308805A (en) | Overhauling method and overhauling system for state of distribution transformer | |
| CN109827679B (en) | Distribution transformer winding temperature rise online monitoring system and online monitoring method | |
| CN204679557U (en) | Judge that AC signal seals in the detection system of straight-flow system | |
| CN107219453A (en) | A kind of substation relay protection hidden failure diagnostic method based on Multidimensional and Hybrid amount | |
| CN109613374A (en) | A kind of capacitor integrated on-line monitoring method based on redundant data | |
| CN111257690B (en) | Fault diagnosis and positioning method for cross-connection high-voltage cable sheath protector | |
| CN111077362A (en) | Method and system for online monitoring running state of reactor in capacitor assembly | |
| CN116381460A (en) | Power supply operation safety supervision system for vehicle-mounted shelter CT | |
| CN115466611A (en) | Thermochromic particle and preparation method thereof, thermochromic coating and application thereof | |
| CN111679163A (en) | On-line insulation monitoring device for turns of dry-type reactor | |
| CN212433321U (en) | On-line insulation monitoring device for turns of dry-type reactor | |
| CN109669062A (en) | A kind of automatic detection elastic test macro of bolt | |
| CN109000819A (en) | A kind of temperature-sensing color-changing material and distribution line arrester Damage by Short Circuit indicating means | |
| CN115549042A (en) | Intelligent power distribution system | |
| CN108761297A (en) | A kind of dry-type air-core reactor partial discharges fault on-line computing model based on high-frequency signal | |
| Jiang et al. | Influence of contamination on deteriorated insulators detection with infrared imaging method | |
| CN212031587U (en) | Reactor running state on-line monitoring system in power capacitor complete equipment | |
| Li et al. | Condition monitoring of high voltage equipment in smart grid | |
| CN208780776U (en) | Dry-type air-core reactor partial discharges fault on-line computing model based on high-frequency signal | |
| CN112327076A (en) | Method for diagnosing running state of series dry type reactor based on tan delta difference |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |