CN117085603A - Method for monitoring failure of kinematic pair in real time - Google Patents
Method for monitoring failure of kinematic pair in real time Download PDFInfo
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- CN117085603A CN117085603A CN202311348888.3A CN202311348888A CN117085603A CN 117085603 A CN117085603 A CN 117085603A CN 202311348888 A CN202311348888 A CN 202311348888A CN 117085603 A CN117085603 A CN 117085603A
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/12—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance
- G01K11/16—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance of organic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- 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
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Measuring Temperature Or Quantity Of Heat (AREA)
Abstract
The invention provides a method for monitoring failure of a kinematic pair in real time. The method comprises the following steps: the high-temperature irreversible thermochromic microcapsule is arranged on the surface of a kinematic pair, when the surface temperature of the kinematic pair changes to the color changing temperature of the high-temperature irreversible thermochromic microcapsule, the high-temperature irreversible thermochromic microcapsule changes color to realize real-time monitoring of whether the kinematic pair fails, the high-temperature irreversible thermochromic microcapsule comprises a core material and a shell material wrapping the surface of the core material, the core material comprises a color former, a color former and a first organic solvent, the first organic solvent is a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water, and the shell material comprises a polymer. The method provided by the invention adopts the high-temperature irreversible thermochromic microcapsules, can monitor the temperature change range to 80-200 ℃ in real time, can realize the visualization of the temperature change, and can realize the real-time monitoring of the failure of the kinematic pair.
Description
Technical Field
The invention relates to a method for monitoring failure of a kinematic pair in real time, and belongs to the technical field of temperature measuring materials and methods.
Background
In the mechanical and electronic fields, the two components are in direct contact and have a defined connection of relative movements called kinematic pairs. When the kinematic pair approaches failure, the temperature of the friction surface can be rapidly increased, so that whether the kinematic pair fails can be judged according to the temperature of the detection kinematic pair. At present, the main method for detecting the local overheating of a mechanical component or an electronic device is to directly measure the temperature of the device through an infrared device or a temperature sensor, but due to the high cost, the device requires energy supply, is not easy to carry and the like, and is still difficult to use in a large scale in a micro or integrated device. Moreover, most kinematic pairs have a narrow installation space, and cannot be measured by using an infrared device or a temperature sensor.
The thermochromic material is a novel material capable of changing color along with temperature change, and has wide application prospect. The research background of this material can be traced to the beginning of the 60 s of the 20 th century, when researchers found that certain organic molecules could undergo a color change when heated. With the progress of technology and the continuous improvement of demands of people on environmental protection, intelligence and the like, the research of thermochromic materials is also getting more and more attention. Development of thermochromic materials has important significance for real-time monitoring and scientific early warning of local overheating of mechanical parts or electronic devices so as to monitor failure of kinematic pairs, but the improvement of the color-changing temperature is still challenging.
The prior art uses pigments such as ammonium vanadate to prepare coatings that achieve irreversible thermochromic behaviour at 150 ℃. The coating is sprayed on hardware fittings at the parts where the lines contact the heating parts, and the coating changes from white to deep yellow when the heating faults occur. However, during the color change, the loss of thermochromic compounds will limit the range of applications for such coatings. And microcapsule technology is an effective method to solve this problem.
In the prior art, core materials and shell materials of the microcapsules are changed by methods such as emulsion polymerization, solvent volatilization and the like, so that different thermochromic materials are prepared. However, the thermochromic microcapsules synthesized in the prior art have the common defect that the temperature of the color change is low (less than 70 ℃), and the color change is reversible.
Therefore, the present thermochromic materials have at least the following technical problems: the high-temperature color-changing material can not be microencapsulated; the temperature response of the microencapsulated thermochromic material is low.
The development of a method for monitoring the failure of a kinematic pair in real time by adopting microcapsules and realizing temperature change monitoring at high temperature is still one of the problems to be solved in the art.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for monitoring the failure of a kinematic pair in real time. The method provided by the invention adopts the high-temperature irreversible thermochromic microcapsules, can monitor the temperature change range to 80-200 ℃ in real time, can realize the visualization of the temperature change, and can realize the real-time monitoring of the failure of the kinematic pair.
In order to achieve the above object, the present invention provides a method for monitoring a failure of a kinematic pair in real time, the method comprising: the method comprises the steps that a high-temperature irreversible thermochromic microcapsule is arranged on the surface of a kinematic pair, and when the surface temperature of the kinematic pair changes to the color changing temperature of the high-temperature irreversible thermochromic microcapsule, the high-temperature irreversible thermochromic microcapsule changes color, so that whether the kinematic pair fails or not is monitored in real time;
the high-temperature irreversible thermochromic microcapsule comprises a core material and a shell material wrapping the surface of the core material, wherein the core material comprises a color former, a color former and a first organic solvent, the first organic solvent is a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water, and the shell material comprises a polymer.
In the above method, preferably, the high temperature irreversible thermochromic microcapsules are prepared by at least the following steps:
(1) Mixing the shell material, the first organic solvent, the second organic solvent, the color former and the color former to obtain a mixed solution; the first organic solvent is a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water; the second organic solvent is a volatile liquid organic solvent which has a boiling point of 30-60 ℃ and is insoluble in water;
(2) Adding the mixed solution into an aqueous solution of an emulsifier, and stirring for a period of time under the condition that the boiling point temperature of the second organic solvent is 10 ℃ higher than the boiling point temperature of the second organic solvent, so that the second organic solvent is completely volatilized, and a reaction product is obtained;
(3) And (3) carrying out solid-liquid separation, washing and drying on the reaction product to obtain the high-temperature irreversible thermochromic microcapsule.
In the above method, preferably, the first organic solvent is an organic solvent that prevents the developer from contacting the developer through interaction between hydrogen bond and the developer.
In the above method, preferably, the first organic solvent includes one or a combination of several of cyclohexane, dimethyl sulfoxide, triethylamine, 1, 2-dimethoxyethane, trichloroethylene, toluene, 1, 2-trichloroethane, 2-methoxyethanol, ethylene bromide, n-octane, dimethylformamide, cyclohexanone, and the like.
In the above method, preferably, the color former includes one or a combination of several of crystal violet lactone, 6' -diethylamino-2 ' -dibenzylaminofluran, 6' - (diethylamino) -1',2' -benzofluoran, and 7, 7-bis (4- (diethylamino) -2-ethoxyphenyl) furo [3,4-b ] pyridin-5 (7H) -one, and the like.
In the above method, preferably, the color-developing agent includes bisphenol a or the like.
In the above method, preferably, the shell material includes one or a combination of several of Polystyrene (PS), polysulfone (PSF), polymethyl methacrylate (PMMA), polyimide (PI), and the like.
In the above method, preferably, the second organic solvent includes methylene chloride or the like.
In the above method, preferably, the mass ratio of the shell material, the first organic solvent, the color former and the color former is (2 to 6): (4-12): (0.02-0.08): (0.06-0.24).
In the above method, preferably, the mass-to-volume ratio of the shell material to the second organic solvent is (2-6) g:45mL.
In the above method, preferably, the emulsifier includes polyvinyl alcohol (PVA) and/or gum arabic and the like. More preferably, the emulsifier comprises the following components in percentage by mass (1-3): (0.5-1.5) a composition of polyvinyl alcohol and acacia.
In the above method, preferably, the mass-to-volume ratio of the emulsifier to water in the aqueous solution of the emulsifier is (1.5-4.5) g: (200-600) mL.
In the above method, preferably, the mixing volume ratio of the mixed solution to the aqueous solution of the emulsifier is 1: (2-5).
In the above method, preferably, in step (2), the second organic solvent is stirred for 3 to 7 hours under the condition that the boiling point temperature of the second organic solvent is 10 ℃ above the boiling point temperature thereof.
In the above method, preferably, in step (2), the stirring speed is 800-160 rpm.
In the above method, the solid-liquid separation, washing and drying in the step (3) may be performed in a conventional manner in the art. For example, the solid-liquid separation may be performed by suction filtration using a buchner funnel; the washing can be repeatedly performed for a plurality of times by deionized water; the drying adopts freeze drying, and the time can be 12-48 h.
In the above method, preferably, the average particle diameter of the high temperature irreversible thermochromic microcapsules is 5 μm or less.
In the above method, preferably, the color-changing temperature of the high-temperature irreversible thermochromic microcapsule is 80-200 ℃, and the color change is irreversible after the microcapsule returns to room temperature.
In the above method, it is preferable that the high-temperature irreversible thermochromic microcapsules are provided on the surface of the kinematic pair by preparing the high-temperature irreversible thermochromic microcapsules into a paint and applying the paint on the surface of the kinematic pair. When the high-temperature irreversible thermochromic microcapsules are provided on the surface of the kinematic pair, they may be provided on the surfaces of two members or on the surface of one of the two members.
According to a specific embodiment of the present invention, the high temperature irreversible thermochromic microcapsules can be mixed with paint to prepare a coating when they are prepared into a coating. Preferably, the mixing mass ratio of the high temperature irreversible thermochromic microcapsules to the paint is 1: (5-10). The coating can be applied to the surface of the kinematic pair by spraying, but is not limited to spraying. The thickness of the spray coating can be adjusted routinely by those skilled in the art. The components of the kinematic pair include, but are not limited to, mechanical components or electronics, and the like.
In the method of the present invention, the high temperature irreversible thermochromic microcapsules are discolored, meaning that the temperature of the friction surface of the member of the kinematic pair is increased, and further meaning that the kinematic pair is failed or is close to being failed, so that whether the kinematic pair is failed can be monitored in real time by observing whether the surface of the kinematic pair provided with the high temperature irreversible thermochromic microcapsules is discolored or not.
Thermochromic microcapsules of the prior art are formed by coating a shell material with a mixture of an electron donor (i.e., a color former), an electron acceptor (i.e., a color former) and an organic solid phase change material. With the rise of temperature, the organic solid phase change material is melted (the melting point is generally 40-70 ℃), so that an electron donor and an electron acceptor are contacted, electron transfer occurs, and further color change occurs; after the temperature is reduced, the liquid phase change material is solidified and is converted into a solid state, and the color disappears, so that the reversible color change function is realized. The phase transition temperature of the organic solid phase change material determines the color change temperature of the microcapsules.
The technical scheme and the color change mechanism of the invention are completely different from those of the prior art. The invention takes a mixture of an electron donor (namely, a color former), an electron acceptor (namely, a color former) and a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water as a core material, and the mixture is coated in a shell material to form microcapsules. The color change mechanism of the high temperature irreversible thermochromic microcapsules of the present invention is shown in FIG. 1. At lower temperatures, i.e., in the presence of the first organic solvent in the microcapsules, the first organic solvent of the present invention is capable of separating the electron acceptor and the electron donor by a stronger interaction between the hydrogen bond and the electron acceptor, thus rendering them colorless at low temperatures. When the temperature rises and reaches the rapid volatilization temperature of the first organic solvent, the first organic solvent volatilizes, and the electron donor contacts with the electron acceptor to transfer electrons so as to change color; after the temperature is reduced, the first organic solvent is volatilized, so that the color fading can not occur, and the irreversible color change function is realized. The color-changing temperature of the microcapsule is 80-200 ℃, and the color change is irreversible, so that the gap of the high-temperature irreversible thermochromic microcapsule can be filled.
The high-temperature irreversible thermochromic microcapsule can be used for monitoring or displaying the temperature in various fields. For example, the microcapsule is prepared into a coating, and the coating is coated on the surface of a component, so that the local overheating of a mechanical part or an electronic device can be monitored in real time and scientifically early-warned, and the microcapsule can be particularly used as a temperature indicator in the welding process and a material for monitoring the failure of a kinematic pair; the microcapsule can be used as an anti-counterfeiting label or packaging material by being mixed with ink; the microcapsules are embedded in fibers and can be used as intelligent textiles or clothing.
In summary, the invention provides a method for monitoring the failure of a kinematic pair in real time. The microcapsule is prepared by adopting a solvent volatilization method, the microcapsule comprises a core material and a shell material wrapping the surface of the core material, the core material comprises a color former, a color former and a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water, and the shell material comprises a polymer. According to the invention, the volatile liquid organic solvent which has the boiling point of 80-200 ℃ and is insoluble in water is creatively adopted, so that the color change mechanism of the microcapsule is completely different from that of the microcapsule which realizes reversible color change by utilizing solvent phase change in the prior art. The invention successfully prepares the high-temperature irreversible thermochromic microcapsule by utilizing a specific volatile liquid organic solvent and a special color change mechanism. The method for monitoring the failure of the kinematic pair in real time adopts the high-temperature irreversible thermochromic microcapsule, thereby realizing the visual monitoring of the temperature change and the real-time monitoring of the temperature change at high temperature, and further realizing the real-time monitoring of the failure of the kinematic pair.
The technical scheme of the invention has at least the following beneficial effects:
the method for monitoring the failure of the kinematic pair in real time adopts the high-temperature irreversible thermochromic microcapsule, makes up the gap of the high-temperature irreversible thermochromic microcapsule, and solves the problems that the high-temperature thermochromic material cannot be microencapsulated, the temperature response of the microencapsulated thermochromic material is lower, and the like. The method for monitoring the failure of the kinematic pair in real time can realize real-time monitoring of temperature change and visual feedback of temperature signals only by arranging the high-temperature irreversible thermochromic microcapsule on the surface of the kinematic pair, and can judge whether the kinematic pair fails by monitoring the temperature of the friction surface through the high-temperature irreversible thermochromic microcapsule when the kinematic pair approaches failure, thereby being beneficial to the first time observation of the failure condition of the kinematic pair when a worker overhauls equipment, realizing the visualization of temperature change, the real-time monitoring of temperature change when the kinematic pair is high, and having the advantages of simplicity, high efficiency, low cost, capability of monitoring whether the kinematic pair fails in real time and the like.
Drawings
FIG. 1 is a schematic illustration of the color change mechanism of the high temperature irreversible thermochromic microcapsules of the present invention.
Fig. 2 is an effect diagram of the method for monitoring the failure of the kinematic pair in real time in the embodiment 1 and the embodiment 2.
Fig. 3 is SEM image, TEM and EDS elemental analysis results of the high temperature irreversible thermochromic microcapsules of example 1.
FIG. 4 is a graph showing the discoloration effect of the thermochromic microcapsules of example 1 under a digital microscope.
FIG. 5 is a graph showing the macroscopic discoloration effect of the thermochromic microcapsules of example 1.
Fig. 6 is an SEM image of the high temperature irreversible thermochromic microcapsules of example 2.
FIG. 7 is a graph showing the macroscopic discoloration effect of the high temperature irreversible thermochromic microcapsules according to example 2.
Fig. 8 is an SEM image of thermochromic microcapsules of comparative example 1.
FIG. 9 is a graph showing the effect of thermochromic microcapsules of comparative example 1 on macroscopic discoloration.
Fig. 10 is an SEM image of the microcapsules of comparative example 2.
FIG. 11 is a graph showing the macroscopic effect of the microcapsules of comparative example 2.
Detailed Description
The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a method for monitoring the failure of a kinematic pair in real time, which comprises the following steps:
the high-temperature irreversible thermochromic microcapsule is mixed with paint to prepare a coating, wherein the mixing mass ratio of the high-temperature irreversible thermochromic microcapsule to the paint is 1: (5-10) spraying the coating on the surface of the kinematic pair, and when the surface temperature of the kinematic pair changes to the color-changing temperature of the high-temperature irreversible thermochromic microcapsule, changing the color of the high-temperature irreversible thermochromic microcapsule to realize real-time monitoring of whether the kinematic pair fails or not;
the high-temperature irreversible thermochromic microcapsule comprises a core material and a shell material wrapping the surface of the core material, wherein the core material comprises a color former crystal violet lactone, a color former bisphenol A and a first organic solvent n-octane, and the shell material comprises Polystyrene (PS).
The preparation method of the high-temperature irreversible thermochromic microcapsule comprises the following steps:
(1) 1g of polyvinyl alcohol (PVA) and 0.5g of Arabic gum are dissolved in 200mL of deionized water to obtain an aqueous solution of an emulsifier; (2) 4g of Polystyrene (PS), 10g of n-octane, 45mL of methylene chloride, 0.08g of crystal violet lactone and 0.24g of bisphenol A were mixed to obtain a mixed solution; (3) Firstly pouring the aqueous solution of the emulsifier obtained in the step (1) into a three-neck flask, then adding the mixed solution obtained in the step (2) into the aqueous solution of the emulsifier, heating the mixture to 45 ℃ in a water bath, stirring the mixture for 4 hours, and obtaining a reaction product at a stirring rotating speed of 1500 rpm; (4) And (3) carrying out suction filtration on the reaction product by using a Buchner funnel, repeatedly flushing the reaction product with deionized water for 3 times, and finally drying the reaction product for 24 hours by using a freeze dryer to obtain the high-temperature irreversible thermochromic microcapsule.
In the method of the embodiment, when the surface temperature of the kinematic pair changes to 130 ℃, the high-temperature irreversible thermochromic microcapsule changes color, so that the visualization of the temperature change and the real-time monitoring of the temperature change at high temperature are realized, and whether the kinematic pair fails or not is monitored in real time.
Example 2
The embodiment provides a method for monitoring the failure of a kinematic pair in real time, which comprises the following steps:
the high-temperature irreversible thermochromic microcapsule is mixed with paint to prepare a coating, wherein the mixing mass ratio of the high-temperature irreversible thermochromic microcapsule to the paint is 1: (5-10) spraying the coating on the surface of the kinematic pair, and when the surface temperature of the kinematic pair changes to the color-changing temperature of the high-temperature irreversible thermochromic microcapsule, changing the color of the high-temperature irreversible thermochromic microcapsule to realize real-time monitoring of whether the kinematic pair fails or not;
the high-temperature irreversible thermochromic microcapsule comprises a core material and a shell material wrapping the surface of the core material, wherein the core material comprises a color former 6 '-diethylamino-2' -dibenzylaminofluran, a color former bisphenol A and a first organic solvent cyclohexanone, and the shell material comprises Polyimide (PI).
The preparation method of the high-temperature irreversible thermochromic microcapsule comprises the following steps:
(1) 1g of polyvinyl alcohol (PVA) and 0.5g of Arabic gum are dissolved in 200mL of deionized water to obtain an aqueous solution of an emulsifier; (2) 4g of Polyimide (PI), 10g of cyclohexanone, 45mL of methylene chloride, 0.02g of 6 '-diethylamino-2' -dibenzylaminofluorane and 0.06g of bisphenol A were mixed to obtain a mixed solution; (3) Firstly pouring the aqueous solution of the emulsifier obtained in the step (1) into a three-neck flask, then adding the mixed solution obtained in the step (2) into the aqueous solution of the emulsifier, heating the mixture to 45 ℃ in a water bath, stirring the mixture for 4 hours, and obtaining a reaction product at a stirring rotating speed of 1200 rpm; (4) And (3) carrying out suction filtration on the reaction product by using a Buchner funnel, repeatedly flushing the reaction product with deionized water for 3 times, and finally drying the reaction product for 24 hours by using a freeze dryer to obtain the high-temperature irreversible thermochromic microcapsule.
In the method of the embodiment, when the surface temperature of the kinematic pair changes to 150 ℃, the high-temperature irreversible thermochromic microcapsule changes color, so that the visualization of the temperature change and the real-time monitoring of the temperature change at high temperature are realized, and whether the kinematic pair fails or not is monitored in real time.
Fig. 2 is an effect diagram of the method for monitoring the failure of the kinematic pair in real time in the embodiment 1 and the embodiment 2. The side surface of the knuckle bearing is evenly divided into two parts along the circumferential direction, wherein one part is sprayed with the coating in the embodiment 1 according to the method of the embodiment 1, and the other part is sprayed with the coating in the embodiment 2 according to the method of the embodiment 2, and the spraying thicknesses are the same and are all 0.3-1.5 mm. The high temperature irreversible thermochromic microcapsules in example 1 change color when the temperature of the side of the knuckle bearing changes to 130 ℃. The high temperature irreversible thermochromic microcapsules in example 2 change color when the temperature of the side of the knuckle bearing changes to 150 ℃. Therefore, the methods of embodiment 1 and embodiment 2 can realize real-time monitoring of bearing temperature and visual feedback of temperature signals, and realize real-time monitoring of whether the kinematic pair fails.
Comparative example 1
The comparative example provides a thermochromic microcapsule, the preparation method of which comprises the following steps:
(1) 1g of polyvinyl alcohol (PVA) and 0.5g of Arabic gum are dissolved in 200mL of deionized water to obtain an aqueous solution of an emulsifier; (2) 4g of Polystyrene (PS), 10g of PAO6, 45mL of methylene chloride, 0.04g of crystal violet lactone and 0.12g of bisphenol A are mixed to obtain a mixed solution; (3) Firstly pouring the aqueous solution of the emulsifier obtained in the step (1) into a three-neck flask, then adding the mixed solution obtained in the step (2) into the aqueous solution of the emulsifier, heating the mixture to 45 ℃ in a water bath, stirring the mixture for 4 hours, and obtaining a reaction product at a stirring rotating speed of 1500 rpm; (4) And (3) carrying out suction filtration on the reaction product by using a Buchner funnel, repeatedly flushing the reaction product with deionized water for 3 times, and finally drying the reaction product for 24 hours by using a freeze dryer to obtain the thermochromic microcapsule.
Comparative example 2
The comparative example provides a microcapsule, the preparation method of which comprises the following steps:
(1) 1g of polyvinyl alcohol (PVA) and 0.5g of Arabic gum are dissolved in 200mL of deionized water to obtain an aqueous solution of an emulsifier; (2) 4g of Polystyrene (PS), 10g of PAO6, 45mL of methylene chloride, 1g of crystal violet lactone and 3g of bisphenol A are mixed to obtain a mixed solution; (3) Firstly pouring the aqueous solution of the emulsifier obtained in the step (1) into a three-neck flask, then adding the mixed solution obtained in the step (2) into the aqueous solution of the emulsifier, heating the mixture to 45 ℃ in a water bath, stirring the mixture for 4 hours, and obtaining a reaction product at a stirring rotating speed of 1500 rpm; (4) And (3) carrying out suction filtration on the reaction product by using a Buchner funnel, repeatedly flushing the reaction product with deionized water for 3 times, and finally drying the reaction product for 24 hours by using a freeze dryer to obtain the microcapsule.
Test case
The following tests were performed on the above examples and comparative examples:
1. color change effect observation under digital microscope and under macroscopic view: photographing by using a digital microscope VHX6000 and a mobile phone.
2. SEM analysis: a field emission scanning electron microscope Gemini SEM300 was used.
3. TEM-EDS analysis: a high resolution transmission electron microscope JEM-2100Plus was used.
The test results are as follows:
fig. 3 is SEM image, TEM and EDS elemental analysis results of the high temperature irreversible thermochromic microcapsules of example 1. As can be seen from fig. 3, the high temperature irreversible thermochromic microcapsule according to example 1 has a core-shell structure, and has an average particle size of less than 5 μm, and can be used for spraying. FIG. 4 is a graph showing the discoloration effect of the thermochromic microcapsules of example 1 under a digital microscope. FIG. 5 is a graph showing the macroscopic discoloration effect of the thermochromic microcapsules of example 1. As can be seen from fig. 4 and 5, the high temperature irreversible thermochromic microcapsules of example 1 have a color change temperature of 130 ℃ (white before color change, blue after color change), and the color change is irreversible after returning to room temperature.
Fig. 6 is an SEM image of the high temperature irreversible thermochromic microcapsules of example 2. FIG. 7 is a graph showing the macroscopic discoloration effect of the high temperature irreversible thermochromic microcapsules according to example 2. As can be seen from fig. 6 and 7, the average particle size of the high temperature irreversible thermochromic microcapsules of example 2 was less than 5 μm, the color change temperature was 150 ℃ (white before color change, light green after color change), and the color change was irreversible after returning to room temperature.
Fig. 8 is an SEM image of thermochromic microcapsules of comparative example 1. FIG. 9 is a graph showing the effect of thermochromic microcapsules of comparative example 1 on macroscopic discoloration. As can be seen from fig. 8 and 9, the thermochromic microcapsules of comparative example 1 had an average particle size of less than 5 μm, a color change temperature of 100 ℃ (white before color change, blue after color change), and the color change was reversible after returning to room temperature.
Fig. 10 is an SEM image of the microcapsules of comparative example 2. FIG. 11 is a graph showing the macroscopic effect of the microcapsules of comparative example 2. Macroscopic observation shows that the microcapsule of comparative example 2 is blue immediately after being prepared, and the color change function cannot be realized under the condition of changing temperature.
Claims (17)
1. A method of monitoring for motion pair failure in real time, wherein the method comprises:
the method comprises the steps that a high-temperature irreversible thermochromic microcapsule is arranged on the surface of a kinematic pair, and when the surface temperature of the kinematic pair changes to the color changing temperature of the high-temperature irreversible thermochromic microcapsule, the high-temperature irreversible thermochromic microcapsule changes color, so that whether the kinematic pair fails or not is monitored in real time;
the high-temperature irreversible thermochromic microcapsule comprises a core material and a shell material wrapping the surface of the core material, wherein the core material comprises a color former, a color former and a first organic solvent, the first organic solvent is a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water, and the shell material comprises a polymer.
2. The method for real-time monitoring of motion-pair failure according to claim 1, wherein the high temperature irreversible thermochromic microcapsules are prepared by at least the steps of:
(1) Mixing the shell material, the first organic solvent, the second organic solvent, the color former and the color former to obtain a mixed solution; the first organic solvent is a volatile liquid organic solvent which has a boiling point of 80-200 ℃ and is insoluble in water; the second organic solvent is a volatile liquid organic solvent which has a boiling point of 30-60 ℃ and is insoluble in water;
(2) Adding the mixed solution into an aqueous solution of an emulsifier, and stirring for a period of time under the condition that the boiling point temperature of the second organic solvent is 10 ℃ higher than the boiling point temperature of the second organic solvent, so that the second organic solvent is completely volatilized, and a reaction product is obtained;
(3) And (3) carrying out solid-liquid separation, washing and drying on the reaction product to obtain the high-temperature irreversible thermochromic microcapsule.
3. The method for monitoring the failure of a kinematic pair in real time according to claim 1 or 2, wherein the first organic solvent is an organic solvent that prevents the developer from contacting the developer through interaction between hydrogen bonds and the developer.
4. The method of real-time monitoring of motion-pair failure according to claim 3, wherein the first organic solvent comprises one or a combination of several of cyclohexane, dimethyl sulfoxide, triethylamine, 1, 2-dimethoxyethane, trichloroethylene, toluene, 1, 2-trichloroethane, 2-methoxyethanol, ethylene bromide, n-octane, dimethylformamide, and cyclohexanone.
5. The method of monitoring motion pair failure in real time according to claim 1 or 2, wherein the color former comprises one or a combination of several of crystal violet lactone, 6' -diethylamino-2 ' dibenzylaminofluran, 6' - (diethylamino) -1',2' -benzofluoran, and 7, 7-bis (4- (diethylamino) -2-ethoxyphenyl) furo [3,4-b ] pyridin-5 (7H) -one;
the color developer includes bisphenol a.
6. The method for real-time monitoring of motion pair failure according to claim 1 or 2, wherein the shell material comprises one or a combination of several of polystyrene, polysulfone, polymethyl methacrylate and polyimide.
7. The method of real-time monitoring for motion pair failure of claim 2, wherein the second organic solvent comprises methylene chloride.
8. The method for monitoring the failure of the kinematic pair in real time according to claim 1 or 2, wherein the mass ratio of the shell material to the first organic solvent to the color former is (2-6): (4-12): (0.02-0.08): (0.06-0.24).
9. The method for monitoring the failure of the kinematic pair in real time according to claim 2, wherein the mass-to-volume ratio of the shell material to the second organic solvent is (2-6) g:45mL.
10. The method of real-time monitoring of kinematic pair failure according to claim 2, wherein the emulsifier comprises polyvinyl alcohol and/or acacia.
11. The method for monitoring the failure of the kinematic pair in real time according to claim 10, wherein the emulsifier comprises the following components in percentage by mass (1-3): (0.5-1.5) a composition of polyvinyl alcohol and acacia.
12. The method for monitoring the failure of the kinematic pair in real time according to claim 2, wherein the mass-volume ratio of the emulsifier to water in the aqueous solution of the emulsifier is (1.5-4.5) g: (200-600) mL.
13. The method for monitoring the failure of the kinematic pair in real time according to claim 2, wherein the mixing volume ratio of the mixed solution to the aqueous solution of the emulsifier is 1: (2-5).
14. The method for monitoring the failure of the kinematic pair in real time according to claim 2, wherein in the step (2), the stirring time is 3-7 h under the condition that the boiling point temperature of the second organic solvent is 10 ℃ above the boiling point temperature of the second organic solvent.
15. The method for real-time monitoring of motion pair failure according to claim 1 or 2, wherein the average particle size of the high temperature irreversible thermochromic microcapsules is 5 μm or less.
16. The method for monitoring the failure of the kinematic pair in real time according to claim 1 or 2, wherein the high-temperature irreversible thermochromic microcapsule has a color change temperature of 80-200 ℃ and is irreversible after being restored to room temperature.
17. The method for real-time monitoring of a motion pair failure according to claim 1, wherein the disposing of the high temperature irreversible thermochromic microcapsules on the surface of the motion pair is achieved by preparing the high temperature irreversible thermochromic microcapsules into a coating and coating the coating on the surface of the motion pair.
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