Preparation method of fire-extinguishing coating, fire-extinguishing coating and fire-extinguishing coating product
By optimizing the wall structure and preparation process of microcapsules, fire extinguishing microcapsules with multiple wall materials are prepared and mixed with the coating base material, the problem of low stability of existing microcapsules is solved, and fire extinguishing coatings with high stability and effective fire extinguishing effect are achieved.
Patent Information
- Application Number
- CN202510254748.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-05
- Publication Date
- 2025-05-16
AI Technical Summary
The dispersion, embedding rate and wall thickness of existing perfluorohexanone microcapsules are difficult to effectively control during the production process, resulting in low yield, large trigger temperature range and low stability.
By optimizing the wall structure and preparation process of the microcapsules, fire-extinguishing microcapsules are prepared into multi-wall materials, which improves the durability and stability of the microcapsules, and mixes them with the coating base to form a high-stability fire-extinguishing coating.
It improves the durability and stability of microcapsules, ensures that the fire extinguishing coating maintains good performance and stability in various environments, and enhances the fire extinguishing effect.
Smart Images

Figure CN120005437A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of image processing, and in particular to a method for preparing a fire extinguishing coating, the fire extinguishing coating and a fire extinguishing coating product. Background Art
[0002] Perfluorohexanone (CAS No. 756-13-8) is a liquid at room temperature. Its heat of evaporation is only 1 / 25 of that of water, while its vapor pressure is 25 times that of water. These properties make it easy to vaporize and can quickly absorb heat to achieve the effect of extinguishing a fire. It is a new type of environmentally friendly fire extinguishing agent. In order to be better applied to various fire prevention and fire extinguishing scenarios, the fire extinguishing agent can be used as the core material to prepare microcapsules. Perfluorohexanone microcapsules need to remain stable under various conventional environments, and rupture in a high temperature environment when a fire occurs to release perfluorohexanone, automatically triggering the fire extinguishing function. However, the existing perfluorohexanone microcapsules have a low yield, a large triggering temperature range, and low stability due to the inability to effectively control the dispersion, embedding rate, and wall material thickness during the production process. Summary of the invention
[0003] The embodiment of the present invention provides a method for preparing a fire extinguishing coating, aiming to provide a method for preparing a fire extinguishing coating, and improving the stability of the fire extinguishing coating by using fire extinguishing microcapsules with multiple wall materials. By optimizing the wall material structure and preparation process of the microcapsules, the fire extinguishing microcapsules with multiple wall materials are prepared to improve the durability and stability of the microcapsules, and are mixed with the base material of the coating to obtain a highly stable fire extinguishing coating.
[0004] In a first aspect, an embodiment of the present invention provides a method for preparing a fire extinguishing coating, the method comprising the following steps:
[0005] S10, preparing multi-walled fire-extinguishing microcapsules: preparing multi-walled fire-extinguishing microcapsules by using perfluorohexanone accounting for 60%-70% of the total mass, a first layer wall material solution accounting for 15%-20% of the total mass of the first layer wall material, a second layer wall material solution accounting for 5%-8% of the total mass of the second layer wall material, and a third layer wall material solution accounting for 3%-5% of the total mass of the third layer wall material;
[0006] S20, mixing the fire extinguishing microcapsules of multi-wall material with the coating base material: adding the fire extinguishing microcapsules of multi-wall material into the coating base material, stirring until uniform, and obtaining the prepared fire extinguishing coating.
[0007] Optionally, the first layer of wall material is a polymer material, the second layer of wall material is a moisture-curable polymer monomer, and the third layer of wall material is an ultraviolet light-curable resin.
[0008] Optionally, before step S10, the method further includes the following steps:
[0009] Purifying perfluorohexanone to obtain perfluorohexanone with a purity of more than 99%;
[0010] Dissolving the polymer material in a desolvent, heating and stirring until completely dissolved, to form a polymer material solution;
[0011] Dissolving the moisture-curable polymer monomer in the desolventizing agent, heating and stirring until completely dissolved, to form a moisture-curable polymer monomer solution;
[0012] The ultraviolet light curing resin is stirred until it is uniform and has no precipitation, so as to form an ultraviolet light curing resin solution.
[0013] Optionally, S10, the step of preparing the fire-extinguishing microcapsules of multi-wall material specifically includes:
[0014] S101, emulsification and first layer wall material coating: dripping perfluorohexanone into the polymer material solution, emulsifying with a high-speed emulsifier, and forming the fire-extinguishing microcapsules of the first layer wall material after detecting that the particle size and the embedding rate meet the first molding conditions;
[0015] S102, coating with the second wall material: dispersing the fire extinguishing microcapsules of the first wall material in the moisture-curable polymer monomer solution, stirring at a first stirring speed, and forming the fire extinguishing microcapsules of the second wall material after detecting that the first dispersion of the fire extinguishing microcapsules of the first wall material in the second wall material solution and the thickness of the first wall material meet the second molding condition;
[0016] S103, coating with a third wall material: dispersing the fire extinguishing microcapsules of the second wall material in an ultraviolet light-curing resin solution and stirring at a second stirring speed, wherein the second stirring speed is lower than the first stirring speed; after detecting that a second dispersion of the fire extinguishing microcapsules of the second wall material in the ultraviolet light-curing resin solution and a second wall material thickness satisfy a third molding condition, curing is performed by ultraviolet light irradiation to form fire extinguishing microcapsules of multiple wall materials.
[0017] Optionally, in step S101, the following steps are specifically included:
[0018] Perfluorohexanone was dropped into the polymer material solution, emulsified using a high-speed emulsifier, an emulsifier was added, and the mixture was stirred and emulsified for 30 minutes. The first particle size detection of the emulsified sample was performed by dynamic light scattering;
[0019] After the first particle size test was passed, a cross-linking agent was added, and stirring was continued for 1 hour, and then a second particle size test was performed on the sample after the cross-linking reaction by dynamic light scattering;
[0020] After the second particle size test was passed, the embedding rate of the sample after the cross-linking reaction was tested by visible light spectrometry;
[0021] After the embedding rate test is passed, the fire extinguishing microcapsules of the first layer of wall material are formed.
[0022] Optionally, in step S102, the following steps are specifically included:
[0023] Dispersing the fire-extinguishing microcapsules of the first layer of wall material in a moisture-curable polymer monomer solution, adjusting the pH value to 7.0, and performing a first dispersion test on the dispersed film sample through an electron microscopic image;
[0024] Based on the result of the first divergence detection, the first stirring speed and the stirring time are matched, and stirring is performed at the first stirring speed. After the stirring reaches the stirring time, the second divergence detection and the wall material thickness detection are performed on the stirred film sample through an electron microscope image;
[0025] After the second divergence detection and the wall material thickness detection, the fire extinguishing microcapsules of the second layer of wall material are formed.
[0026] Optionally, in step S103, the following steps are specifically included:
[0027] Dispersing the fire extinguishing microcapsules of the second layer wall material in the ultraviolet light curing resin solution, stirring at a second stirring speed, the second stirring speed being lower than the first stirring speed;
[0028] During the stirring process, the third divergence detection and the corresponding wall material thickness detection are performed on the stirred film sample multiple times through the electron microscopic images corresponding to multiple stirring time points;
[0029] During the multiple third divergence detection processes, if any third divergence detection and the wall material thickness detection are passed at the same time, the microcapsules are cured by ultraviolet light irradiation to form fire-extinguishing microcapsules with multiple wall materials.
[0030] In a second aspect, an embodiment of the present invention further provides a fire extinguishing coating, which is obtained according to the preparation method of the fire extinguishing coating as described in any one of the embodiments of the present invention.
[0031] In a third aspect, an embodiment of the present invention provides a fire extinguishing sheet, comprising a sheet-like substrate, a coating layer and an adhesive layer, wherein the coating layer and the adhesive layer are respectively located on both sides of the sheet-like substrate, and the coating layer is obtained by coating a fire extinguishing coating, and the fire extinguishing coating is obtained according to the preparation method of the fire extinguishing coating as described in any one of the embodiments of the present invention.
[0032] In a fourth aspect, an embodiment of the present invention provides a fire extinguishing electrical cabinet, the inner surface of which is coated with a coating layer, the coating layer is obtained by coating with a fire extinguishing paint, and the fire extinguishing paint is obtained according to the preparation method of the fire extinguishing paint as described in any one of the embodiments of the present invention.
[0033] In the embodiment of the present invention, S10, preparing fire-extinguishing microcapsules of multi-wall materials: preparing fire-extinguishing microcapsules of multi-wall materials by using perfluorohexanone accounting for 60%-70% of the total mass, a first layer wall material solution accounting for 15%-20% of the total mass, a second layer wall material solution accounting for 5%-8% of the total mass, and a third layer wall material solution accounting for 3%-5% of the total mass; S20, mixing the fire-extinguishing microcapsules of multi-wall materials with a coating base material: adding the fire-extinguishing microcapsules of multi-wall materials to the coating base material, stirring until uniform, and obtaining a prepared fire-extinguishing coating. By optimizing the wall material structure and preparation process of the microcapsules, the fire-extinguishing microcapsules of multi-wall materials are prepared to improve the durability and stability of the microcapsules, and are mixed with the base material of the coating to obtain a highly stable fire-extinguishing coating. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0035] Figure 1 It is a flow chart of a method for preparing a fire extinguishing coating provided by an embodiment of the present invention;
[0036] Figure 2 The present invention provides a flowchart of a method for producing a multi-walled fire-extinguishing microcapsule. DETAILED DESCRIPTION
[0037] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0038] like Figure 1 As shown, Figure 1 The figure is a flow chart of a method for preparing a fire extinguishing coating provided by an embodiment of the present invention. The method for preparing the fire extinguishing coating comprises the following steps:
[0039] S10. Preparation of fire-extinguishing microcapsules with multiple wall materials: fire-extinguishing microcapsules with multiple wall materials are prepared by using perfluorohexanone accounting for 60%-70% of the total mass, a first layer wall material solution accounting for 15%-20% of the total mass of the first layer wall material, a second layer wall material solution accounting for 5%-8% of the total mass of the second layer wall material, and a third layer wall material solution accounting for 3%-5% of the total mass of the third layer wall material.
[0040] S20, mixing the fire extinguishing microcapsules of multi-wall material with the coating base material: adding the fire extinguishing microcapsules of multi-wall material into the coating base material, stirring until uniform, and obtaining the prepared fire extinguishing coating.
[0041] In one preparation, perfluorohexanone accounts for 60%-70% of the total mass, the first layer of wall material accounts for 15%-20% of the total mass, the second layer of wall material accounts for 5%-8% of the total mass, and the third layer of wall material accounts for 3%-5% of the total mass. The specific proportions are determined according to different wall thicknesses.
[0042] Furthermore, in the embodiment of the present invention, the purity of perfluorohexanone reaches more than 99%. Perfluorohexanone can be distilled and purified by rectification, and after the crude perfluorohexanone is reacted with a specific catalyst and a nucleophilic reagent, the lower layer of liquid is taken for rectification, and perfluorohexanone with a purity of more than 99% can be obtained.
[0043] Furthermore, in the embodiment of the present invention, the first layer of wall material is a polymer material, the second layer of wall material is a moisture-curable polymer monomer, and the third layer of wall material is an ultraviolet light-curable resin.
[0044] The softening point of the polymer material after curing is the desired temperature point. When the temperature reaches the desired temperature point, the polymer material softens and releases the internal perfluorohexanone. The desired temperature point is, for example, 70-100° C. The polymer material can be gelatin, alginate, gum arabic, β-cyclodextrin or a combination thereof.
[0045] The polymer material is dissolved in a deionized water, and heated and stirred until it is completely dissolved to form a polymer material solution; the solvent may be deionized water.
[0046] The moisture-curable polymer monomer can be selected from any one of α-silane modified polyether, α-methyl cyanoacrylate, and aminopropyl trimethoxysilane. The moisture-curable polymer monomer is dissolved in a desolvent, heated and stirred until completely dissolved to form a moisture-curable polymer monomer solution; the solvent can be deionized water.
[0047] The UV-curable resin can be any one of epoxy acrylate resin, polyurethane acrylate resin, unsaturated polyester resin and acrylate polymer. The UV-curable resin is stirred until it is uniform and has no precipitation, so as to form a UV-curable resin solution.
[0048] like Figure 2 As shown, Figure 2 The following is a schematic diagram of a process for preparing a multi-walled fire-extinguishing microcapsule according to an embodiment of the present invention. The steps for preparing the multi-walled fire-extinguishing microcapsule specifically include:
[0049] S101, emulsification and first layer wall material coating: drip perfluorohexanone into the polymer material solution, use a high-speed emulsifier to emulsify, and after detecting that the particle size and embedding rate meet the first molding conditions, form the fire-extinguishing microcapsules of the first layer wall material.
[0050] In an embodiment of the present invention, step S101 is mainly to prepare the fire-extinguishing microcapsules of the first layer of wall material. First, perfluorohexanone is dripped into the polymer material solution. As the first layer of wall material, the main function of the polymer material is to wrap and protect the perfluorohexanone inside. Next, a high-speed emulsifier is used for emulsification treatment. During this process, the polymer material will gradually wrap the perfluorohexanone droplets to form a microcapsule structure. During the emulsification process, the particle size and embedding rate of the microcapsules are continuously tested to ensure that the size and embedding effect of the microcapsules meet the preset standards. When the particle size and embedding rate meet the first molding condition, it means that the fire-extinguishing microcapsules of the first layer of wall material have been successfully prepared.
[0051] The first molding condition is that the particle size distribution is between 20 μm and 90 μm, and the embedding rate is above 90%.
[0052] Specifically, under the conditions of temperature 25±5°C and humidity 50±10%RH, perfluorohexanone can be dropped into the polymer material solution, emulsified using a high-speed emulsifier, added with an emulsifier, stirred and emulsified for 25-35 minutes, with a stirring speed of 1400-1600rpm, and the emulsified sample is subjected to a first particle size test by dynamic light scattering; after the first particle size test is passed, a cross-linking agent is added, and stirring is continued for 1 hour, and the sample after the cross-linking reaction is subjected to a second particle size test by dynamic light scattering again; after the second particle size test is passed, the sample after the cross-linking reaction is subjected to an embedding rate test by visible light spectrometry; after the embedding rate test is passed, a fire-extinguishing microcapsule of the first layer of wall material is formed.
[0053] During the first particle size detection process, a certain amount of sample is taken from the emulsified polymer material solution to ensure the representativeness and uniformity of the sampling. The sample taken out is appropriately diluted to avoid multiple scattering effects, so that the dynamic light scattering (DLS) instrument can more accurately measure the particle size. The diluted sample is measured using a DLS instrument. DLS technology infers the particle size by measuring the speed of the Brownian motion of particles in the solution. Record the particle size distribution data output by the DLS instrument, including information such as the average particle size and the particle size distribution width. Evaluate the measurement results based on the expected particle size range (particle size distribution between 30μm and 110μm). If the particle size distribution is as expected, proceed to the next step of the cross-linking reaction.
[0054] During the second particle size test, after adding the cross-linking agent and stirring for 1 hour, a certain amount of sample is taken out from the polymer material solution again. The sample taken out is also appropriately diluted and measured using DLS. The particle size data of the sample after the cross-linking reaction is analyzed and compared with the results of the first particle size test. The cross-linking reaction may cause a change in particle size, which is within the expected range (particle size distribution between 20μm and 90μm). If the particle size distribution after cross-linking meets the requirements, prepare for the embedding rate test.
[0055] The embedding rate is used to evaluate the encapsulation efficiency of the active ingredients in the fire-extinguishing microcapsules. The embedding rate can be detected using visible light spectrophotometry. First, a series of perfluorohexanone solutions of known concentrations are prepared, and their absorbances are measured using a visible light spectrophotometer to draw a standard curve of concentration and absorbance. Take a certain amount of the polymer material solution after the cross-linking reaction, and separate the microcapsules by an appropriate method (such as centrifugation or filtration). The separated microcapsules are dissolved or destroyed to release the perfluorohexanone therein, and then the absorbance is measured using a visible light spectrophotometer. According to the pre-set standard curve, the measured absorbance is converted into the concentration of perfluorohexanone, and then the amount of perfluorohexanone embedded in the microcapsules is calculated. Finally, the embedding rate can be calculated by comparing the amount of perfluorohexanone before and after embedding. If the embedding rate reaches the expected standard (the embedding rate reaches more than 90%), it means that the preparation of the fire-extinguishing microcapsules is successful.
[0056] When it is detected that the particle size distribution is between 20 μm and 90 μm and the embedding rate reaches more than 90%, the cross-linking stirring is terminated to form the fire-extinguishing microcapsules of the first layer wall material.
[0057] S102, second layer wall material coating: disperse the fire extinguishing microcapsules of the first layer wall material in the moisture-curable polymer monomer solution, stir at a first stirring speed, and after detecting that the first dispersion of the fire extinguishing microcapsules of the first layer wall material in the second layer wall material solution and the thickness of the first wall material meet the second molding condition, form the fire extinguishing microcapsules of the second layer wall material.
[0058] In an embodiment of the present invention, after the coating of the first layer of wall material is completed, the coating of the second layer of wall material is carried out. The prepared fire-extinguishing microcapsules of the first layer of wall material are dispersed in a moisture-curing polymer monomer solution. The moisture-curing polymer monomer solution is solidified in the subsequent treatment process to form a second layer of wall material. Stirring is performed at a certain stirring speed (first stirring speed, 400-600rpm) to ensure that the microcapsules of the first layer of wall material can be evenly dispersed in the solution and that the polymer monomer can be evenly coated on the outer layer of the microcapsules. In this process, it is necessary to monitor the dispersion degree (first divergence) of the microcapsules of the first layer of wall material in the second layer of wall material solution and the thickness of the first wall material to ensure that the second layer of wall material can be evenly and completely coated on the first layer of wall material. When these parameters meet the second molding condition, it means that the fire-extinguishing microcapsules of the second layer of wall material have been successfully prepared. The thickness of the first wall material is 5μm to 15μm, and the thickness of the first wall material is the total thickness of the first layer of wall material and the second layer of wall material.
[0059] Under the conditions of temperature of 30±5°C and humidity of 50±10% RH, the fire extinguishing microcapsules of the first layer wall material are dispersed in the moisture-curing polymer monomer solution, and after adjusting the pH value to 7.0, the first divergence test is performed on the dispersed film sample through electron microscopy images; based on the result of the first divergence test, the first stirring speed (500rpm) and the stirring time (1 hour) are matched, and stirring is performed at the first stirring speed. After stirring for the stirring time, the second divergence test and the wall material thickness test are performed on the stirred film sample through electron microscopy images; after the second divergence test and the wall material thickness test are performed, the fire extinguishing microcapsules of the second layer wall material are formed.
[0060] S103, coating with the third wall material: dispersing the fire extinguishing microcapsules of the second wall material in the ultraviolet light-curing resin solution, stirring at a second stirring speed, the second stirring speed being lower than the first stirring speed, and after detecting that the second dispersion of the fire extinguishing microcapsules of the second wall material in the ultraviolet light-curing resin solution and the thickness of the second wall material meet the third molding condition, curing is performed by ultraviolet light irradiation to form fire extinguishing microcapsules of multiple wall materials.
[0061] In an embodiment of the present invention, the fire extinguishing microcapsules of the second layer of wall material are dispersed in the ultraviolet curing resin solution, and the fire extinguishing microcapsules of the second layer of wall material that have been formed can be coated again. By using ultraviolet curing resin, the number of wall material layers of the microcapsules is increased to improve their stability and durability. Ultraviolet curing resin is a special resin that can be quickly cured under ultraviolet light to form a hard protective layer. Stirring is performed at a second stirring speed (300rpm), and the second stirring speed is less than the first stirring speed. After the fire extinguishing microcapsules of the second layer of wall material are dispersed in the ultraviolet curing resin solution, stirring is performed to ensure that the microcapsules are uniformly dispersed in the resin solution. In order to avoid the excessively fast stirring speed from destroying the already formed microcapsule structure, the second stirring speed is less than the first stirring speed, and it is also ensured that the microcapsules can be fully dispersed in the resin solution. It is detected that the second dispersion of the fire extinguishing microcapsules of the second layer of wall material in the ultraviolet curing resin solution and the second wall material thickness meet the third molding condition. During the stirring process, the dispersion degree of the microcapsules in the resin solution (the second dispersion) and the thickness of the newly formed wall material (the second wall material thickness) are monitored in real time. The thickness of the second wall material is 2 μm to 6 μm, and the thickness of the second wall material is the total thickness of the third layer of wall material.
[0062] The above dispersion is used to indicate the degree of dispersion of the fire extinguishing microcapsules of the second layer of wall material. The greater the dispersion, the lower the density of the fire extinguishing microcapsules of the second layer of wall material in the UV-curable resin solution. The smaller the dispersion, the less likely it is to aggregate. The dispersion is the ratio of the standard deviation of the distance between the fire extinguishing microcapsules of the second layer of wall material to the average distance. The first dispersion can be set between 0.1 and 0.3, for example, to 0.2. The second dispersion can be set between 0.1 and 0.4, for example, to 0.3.
[0063] The third molding condition includes the uniformity of the dispersion of the microcapsules and whether the thickness of the new wall material meets the expected standards. The fire-extinguishing microcapsules with multiple wall materials are cured by ultraviolet light irradiation. When it is detected that the dispersion degree of the microcapsules and the thickness of the wall material meet the requirements, the resin solution is irradiated with ultraviolet light to quickly cure the resin, thereby forming another protective layer outside the microcapsules of the second wall material. After the third layer of wall material is coated, a multi-layer wall material fire-extinguishing microcapsule is formed, which improves the durability and stability of the microcapsule and controls the release rate of the fire extinguishing agent. On the basis of the fire-extinguishing microcapsules that already have two layers of wall material, another layer of wall material is coated with ultraviolet light-cured resin to enhance the performance of the microcapsules.
[0064] At a temperature of 20±5°C, humidity ≤60%RH, and light-proof conditions, the fire-extinguishing microcapsules of the second wall material are dispersed in the UV-curable resin solution, stirred evenly, and the stirring speed is controlled to be 300rpm, and the curing time is 4 hours. The second stirring speed is lower than the first stirring speed; during the stirring process, the stirred film samples are subjected to multiple third divergence tests and corresponding multiple wall material thickness tests through electron microscopic images corresponding to multiple stirring time points; during the multiple third divergence tests, if any of the third divergence tests and the wall material thickness tests are passed at the same time, the fire-extinguishing microcapsules are cured by UV irradiation to form multi-wall material fire-extinguishing microcapsules.
[0065] In the embodiment of the present invention, by optimizing the wall material structure and preparation process of the microcapsules, fire-extinguishing microcapsules with multiple wall materials are prepared to improve the durability and stability of the microcapsules, which are then mixed with the base material of the coating to obtain a highly stable fire-extinguishing coating.
[0066] The present invention provides a fire extinguishing coating, which is obtained according to the preparation method of the fire extinguishing coating.
[0067] The present invention provides a fire extinguishing sheet, which comprises a sheet-like substrate, a coating layer and an adhesive layer, wherein the coating layer and the adhesive layer are respectively located on both sides of the sheet-like substrate, and the coating layer is obtained by coating a fire extinguishing coating, and the fire extinguishing coating is obtained according to the preparation method of the above-mentioned fire extinguishing coating.
[0068] The invention provides a fire extinguishing electrical cabinet, the inner surface of which is coated with a coating layer, the coating layer is obtained by coating a fire extinguishing paint, and the fire extinguishing paint is obtained according to the preparation method of the fire extinguishing paint.
[0069] Example 1, prepare perfluorohexanone accounting for 65% of the total mass, gelatin accounting for 18% of the total mass of gelatin solution, α-silane modified polyether accounting for 7% of the total mass of α-silane modified polyether solution and epoxy acrylate resin accounting for 4% of the total mass of epoxy acrylate resin solution, the rest is 3% emulsifier, 3% cross-linking agent. During the preparation process, under the conditions of temperature 25±5℃ and humidity 50±10%RH, perfluorohexanone is dripped into the gelatin solution, emulsified using a high-speed emulsifier, emulsifier is added, stirred and emulsified for 30 minutes, the stirring speed is 1500rpm, and the emulsified sample is subjected to the first particle size detection by dynamic light scattering. When the particle size distribution is between 30μm and 110μm, a cross-linking agent is added and stirred for 1 hour, and then a certain amount of sample is taken out from the polymer material solution again. Similarly, the sample taken out is appropriately diluted and measured using DLS. The particle size data of the sample after the cross-linking reaction is analyzed. When the particle size distribution is between 20 μm and 90 μm and the embedding rate is above 90%, the mixed solution is air-dried to prepare the fire-extinguishing microcapsules of the first layer wall material. Under the conditions of temperature of 30±5°C and humidity of 50±10%RH, the fire extinguishing microcapsules of the first layer wall material are dispersed in an α-silane modified polyether solution, and after adjusting the pH value to 7.0, the first divergence detection is performed on the dispersed film sample through electron microscopy images; when the dispersion is detected to be between 0.1 and 0.3, the first stirring speed (600rpm at 0.1, 500rpm at 0.2, and 400rpm at 0.3) and stirring time (50 minutes at 0.1, 60 minutes at 0.2, and 70 minutes at 0.3) are matched, and stirring is performed at the first stirring speed. After stirring for the stirring time, the second divergence detection and wall material thickness detection are performed on the stirred film sample through electron microscopy images. When the dispersion is detected to be between 0.1 and 0.3 and the wall material thickness is between 5μm and 15μm, the fire extinguishing microcapsules of the second layer wall material are dried. At a temperature of 20±5°C, humidity ≤60% RH, and in a light-proof condition, the fire-extinguishing microcapsules of the second layer wall material are dispersed in a UV-curable resin solution and stirred evenly. The stirring speed is controlled at 300rpm. During the stirring process, the stirred film samples are subjected to multiple third divergence tests and corresponding multiple wall material thickness tests through electron microscopic images corresponding to multiple stirring time points. During the multiple third divergence tests, if any of the third divergence tests and the wall material thickness tests are passed at the same time, and the dispersion is detected to be between 0.1 and 0.3, and the thickness of the second wall material is between 2μm and 6μm, the microcapsules are cured by UV irradiation for 4 hours to form fire-extinguishing microcapsules with multiple wall materials.
[0070] After baking at 40°C, 50°C and 60°C for 24 hours, the morphological changes of the multi-walled fire-extinguishing microcapsules prepared in Example 1 were tested, such as cracking, deformation, leakage of contents, etc. The thermal stability was high within the safe range, and the test results were as follows:
[0071] temperature rupture(%) Deformation (%) Content leakage (%) 40℃ 0.01 0.02 0.01 50℃ 0.01 0.02 0.01 60℃ 0.02 0.03 0.02
[0072] In a simulated small fire scene (flame length 10CM), within a distance of 10CM, different amounts of fire extinguishing microcapsules can extinguish the flame in a short time. The fire extinguishing performance test results are as follows:
[0073] Dosage of fire extinguishing microcapsules (g) Flame extinguishing time(s) 5 16 10 13 15 11 20 9 25 8
[0074] After one month of exposure to the natural environment, the prepared multi-walled fire extinguishing microcapsules still maintained good integrity, embedding rate and fire extinguishing performance. The fire extinguishing performance was tested in a simulated small fire scene (flame length 10CM), within a distance of 3CM, with a dosage of 25g. The specific test results are as follows:
[0075]
[0076] Example 2: Prepare 70% of perfluorohexanone, 15% of gelatin solution, 5% of α-silane modified polyether solution, and 4% of epoxy acrylate resin solution, and the rest are 3% of emulsifier and 3% of cross-linking agent to prepare multi-walled fire extinguishing microcapsules.
[0077] After baking at 40°C, 50°C and 60°C for 24 hours, the morphological changes of the multi-walled fire-extinguishing microcapsules prepared in Example 2 were tested, such as cracking, deformation, leakage of contents, etc. The thermal stability was high within the safe range, and the test results were as follows:
[0078] temperature rupture(%) Deformation (%) Content leakage (%) 40℃ 0.01 0.02 0.01 50℃ 0.02 0.02 0.02 60℃ 0.03 0.03 0.03
[0079] In a simulated small fire scene (flame length 10CM), within a distance of 3CM, different amounts of fire extinguishing microcapsules can extinguish the flame in a short time. The fire extinguishing performance test results are as follows:
[0080] Dosage of fire extinguishing microcapsules (g) Flame extinguishing time(s) 5 15 10 12 15 10 20 8 25 7
[0081] After one month of exposure to the natural environment, the prepared multi-walled fire extinguishing microcapsules still maintained good integrity, embedding rate and fire extinguishing performance. The fire extinguishing performance was tested in a simulated small fire scene (flame length 10CM), within a distance of 3CM, with a dosage of 25g. The specific test results are as follows:
[0082]
[0083] Example 3, prepare perfluorohexanone accounting for 62% of the total mass, gelatin accounting for 19% of the total mass of gelatin solution, α-silane modified polyether accounting for 8% of the total mass of α-silane modified polyether solution and epoxy acrylate resin accounting for 5% of the total mass of epoxy acrylate resin solution, and the rest are 3% of emulsifier and 3% of cross-linking agent to prepare multi-walled fire extinguishing microcapsules.
[0084] After baking at 40°C, 50°C and 60°C for 24 hours, the morphological changes of the multi-walled fire-extinguishing microcapsules prepared in Example 3 were tested, such as cracking, deformation, leakage of contents, etc. The thermal stability was high within the safe range, and the test results were as follows:
[0085] temperature rupture(%) Deformation (%) Content leakage (%) 40℃ 0.01 0.01 0.01 50℃ 0.01 0.01 0.01 60℃ 0.01 0.02 0.01
[0086] In a simulated small fire scene (flame length 10CM), within a distance of 3CM, different amounts of fire extinguishing microcapsules can extinguish the flame in a short time. The fire extinguishing performance test results are as follows:
[0087] Dosage of fire extinguishing microcapsules (g) Flame extinguishing time(s) 5 17 10 14 15 12 20 11 25 10
[0088] After one month of exposure to the natural environment, the prepared multi-walled fire extinguishing microcapsules still maintained good integrity, embedding rate and fire extinguishing performance. The fire extinguishing performance was tested in a simulated small fire scene (flame length 10CM), within a distance of 3CM, with a dosage of 25g. The specific test results are as follows:
[0089]
[0090] By optimizing the wall material structure and preparation process of the microcapsule, the fire-extinguishing microcapsule with multiple wall materials is prepared to improve the durability and stability of the microcapsule, thereby obtaining the fire-extinguishing microcapsule with high stability.
[0091] The above disclosure is only the preferred embodiment of the present invention, which certainly cannot be used to limit the scope of the present invention. Therefore, equivalent changes made according to the claims of the present invention are still within the scope of the present invention.
Claims
1. A method for preparing a fire extinguishing coating, characterized in that: The method comprises the following steps: S10, preparing multi-walled fire-extinguishing microcapsules: preparing multi-walled fire-extinguishing microcapsules by using perfluorohexanone accounting for 60%-70% of the total mass, a first layer wall material solution accounting for 15%-20% of the total mass of the first layer wall material, a second layer wall material solution accounting for 5%-8% of the total mass of the second layer wall material, and a third layer wall material solution accounting for 3%-5% of the total mass of the third layer wall material; S20, mixing the fire extinguishing microcapsules of multi-wall material with a coating base material: adding the fire extinguishing microcapsules of multi-wall material into the coating base material, stirring until uniform, and obtaining a prepared fire extinguishing coating.
2. The method for preparing the fire extinguishing coating according to claim 1, characterized in that: The first layer of wall material is a polymer material, the second layer of wall material is a moisture-curable polymer monomer, and the third layer of wall material is an ultraviolet light-curable resin.
3. The method for preparing the fire extinguishing coating according to claim 2, characterized in that: Before step S10, the method further includes the following steps: Purifying perfluorohexanone to obtain perfluorohexanone with a purity of more than 99%; Dissolving the polymer material in a desolvent, heating and stirring until completely dissolved, to form a polymer material solution; Dissolving the moisture-curable polymer monomer in the desolventizing agent, heating and stirring until completely dissolved, to form a moisture-curable polymer monomer solution; The ultraviolet light curing resin is stirred until it is uniform and has no precipitation, so as to form an ultraviolet light curing resin solution.
4. The method for preparing the fire extinguishing coating according to claim 3, characterized in that: S10, the steps of preparing the multi-walled fire extinguishing microcapsules specifically include: S101, emulsification and first layer wall material coating: dripping perfluorohexanone into the polymer material solution, emulsifying with a high-speed emulsifier, and forming the fire-extinguishing microcapsules of the first layer wall material after detecting that the particle size and the embedding rate meet the first molding conditions; S102, coating with the second wall material: dispersing the fire extinguishing microcapsules of the first wall material in the moisture-curable polymer monomer solution, stirring at a first stirring speed, and forming the fire extinguishing microcapsules of the second wall material after detecting that the first dispersion of the fire extinguishing microcapsules of the first wall material in the second wall material solution and the thickness of the first wall material meet the second molding condition; S103, coating with a third wall material: dispersing the fire extinguishing microcapsules of the second wall material in an ultraviolet light-curing resin solution and stirring at a second stirring speed, wherein the second stirring speed is lower than the first stirring speed; after detecting that a second dispersion of the fire extinguishing microcapsules of the second wall material in the ultraviolet light-curing resin solution and a second wall material thickness satisfy a third molding condition, curing is performed by ultraviolet light irradiation to form fire extinguishing microcapsules of multiple wall materials.
5. The method for preparing the fire extinguishing coating according to claim 4, characterized in that: In step S101, it specifically includes: Perfluorohexanone was dropped into the polymer material solution, emulsified using a high-speed emulsifier, an emulsifier was added, and the mixture was stirred and emulsified for 30 minutes. The first particle size detection of the emulsified sample was performed by dynamic light scattering; After the first particle size test was passed, a cross-linking agent was added, and stirring was continued for 1 hour, and then a second particle size test was performed on the sample after the cross-linking reaction by dynamic light scattering; After the second particle size test was passed, the embedding rate of the sample after the cross-linking reaction was tested by visible light spectrometry; After the embedding rate test is passed, the fire extinguishing microcapsules of the first layer of wall material are formed.
6. The method for preparing the fire extinguishing coating according to claim 4, characterized in that: In step S102, it specifically includes: Dispersing the fire-extinguishing microcapsules of the first layer of wall material in a moisture-curable polymer monomer solution, adjusting the pH value to 7.0, and performing a first dispersion test on the dispersed film sample through an electron microscopic image; Based on the result of the first divergence detection, the first stirring speed and the stirring time are matched, and stirring is performed at the first stirring speed. After the stirring reaches the stirring time, the second divergence detection and the wall material thickness detection are performed on the stirred film sample through an electron microscope image; After the second divergence detection and the wall material thickness detection, the fire extinguishing microcapsules of the second layer of wall material are formed.
7. The method for preparing the fire extinguishing coating according to claim 4, characterized in that: In step S103, it specifically includes: Dispersing the fire extinguishing microcapsules of the second layer wall material in the ultraviolet light curing resin solution, stirring at a second stirring speed, the second stirring speed being lower than the first stirring speed; During the stirring process, the third divergence detection and the corresponding wall material thickness detection are performed on the stirred film sample multiple times through the electron microscopic images corresponding to multiple stirring time points; During the multiple third divergence detection processes, if any third divergence detection and the wall material thickness detection are passed at the same time, the microcapsules are cured by ultraviolet light irradiation to form fire-extinguishing microcapsules with multiple wall materials.
8. A fire extinguishing coating, characterized in that: The fire extinguishing coating is obtained according to the preparation method of any one of claims 1 to 7.
9. A fire extinguishing sheet, characterized in that: The fire extinguishing sheet includes a sheet-like substrate, a coating layer and an adhesive layer, wherein the coating layer and the adhesive layer are respectively located on both sides of the sheet-like substrate, and the coating layer is obtained by coating a fire extinguishing coating, and the fire extinguishing coating is obtained according to the preparation method of the fire extinguishing coating as described in any one of claims 1 to 7.
10. A fire extinguishing electrical cabinet, characterized in that: The inner surface of the fire-extinguishing electrical cabinet is coated with a coating layer, and the coating layer is obtained by coating with a fire-extinguishing paint, and the fire-extinguishing paint is obtained according to the preparation method of the fire-extinguishing paint as described in any one of claims 1 to 7.