Plugging glue and preparation method thereof

Abstract

The application discloses a plugging glue and a preparation method thereof. The plugging glue raw material comprises the following components in percentage by mass: 9-25% of photocuring resin, 0.5-1% of a photo initiator, 70-85% of modified inorganic fillers and 4-6% of modified heat-conducting fillers; the modified inorganic fillers are inorganic fillers modified by a silane coupling agent; and the modified heat-conducting fillers are heat-conducting fillers modified by a silane coupling agent. The photocuring resin, the modified inorganic fillers and the modified heat-conducting fillers are compounded, so that the plugging glue has excellent viscosity and rapid curing performance, the shortcomings of traditional high polymer adhesives are overcome, and the plugging glue can be used for rapidly plugging the inflatable equipment under pressure, and can be applied to the rapid pressure plugging of the sand eye cracks, micro cracks and annular leaking parts of the inflatable equipment.

Description

Technical Field

[0001] This invention relates to the field of sealing materials technology, and more specifically, to a sealing adhesive and its preparation method. Background Technology

[0002] Inflatable equipment is used in many industries, but pressurized inflatable equipment has a certain maintenance period. Gas leaks are prone to occur near the maintenance period, which can cause losses to enterprises and sometimes harm the health of workers. Managing leaks is an effective way to reduce the defect rate. Among these methods, live leak sealing is a primary means of solving equipment leaks. Live leak sealing, also known as "rapid live leak sealing of pipelines and containers without stopping power or heat," refers to leak sealing measures that do not interrupt power supply, pressure, or heat supply when pipelines or containers experience corrosion, perforation, leaks, or drips. The materials used in live leak sealing are crucial to its success.

[0003] In recent years, researchers have conducted extensive studies on pressurized leak sealing of inflatable equipment, mainly focusing on sealing defects such as pinholes, microcracks, and bolt gaps in the equipment or pipelines. However, existing polymer adhesive sealing methods cannot achieve rapid sealing of high-pressure inflatable equipment under pressure. Furthermore, existing polymer adhesives are low-viscosity, flowable liquids at room temperature, and are easily dispersed by airflow when applied to gas leak sites. Summary of the Invention

[0004] The purpose of this invention is to overcome the above-mentioned defects in the prior art and provide a leak-sealing adhesive and its preparation method. By compounding a photocurable resin, a modified inorganic filler, and a modified thermally conductive filler, the leak-sealing adhesive has excellent adhesion and rapid curing performance, overcoming the shortcomings of traditional polymer adhesives. It enables rapid pressurized leak sealing of inflatable equipment with air pressure and is applicable to rapid pressurized sealing of sand holes, microcracks, and annular leaks in inflatable equipment.

[0005] To achieve the above objectives, the technical solution of the present invention is as follows:

[0006] A sealing adhesive, the raw materials of which include the following components by mass percentage: 9% to 25% photocurable resin, 0.5% to 1% photoinitiator, 70% to 85% modified inorganic filler and 4% to 6% modified thermally conductive filler; wherein the modified inorganic filler is an inorganic filler modified with silane coupling agent; and the modified thermally conductive filler is a thermally conductive filler modified with silane coupling agent.

[0007] This invention also discloses a method for preparing the sealing adhesive as described above, comprising the following steps:

[0008] A modified inorganic filler is obtained by mixing a silane coupling agent and an inorganic filler.

[0009] A modified thermally conductive filler is obtained by mixing a silane coupling agent and a thermally conductive filler.

[0010] The photocurable resin, photoinitiator, modified inorganic filler, and modified thermally conductive filler are mixed to obtain the sealing adhesive.

[0011] Implementing the embodiments of the present invention will have the following beneficial effects:

[0012] The sealing adhesive of this invention uses a photocurable resin as the main body, with the addition of a photoinitiator, modified inorganic filler, and modified thermally conductive filler, enabling it to cure rapidly under light irradiation, thereby instantly sealing leaks. Simultaneously, a high proportion of modified inorganic filler modified with a silane coupling agent is added. During curing, the silane coupling agent can undergo a coupling reaction with the photocurable resin, forming an interpenetrating network structure between the modified inorganic filler and the main body, increasing the crosslinking density and thus enhancing the adhesive's viscosity. Combined with the toughening effect of the inorganic filler, this further improves the compressive strength of the sealing adhesive, allowing it to withstand the pressure inside the inflation device during curing and preventing bulging, film damage, and other phenomena. However, adding a large amount of modified inorganic filler can absorb light to some extent, affecting the depth of photocuring and leading to incomplete photocuring. Therefore, this embodiment of the invention adds a modified thermally conductive filler modified with a silane coupling agent. The modified thermally conductive filler is dispersed in the bulk to form a thermally conductive network, allowing the heat generated during photocuring to be quickly conducted to the deep photocurable resin, accelerating the molecular thermal motion of the deep photocurable resin, thereby increasing the curing speed. This overcomes the problem of reduced curing speed caused by high amounts of modified inorganic filler, achieving improved adhesion of the sealing adhesive while ensuring rapid and complete curing. Therefore, the sealing adhesive of this embodiment of the invention, by compounding photocurable resin, modified inorganic filler, and modified thermally conductive filler, gives the sealing adhesive excellent adhesion and rapid curing performance.

[0013] In addition, the sealant used in this invention can quickly seal leaks under pressure in inflatable equipment with air pressure, overcoming the shortcomings of traditional polymer adhesives. It is suitable for rapid sealing of pinholes, microcracks, and annular leaks in inflatable equipment under pressure. Attached Figure Description

[0014] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0015] in:

[0016] Figure 1This is a schematic diagram of the sealant applied to pinhole cracks in an air-filled device according to an embodiment of the present invention.

[0017] Figure 2 This is a schematic diagram of the sealing adhesive applied to the flange in the inflation device according to an embodiment of the present invention.

[0018] Figure 3 This is a schematic diagram of the sealant applied to the bolt joint in an inflatable device according to an embodiment of the present invention. Detailed Implementation

[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] This invention discloses a sealing adhesive, the raw materials of which include the following components by weight percentage: 9%–25% photocurable resin, 0.5%–1% photoinitiator, 70%–85% modified inorganic filler, and 4%–6% modified thermally conductive filler; the modified inorganic filler is an inorganic filler modified with a silane coupling agent; the modified thermally conductive filler is a thermally conductive filler modified with a silane coupling agent.

[0021] Specifically, the sealant of the present invention uses light-curing resin as the main body, and adds photoinitiator, modified inorganic filler and modified thermally conductive filler to enable it to cure rapidly under light irradiation, thereby instantly sealing the leak.

[0022] In one specific embodiment, the photocurable resin includes one or more of epoxy acrylate, polyurethane acrylate, and polyester acrylate.

[0023] In one specific embodiment, the photoinitiator includes one or more of benzoyl ketal, benzoin, and ferrocene salts.

[0024] In one specific embodiment, the modified inorganic filler comprises the following components in weight percentages: 70% to 85% inorganic filler and 15% to 30% silane coupling agent.

[0025] Specifically, the modified inorganic filler content in the sealing adhesive of the present invention can reach 70% to 85%. The higher proportion of modified inorganic filler is silane coupling agent modified inorganic filler. Silane coupling agent has both inorganic-philic and organic-philic groups. Therefore, silane coupling agent can simultaneously undergo coupling reaction with inorganic filler and photocurable resin to form an interpenetrating network structure between modified inorganic filler and the main body, which increases the crosslinking density and thus enhances the adhesion of the sealing adhesive. Combined with the toughening effect of inorganic filler, the compressive strength of the sealing adhesive is further improved, enabling it to resist the pressure inside the inflation equipment during the curing process and avoid bulging, film damage and other phenomena.

[0026] In one specific embodiment, the modified thermally conductive filler comprises the following components in weight percentages: 70% to 85% thermally conductive filler and 15% to 30% silane coupling agent.

[0027] Specifically, since adding a large amount of modified inorganic filler can absorb light to a certain extent, affecting the depth of photocuring and leading to incomplete photocuring, this invention adds a modified thermally conductive filler modified with a silane coupling agent. The modified thermally conductive filler is dispersed in the main body to form a thermally conductive network, which allows the heat generated by photocuring to be quickly conducted to the deep photocurable resin, accelerating the molecular thermal motion of the deep photocurable resin, thereby improving the curing speed. This overcomes the problem of reduced curing speed caused by high amounts of modified inorganic filler, and achieves improved adhesion of the sealing adhesive while ensuring its rapid and complete curing.

[0028] In one specific embodiment, the mass ratio of photocurable resin, photoinitiator, and modified inorganic filler is (8-25):(0.5-1):(70-85). Specifically, the present invention further specifies the ratio of photocurable resin, photoinitiator, and modified inorganic filler, which is beneficial to the better formation of interpenetrating network structure, thereby further improving the adhesive strength and compressive strength of the sealing adhesive.

[0029] In one specific embodiment, the modified inorganic filler includes modified inorganic micron fillers and modified inorganic nano fillers. Specifically, two inorganic fillers with different particle sizes are blended, allowing the smaller filler particles to fill the defects and pores between the larger filler particles or between the larger filler particles and the substrate, thereby increasing the packing density and further improving the toughness and adhesion of the sealing adhesive.

[0030] In one specific embodiment, the particle size of the modified inorganic micron filler is 1 μm to 10 μm.

[0031] In one specific embodiment, the particle size of the modified inorganic micron filler includes, but is not limited to, 1μm, 3μm, 5μm, 10μm, etc.

[0032] In one specific embodiment, the particle size of the modified inorganic nanofiller is 10 nm to 20 nm.

[0033] In one specific embodiment, the particle size of the modified inorganic nanofiller includes, but is not limited to, 10 nm, 12 nm, 15 nm, 18 nm, 20 nm, etc.

[0034] In one specific embodiment, the mass ratio of modified inorganic micron filler to modified inorganic nano filler is (15-20):1.

[0035] In one specific embodiment, the mass ratio of the photocurable resin to the modified thermally conductive filler is (8-25):(4-6). Specifically, the sealing adhesive of the present invention, by compounding the photocurable resin and the modified thermally conductive filler in an appropriate ratio, not only ensures that the sealing adhesive has excellent thermal conductivity, thereby improving the curing speed of the sealing adhesive, but also reduces the preparation cost, making it highly applicable to industrial applications.

[0036] In one specific embodiment, the modified thermally conductive filler is a modified thermally conductive nanofiller. Specifically, using a nanoscale modified thermally conductive filler allows it to establish thermally conductive pathways within the gaps of the modified inorganic micron-sized filler, forming a denser thermally conductive network, which is beneficial for improving the thermal conductivity of the substrate.

[0037] In one specific embodiment, the particle size of the modified thermally conductive filler is 50 nm to 80 nm.

[0038] In one specific embodiment, the particle size of the modified thermally conductive filler includes, but is not limited to, 50nm, 60nm, 70nm, 80nm, 90nm, etc.

[0039] In one specific embodiment, the inorganic filler includes one or more of silica, calcium carbonate, and diatomaceous earth.

[0040] In one specific embodiment, the thermally conductive filler includes one or more of boron nitride, aluminum oxide, aluminum nitride, graphene, and carbon nanotubes.

[0041] In one specific embodiment, the silane coupling agent includes one or more of aminosilanes, epoxysilanes, methacryloxysilanes, vinylsilanes, alkylsilanes, sulfur-containing silanes, phenoxysilanes, isocyanate silanes, and fluorosilanes.

[0042] This invention also discloses a method for preparing a sealing adhesive as described in any embodiment of this invention, comprising the following steps:

[0043] 1) Mix the silane coupling agent and the inorganic filler to obtain the modified inorganic filler.

[0044] In one specific embodiment, step 1) specifically includes the following steps:

[0045] 1.1) The inorganic filler and silane coupling agent are mixed with an organic solvent and modified at 50℃~90℃. The silane coupling agent modifies the inorganic filler to obtain the modified inorganic filler.

[0046] 2) Mix the silane coupling agent and the thermally conductive filler to obtain the modified thermally conductive filler.

[0047] In one specific embodiment, step 2) specifically includes the following steps:

[0048] 2.1) The thermally conductive filler and silane coupling agent are mixed with an organic solvent and modified at 50℃~90℃. The silane coupling agent modifies the thermally conductive filler to obtain the modified thermally conductive filler.

[0049] 3) Mix the photocurable resin, photoinitiator, modified inorganic filler and modified thermally conductive filler to obtain the sealing adhesive.

[0050] In one specific embodiment, step 3) specifically includes the following steps:

[0051] 3.1) Mix and grind the modified inorganic filler and the modified thermally conductive filler.

[0052] 3.2) The ground filler is mixed with photocurable resin and photoinitiator in the proportions of any embodiment of the present invention to obtain a sealing adhesive.

[0053] In one specific embodiment, the organic solvent includes one or more of anhydrous ethanol, DMF, ethyl acetate, and acetone.

[0054] The present invention also discloses a pressurized leak sealing method for a leak sealing adhesive prepared using any embodiment of the present invention or the preparation method of any embodiment of the present invention, as detailed below:

[0055] S100. Identify the leak location 11 on the inflation device 10.

[0056] In one specific embodiment, when the leakage location 11 is a pinhole crack or micro-crack, please refer to... Figure 1 As shown, Figure 1 This is a schematic diagram illustrating the application of the sealant to pinhole cracks in an inflation device according to an embodiment of the present invention. The sealant method is as follows:

[0057] S210. Apply sealant to the leaking area 11 and then cure it to form a light-cured coating 20 on the leaking area 11.

[0058] In one specific embodiment, when the leakage location 11 is a ring-shaped leakage location 11, please refer to... Figure 2 and Figure 3 As shown, Figure 2 This is a schematic diagram illustrating the application of the sealing adhesive to the flange in an inflation device according to an embodiment of the present invention. Figure 3 This is a schematic diagram illustrating the application of the sealant to the bolt joints in an inflation device according to an embodiment of the present invention. The sealant method is as follows:

[0059] S220. A drainage pipe 30 is installed at the leakage point 11 to drain the high-pressure fluid and effectively reduce the pressure.

[0060] S221. Apply sealing adhesive to the leaking parts 11 other than the leaking part 11 corresponding to the drainage pipe 30, and cure the sealing adhesive to form a light-cured covering layer 20.

[0061] S222. Remove the drainage tube 30 and use the sealing component 40 to seal the leakage part 11 corresponding to the drainage tube 30.

[0062] In one specific embodiment, the sealing element 40 includes one of screws and bolts.

[0063] In summary, the pressurized sealing method of the present invention uses sealing adhesive on the leaking part 11 and provides light to the leaking part 11 to cure the sealing adhesive and form a light-cured covering layer 21. Since the sealing adhesive can cure quickly under light conditions, it can instantly seal the leaking part 11 and resist the pressure inside the inflation device 10.

[0064] The following are specific embodiments.

[0065] Example 1

[0066] The sealing adhesive of this embodiment comprises the following components by weight percentage: 9% photocurable resin, 1% photoinitiator, 80% modified micron silica (particle size 1μm), 5% modified nano silica (particle size 20nm), and 5% modified nano boron nitride (particle size 50nm).

[0067] Modified micronized silica comprises the following components by weight percentage: 76% silica and 24% fluorosilane.

[0068] Modified nano silica comprises the following components by weight percentage: 76% silica and 24% fluorosilane.

[0069] The modified nano boron nitride comprises the following components by mass percentage: 76% boron nitride and 24% fluorosilane.

[0070] The method for preparing the sealant in this embodiment includes the following steps:

[0071] Weigh according to the above proportions.

[0072] 1) Micron-sized silica and nano-sized silica were respectively mixed with fluorosilane and anhydrous ethanol and then modified at 70°C to obtain modified micron-sized silica and modified nano-sized silica.

[0073] 2) Modified boron nitride nanoparticles were obtained by mixing boron nitride nanoparticles and fluorosilane with anhydrous ethanol and then modifying the mixture at 70°C.

[0074] 3) Mix and grind the modified inorganic filler and the modified thermally conductive filler.

[0075] 4) The ground modified micron silica, modified nano silica, modified nano boron nitride are mixed with photocurable resin and photoinitiator to obtain a sealing adhesive.

[0076] Example 2

[0077] The sealing adhesive of this embodiment comprises the following components by weight percentage: 23% photocurable resin, 1% photoinitiator, 66% modified micron silica (particle size 1μm), 4% modified nano silica (particle size 20nm), and 6% modified nano alumina (particle size 50nm).

[0078] The preparation method of the sealing adhesive in this embodiment is the same as that in Example 1.

[0079] Example 3

[0080] The sealing adhesive of this embodiment comprises the following components by weight percentage: 15% photocurable resin, 1% photoinitiator, 75% modified micron silica (particle size 1μm), 5% modified nano silica (particle size 20nm) and 4% modified nano alumina (particle size 50nm).

[0081] The preparation method of the sealing adhesive in this embodiment is the same as that in Example 1.

[0082] Comparative Example 1

[0083] The only difference between this comparative example and Example 1 is that the modified inorganic filler accounts for 20% of the mass of the sealing adhesive in this comparative example, as follows: The sealing adhesive in this comparative example includes the following components in the following mass ratio: 74% photocurable resin, 1% photoinitiator, 19% modified micron silica, 1% modified nano silica and 5% modified nano boron nitride.

[0084] Comparative Example 2

[0085] The only difference between this comparative example and Example 1 is that the silica in this comparative example is not modified with fluorosilane.

[0086] Comparative Example 3

[0087] The only difference between this comparative example and Example 1 is that the boron nitride in this comparative example is not modified with fluorosilane.

[0088] Comparative Example 4

[0089] The only difference between this comparative example and Example 1 is that this comparative example does not contain modified nano boron nitride.

[0090] Test case

[0091] The adhesive properties, compressive strength, and curing speed of the sealing adhesives of Examples 1-3 and Comparative Examples 1-4 were tested, and the test procedures are as follows:

[0092] The initial tack of the sealing adhesives of Examples 1-3 and Comparative Examples 1-4 was tested according to GB / T 39289-2020 standard;

[0093] The compressive strength of the sealant used in Examples 1-3 and Comparative Examples 1-4 was tested according to GB / T 1041-2008 standard.

[0094] The curing speed of the sealing adhesives of Examples 1-3 and Comparative Examples 1-4 was tested according to GB / T 13477.5-2002 standard;

[0095] The test results are shown in Table 1, which presents the performance tests of the sealing adhesives in Examples 1-3 and Comparative Examples 1-4.

[0096] Table 1 Performance tests of the sealing adhesives in Examples 1-3 and Comparative Examples 1-4

[0097] compressive strength Curing speed Bond strength Example 1 10.8MPa 8s 3.7MPa Example 2 10.6MPa 9s 3.9MPa Example 3 10.2MPa 9s 4.4MPa Comparative Example 1 8.8MPa 11s 2.2MPa Comparative Example 2 8.3MPa 13s 2.8MPa Comparative Example 3 8.6MPa 12s 2.8MPa Comparative Example 4 9.8MPa 11s 2.6MPa

[0098] As shown in Table 1, Examples 1-3 all exhibit high bonding strength, compressive strength, and fast curing speed.

[0099] As shown in Table 1, the curing speeds of Comparative Examples 3 and 4 were significantly slower than those of Example 1 compared to Example 1. This is because the high amount of modified inorganic filler added will absorb light to a certain extent, affecting the photocuring speed. However, Example 1 improved the dispersion of modified boron nitride nanoparticles modified with fluorosilane in the matrix by adding the modified boron nitride nanoparticles modified with fluorosilane, forming a thermally conductive network. This allowed the heat generated by photocuring to be quickly conducted to the deep photocurable resin, accelerating the molecular thermal motion of the deep photocurable resin and thus increasing the curing speed.

[0100] As shown in Table 1, the bonding performance of Comparative Examples 1 and 2 is significantly worse than that of Example 1 compared to Example 1. This is because the sealing adhesive of Example 1 contains a higher proportion of modified inorganic filler, namely fluorosilane-modified inorganic filler. Therefore, during the curing process, the modified inorganic filler can be introduced into the substrate in a covalent manner, forming an interpenetrating network structure between the modified inorganic filler and the substrate, which increases the crosslinking density and thus enhances the adhesion of the sealing adhesive.

[0101] According to the results in Table 1, the compressive strength of Comparative Examples 1 and 2 is significantly worse than that of Example 1 compared with Example 1. This is because the modified inorganic filler in the sealing adhesive of Example 1 is introduced into the main body in a covalent manner, and the toughening effect of the inorganic filler further improves the compressive strength of the sealing adhesive.

[0102] In summary, the sealing adhesive of the present invention, through the synergistic effect of specific amounts of light-curing resin, modified inorganic filler and modified thermally conductive filler, enables the sealing adhesive to have excellent adhesion, toughness and rapid curing performance.

[0103] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A sealing adhesive, characterized in that, Its raw materials include the following components by mass percentage: The composition comprises 9%–25% photocurable resin, 0.5%–1% photoinitiator, 70%–85% modified inorganic filler, and 4%–6% modified thermally conductive filler; the sum of all components is 100%. The modified inorganic filler is an inorganic filler modified with a silane coupling agent; The modified thermally conductive filler is a silane coupling agent modified thermally conductive filler; The modified inorganic filler includes modified inorganic micron fillers and modified inorganic nano fillers; The modified thermally conductive filler is a modified thermally conductive nanofiller; The mass ratio of the modified inorganic micron filler to the modified inorganic nano filler is (15~20):1; The particle size of the modified thermally conductive filler is 50nm~80nm; The particle size of the modified inorganic micron filler is 1μm~10μm; The particle size of the modified inorganic nanofiller is 10nm~20nm; The inorganic filler includes one or more of silicon dioxide, calcium carbonate, and diatomaceous earth. The thermally conductive filler includes one or more of boron nitride, aluminum oxide, aluminum nitride, graphene, and carbon nanotubes.

2. The sealing adhesive according to claim 1, characterized in that, The modified inorganic filler comprises the following components by mass percentage: 70% to 85% of the inorganic filler and 15% to 30% of the silane coupling agent.

3. The sealing adhesive according to claim 2, characterized in that, The modified thermally conductive filler comprises the following components by mass percentage: 70% to 85% of the thermally conductive filler and 15% to 30% of the silane coupling agent.

4. The sealing adhesive according to claim 3, characterized in that, The silane coupling agent includes one or more of aminosilane, epoxysilane, methacryloxysilane, vinylsilane, alkylsilane, sulfur-containing silane, phenoxysilane, isocyanate-based silane, and fluorosilane.

5. The sealing adhesive according to claim 1, characterized in that, The photocurable resin includes one or more of epoxy acrylate, polyurethane acrylate, and polyester acrylate; The photoinitiator includes one or more of benzoyl ketone, benzoin, and ferrocene salts.

6. A method for preparing a sealing adhesive as described in any one of claims 1 to 5, characterized in that, Includes the following steps: A modified inorganic filler is obtained by mixing a silane coupling agent and an inorganic filler. A modified thermally conductive filler is obtained by mixing a silane coupling agent and a thermally conductive filler. The photocurable resin, photoinitiator, modified inorganic filler, and modified thermally conductive filler are mixed to obtain the sealing adhesive.

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