Near-infrared curing composition with high filler loading

Abstract

The present invention relates to a near-infrared curing composition with high filler loading, and more specifically, to a near-infrared-curing balancing clay and a preparation method therefor. The balancing clay is a single component, and is characterized by a high specific gravity, a fast curing rate, high filler loading, and a deep curing thickness. The present invention utilizes near-infrared curing technology to flexibly adjust a proportion of resin to filler, allowing for rapid curing of low-resin, high-filler systems. The prepared balancing clay has a wide density range, and can be applied to various motor rotors. Moreover, the product is easy to handle and use, and exhibits excellent adhesion performance and flexibility. Using a near-infrared curing mechanism allows for a balancing clay having a high filler, a large area, and a deep thickness (> 10 mm) to be cured within a short period of time, while reducing working time, and optimizing application steps.

Description

A near-infrared curing composition with a high filler content Technical Field

[0001] This invention relates to a near-infrared curing composition with a high filler content, and more specifically, to a near-infrared curing balanced mud adhesive. Background Technology

[0002] Balanced mortar, also known as specific gravity mortar or dynamic balancing mortar, can cure quickly and is used in various precision motor systems to help maintain balance during high-speed operation.

[0003] An electric motor rotor has two centers: a center of mass and a center of rotation. In a perfectly designed and manufactured state, the center of mass and the center of rotation coincide. During high-speed rotation, the centrifugal forces in all directions are balanced, resulting in peak motor efficiency and low noise and vibration levels. However, due to limitations in raw materials and assembly errors, a certain deviation often exists between the center of mass and the center of rotation in actual operation. Adding a certain mass of balancing adhesive to specific locations on the rotor alters its mass distribution, thereby adjusting the rotor's center of mass to be as close as possible to the center of rotation. This balancing adhesive is typically viscous and elastic, not only adjusting the mass distribution but also absorbing vibration energy caused by rotor imbalance, further mitigating the impact of vibration on the motor rotor.

[0004] Balanced putty is mainly a mixture of resin and filler, with the resin typically having a density of 1 g / cm³. 3 The density of fillers varies considerably depending on their properties. To ensure complete curing of the balancing putty, the resin component often constitutes a large proportion, resulting in a generally low density of the balancing putty. Since the motor rotor is made of copper, a large amount of balancing putty is needed to balance the center of gravity when the balancing putty density is low.

[0005] In existing technologies, most balancing putty adhesives are thermosetting, requiring several hours to fully cure, making the process complex and unsuitable for automated production. Patent CN 108504043A, however, uses AB-component epoxy resin to prepare a balancing putty adhesive with weather resistance, anti-peeling, and stain resistance; the density of this balancing putty adhesive is 3.7–4.3 g / cm³. 3 The curing time is 5–5.5 hours. Patent publication CN 116535139A describes the preparation of a thermally conductive and high-temperature resistant balancing putty using organosilicon epoxy resin; the density of this balancing putty is 3.94–4.17 g / cm³. 3 The curing time is 4.8–5.5 hours. In the aforementioned thermosetting patents, the curing time of the balancing putty adhesive all exceeds 5.5 hours, and the density does not exceed 4.3 g / cm³. 3 .

[0006] UV-curable balancing putty has advantages such as fast curing speed and convenient operation. Patent publication CN 116970365A describes a highly weather-resistant UV-curable balancing putty prepared using modified organosilicon acrylic resin; the density of this balancing putty is 2.90–4.20 g / cm³. 3 The curing depth is 3.85–5.28 mm. Patent publication CN117143558A describes the preparation of a UV-curable adhesive; the density of this balanced putty is 2.62–3.10 g / cm³. 3 The curing depth is 3.98–5.46 mm. The thickness of the aforementioned light-cured balancing putty does not exceed 5.5 mm, and the density does not exceed 4.2 g / cm³. 3 .

[0007] The motor rotor is primarily made of high-purity copper (density 8.96 g / cm³). 3 Currently, most patented balanced clay adhesives have a low density (not exceeding 5 g / cm³). 3 The density of this low-density balancing mud differs significantly from that of the motor rotor itself, often requiring a large amount to balance the center of gravity during use. On the one hand, a large amount of low-density balancing mud increases the difficulty of use; on the other hand, it occupies a large amount of internal space in the motor, which is not conducive to optimizing the motor's size.

[0008] Therefore, it is necessary to develop a new balanced mud composition to address the shortcomings of existing balanced mud adhesives, such as long curing time, insufficient curing depth, and low specific gravity. Summary of the Invention

[0009] To address the shortcomings of current technology, this invention provides a near-infrared curing balanced mud composition with a high filler content.

[0010] This invention utilizes a near-infrared light curing mechanism. Firstly, near-infrared light has high penetrability; the upconversion material absorbs near-infrared light and converts it into ultraviolet-visible light, thereby exciting the photoinitiator to induce the polymerization of the photosensitive resin. Secondly, near-infrared light is an electromagnetic wave, which causes friction-collision and reciprocating motion of molecules during propagation, generating a thermal effect. Under the action of this thermal effect, the resin system is promoted to cross-link and cure, requiring only a small amount of resin to achieve rapid curing under conditions of high filler content and deep thickness.

[0011] This invention features a low resin content and a high filler content, resulting in a wide adjustable density range for the near-infrared curing equilibrium mud. Furthermore, the near-infrared curing system is compatible with various filler systems, such as ceramic powder, metal powder, metal oxide powder, and non-metal oxide powder. When combined with fillers of high thermal conductivity, it further enhances the heat transfer of the resin system, increasing the reaction rate and conversion efficiency.

[0012] The first aspect of the present invention provides a near-infrared photocurable high filler content balanced mud adhesive, comprising the following components in parts by weight: main resin: 5-50 parts, reactive diluent: 0-20 parts, filler: 50-95 parts, photoinitiator: 1-6 parts, upconversion material: 0.5-4 parts, thixotropic agent: 1-6 parts, and additives: 1-5 parts.

[0013] In a further preferred embodiment, the present invention provides a near-infrared photothermal synergistic curing high filler content balanced mud adhesive, comprising the following components in parts by weight: main resin: 5-50 parts, reactive diluent: 0-20 parts, filler: 50-95 parts, thermal initiator: 1-6 parts, upconversion material: 0.5-4 parts, thixotropic agent: 1-6 parts, and additives: 1-5 parts.

[0014] In a preferred embodiment of the present invention, a near-infrared photothermal synergistic curing mechanism is formed by adding a thermal initiator to the near-infrared photocuring system. The thermal effect generated by the near-infrared light source and upconversion particles can promote the decomposition of the thermal initiator without heating, generating highly active free radicals, which can further accelerate the polymerization reaction between resins, resulting in an extremely high double bond conversion rate in the resin system. Compared with the near-infrared photocuring mechanism, the near-infrared photothermal synergistic curing mechanism requires less resin, has a faster rate, and a higher resin double bond conversion rate.

[0015] Furthermore, the main resin is a multifunctional acrylate oligomer containing two or more acrylate functional groups.

[0016] Further preferably, the multifunctional acrylate oligomer is selected from multifunctional epoxy acrylate, multifunctional polyurethane acrylate, multifunctional polyester acrylate, and multifunctional polyether acrylate.

[0017] In some preferred embodiments, the main resin is one or a mixture of multiple of the following: 6126, 6147, 6145-100, 6146-100, 6196-100, 6261, and 6311-100 from Changxing Materials Industry Co., Ltd., and RY1101, RY1102, RY2232, RY2250, and RY2252 from Ruiyang Chemical Co., Ltd.

[0018] Furthermore, the active diluent contains one or more acrylate groups in its structure; and has a molecular weight of less than 1000 g / mol and a viscosity of less than 500 cps (at 25°C).

[0019] In some preferred embodiments, the reactive diluent is selected from one or a combination of stearate acrylate (SA), isobornyl methacrylate (IBOA), benzyl acrylate, tetrahydroconjugyl methacrylate (THFA), 1,6-hexanediol acrylate (HDDA), 1,4-butanediol diacrylate (BDDA), pentaerythritol triacrylate (PETA), trimethylolpropane triacrylate (TMPTA), tricyclopropane oxide trimethylolpropane triacrylate, pentaerythritol tetraacrylate (PETEA), bis(trimethylolpropane tetraacrylate) (DTMPTA), and bis(pentaerythritol hexaacrylate) (DPHA).

[0020] In some preferred embodiments, the near-infrared light-curable high filler content balanced mud adhesive comprises the following components in parts by weight: main resin: 8-30 parts, reactive diluent: 1-5 parts, filler: 65-95 parts, photoinitiator: 1-4 parts, upconversion material: 0.5-3 parts, thixotropic agent: 1-3 parts, and additives: 1-3 parts.

[0021] In some preferred embodiments, the near-infrared photothermal synergistic curing high filler content balanced mud adhesive comprises the following components in parts by weight: main resin: 8-30 parts, reactive diluent: 1-5 parts, filler: 65-95 parts, photoinitiator: 1-4 parts, thermal initiator: 1-4 parts, upconversion material: 0.5-3 parts, thixotropic agent: 1-3 parts, and additives: 1-3 parts.

[0022] Furthermore, the filler is selected from one or a combination of ceramic powder, metal powder, metal oxide powder, and inorganic non-metallic powder. Further explanation: the ceramic powder includes, but is not limited to, alumina, zirconium oxide, zinc oxide, barium titanate, aluminum titanate, boron nitride, aluminum nitride, silicon nitride, and silicon nitride; the metal powder includes, but is not limited to, tungsten powder, magnesium powder, silver powder, tin powder, nickel powder, iron powder, copper powder, and aluminum alloy powder; the metal oxide powder includes, but is not limited to, magnesium oxide powder, calcium oxide powder, copper oxide powder, alumina powder, and titanium oxide; the inorganic non-metallic powder includes, but is not limited to, silicon dioxide, mica powder, graphite powder, and kaolin powder.

[0023] In some embodiments, the filler is a high thermal conductivity filler or a mixed filler including the high thermal conductivity filler; in some embodiments, the high thermal conductivity filler is metal powder or metal oxide powder. In some preferred embodiments, the filler is a mixture of metal powder and a first filler; the first filler is selected from the ceramic powder, metal oxide powder, and inorganic non-metallic powder. In some embodiments, the mass ratio of metal powder to the first filler is 1:2 to 2:1.

[0024] Near-infrared light irradiation and the thermal effect generated by upconversion particles act on the highly thermally conductive filler, accelerating the heat transfer of the system and further promoting cross-linking and curing, thus achieving a better curing effect.

[0025] In some preferred embodiments, fillers with highly conductive metals are used. Compared to mixed filler systems, these systems exhibit faster curing rates and higher resin conversion efficiency.

[0026] In some embodiments, the filler is a mixture of ceramic powder and a second filler; the second filler is selected from metal powder, metal oxide powder, and inorganic non-metallic powder.

[0027] Furthermore, the photoinitiator is a free radical initiator. In some embodiments, the photoinitiator is selected from phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide (819), diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO), 2-hydroxy-2-methyl-1-phenyl-1-propanone (1173), bis(2,6-difluoro-3-pyrrolephenyl)dicenoctane (784), benzophenone (BP), or a combination thereof.

[0028] In some preferred embodiments, the photoinitiator is a composite photoinitiator consisting of phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide (819) and bis(2,6-difluoro-3-pyrrolidinyl)dicenoctanetane (784).

[0029] Furthermore, the thermal initiator is a free radical initiator. In some embodiments, the thermal initiator is selected from one or a combination of benzoyl peroxide (BPO), di-tert-butyl peroxide (DTBP), methyl ethyl ketone peroxide (MEKP), azobisisobutyronitrile (AIBN), and azobisisoheptanenitrile (ABVN).

[0030] In some preferred embodiments, the thermal initiator is a compound thermal initiator composed of azobisisobutyronitrile (AIBN) and azobisisoheptanenitrile (ABVN).

[0031] Furthermore, the upconversion material is selected from one or a combination of NaYF4, BaYF5, NaGdF4, LiYF4, NaYbF4, Na3ScF6, YF3, and GdOF; in some preferred embodiments, NaYF4 is used as the upconversion material.

[0032] Furthermore, the thixotropic agent is selected from one or a combination of fumed silica, hydrogenated castor oil, organobentonite, and polyamide wax.

[0033] Furthermore, the additives include: silane coupling agents, adhesion promoters, antioxidants, and dispersants.

[0034] In some embodiments of the present invention, the additives include silane coupling agents and dispersants; further, the silane coupling agent is selected from one or a combination of KH 550, KH 560, and KH 570; further, the dispersant is selected from one or a combination of BYK-4310 and BYK 110.

[0035] Furthermore, the specific gravity of the balancing mud can reach 2-9 g / cm³. 3 Further optimization is to select a specific gravity of 6-9 g / cm³. 3 .

[0036] In some embodiments of the present invention, the specific gravity of the balancing mud is 2.75-8.93 g / cm³. 3 .

[0037] In some embodiments of the present invention, the curing depth of the balancing mud is ≥8 mm. In some preferred embodiments, the curing depth is ≥10 mm.

[0038] Another aspect of the present invention is to provide a method for preparing the near-infrared curable high filler content balanced mud, the specific steps of which are: S1. The main resin, reactive diluent and filler are placed in a planetary disperser and dispersed evenly under vacuum and light-proof conditions; S2. Initiator, upconversion particles, thixotropic agent and additives are added and dispersed further under vacuum and light-proof conditions. After the composition is evenly mixed, it is taken out and sealed in a light-proof package for later use.

[0039] In some embodiments, the stirring time in step S1 is 10-40 min; in some embodiments, the stirring time in step S2 is 10-40 min.

[0040] In one embodiment of the present invention, the preparation method of the balanced mud adhesive includes the following steps: placing the main resin, reactive diluent, and filler into a planetary disperser and dispersing and stirring for 30 minutes under vacuum and light-proof conditions; then placing the initiator, upconversion particles, thixotropic agent, and additives into the planetary disperser and dispersing and stirring for 30 minutes under vacuum and light-proof conditions; after mixing evenly, removing and sealing the mixture in a light-proof and airtight package for later use.

[0041] Another aspect of the present invention is to provide a method for using the near-infrared curing high filler content balancing mud, the steps of which are: applying the balancing mud to the area to be used, and curing it using a near-infrared light source.

[0042] Furthermore, the near-infrared light source is a light source with a wavelength of 780nm-2000nm. In some embodiments, the curing time is 0-10 seconds.

[0043] The present invention discloses a curing method for a balanced putty that utilizes upconversion particles of lanthanide rare earth elements as a medium. Irradiation with a near-infrared light source converts near-infrared light at a long wavelength of 980 nm into short-wave ultraviolet light. The photoinitiator in the system absorbs ultraviolet light and undergoes cleavage to form active free radicals, which promote cross-linking polymerization of the resin and reactive diluent. Only a small amount of resin is needed for the balanced putty to cure completely in a short time.

[0044] Adding a thermal initiator to a near-infrared light curing system can promote the action of the thermal initiator due to the thermal effect of near-infrared light and upconversion particles, further accelerating the cross-linking and curing of the resin system, allowing for complete curing in a shorter time.

[0045] Beneficial effects of the present invention

[0046] This invention provides a near-infrared curing balanced putty with a high filler content, compared to existing technologies:

[0047] (1) The balancing mud adhesive of the present invention is a single component, which can be used directly according to needs, which is convenient and quick, has a short curing time, can improve construction efficiency, and has excellent bonding performance and flexibility; compared with the existing thermosetting technology, it has a faster curing speed and a higher specific gravity.

[0048] (2) The balanced mud adhesive of the present invention can achieve deep curing in a short time, with a curing depth of 8-10mm; it can cure high filler content systems, large areas, and thick depth specific gravity mud adhesives; and it has a wider range of applications.

[0049] (3) The resin content in the balanced mud adhesive of the present invention is low (the filler content is high). The heat effect generated by the near-infrared light source and upconversion particles further promotes the curing and cross-linking of the balanced mud adhesive. Only a small amount of resin is needed to completely cure the balanced mud adhesive.

[0050] (4) The balancing clay of the present invention can be completely cured with a small amount of resin, so the product has the characteristics of high solid content and high specific gravity, with a density of 2.75-8.93 g / cm³. 3 The single-component balanced mud adhesive of the present invention can achieve different densities not only by adjusting the ratio of the main resin and filler, but also by adjusting the type and combination of fillers; thus achieving a wider density range; and the specific gravity is easy to adjust, making it suitable for a wider range of applications. Attached Figure Description

[0051] The accompanying drawings are provided to further illustrate the present application and form part of the specification. They are used together with the embodiments of the present application to explain the application and do not constitute a limitation thereof. In the drawings:

[0052] Figure 1. Infrared test results of the near-infrared curing system in Example 1;

[0053] Figure 2 shows the infrared test results of the near-infrared photothermal curing system in Example 11. Detailed Implementation

[0054] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the examples in the specification. Many specific details are set forth in the following description to provide a thorough understanding of the present invention; however, the present invention may also be implemented in other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of the present invention. Therefore, the present invention is not limited to the embodiments disclosed below.

[0055] The testing method is as follows:

[0056] Curing depth: Place the sample in a cube mold. After curing, remove it from the mold and measure the thickness of the cured part of the adhesive layer with a vernier caliper.

[0057] Specific gravity (density): Using a specific gravity cup with a known volume, first weigh the empty specific gravity cup, then weigh the cup filled with equilibrium mud, and calculate the density.

[0058] Viscosity: Rheometer (Model: Thermo Fisher-MARS60, Rotor: P20)

[0059] Compressive strength: A universal testing machine is used to apply pressure to a cylinder with a diameter of 50 mm and a height of 100 mm until the sample breaks. The maximum pressure that the sample can withstand at the point of failure is measured.

[0060] Resin conversion rate test: Fourier transform infrared spectroscopy was used to characterize the resin before and after curing, and the area of ​​double bond absorption peaks was calculated.

[0061] Surface temperature: Tested using an infrared thermometer.

[0062] Table 1 Raw material ratios for each embodiment

[0063] Example 1: Preparation of a near-infrared photocurable composition with a high filler content:

[0064] Sequentially, 28 parts of 6145-100, 2 parts of TMPTA, and 70 parts of alumina were placed in a planetary disperser, heated to 50°C, and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of fumed silica, 1 part of silane coupling agent KH 550, and 1 part of dispersant BYK 110 were placed in a 50°C reactor and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0065] When using, take out a certain amount of balancing mud and apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0066] Example 2: Preparation of a near-infrared light-cured composition with a high filler content:

[0067] RY2250 (25 parts), HDDA (5 parts), and zirconium oxide (70 parts) were sequentially placed into a planetary disperser and heated to 50°C. The mixture was dispersed and stirred under vacuum and light-protected conditions for 30 minutes. Then, photoinitiator 819 (1 part), photoinitiator 784 (2 parts), NaYF4 (1 part), fumed silica (1 part), silane coupling agent KH 570 (1 part), and dispersant BYK 110 (1 part) were placed into a 50°C reactor and dispersed and stirred under vacuum and light-protected conditions for 30 minutes. After dispersion, the mixture was removed and sealed in a light-protected container for later use.

[0068] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0069] Example 3: Preparation of a near-infrared light-cured composition with a high filler content:

[0070] 6145-100 (15 parts), TMPTA (3 parts), and barium titanate (82 parts) were sequentially placed into a planetary disperser and heated to 55°C. The mixture was dispersed and stirred under vacuum and in the dark for 40 minutes. Then, photoinitiator 819 (1 part), photoinitiator 784 (2 parts), fumed silica (1 part), silane coupling agent KH 550 (1 part), and dispersant BYK 110 (1 part) were placed into a 55°C reactor and dispersed and stirred under vacuum and in the dark for 40 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0071] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0072] Example 4: Preparation of a near-infrared light-curable composition with a high filler content:

[0073] Sequentially, 21 parts of 6145-100, 4 parts of TMPTA, 50 parts of zirconium oxide, and 25 parts of copper powder were placed in a planetary disperser, heated to 55°C, and dispersed and stirred under vacuum and light-proof conditions for 40 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of fumed silica, 1 part of silane coupling agent KH 550, and 1 part of dispersant BYK 110 were placed in a 55°C reactor and dispersed and stirred under vacuum and light-proof conditions for 40 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0074] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0075] Example 5: Preparation of a near-infrared light-cured composition with a high filler content:

[0076] Sequentially, 17 parts of 6146-100, 3 parts of DPHA, 30 parts of barium titanate, and 25 parts of nickel powder were placed in a planetary disperser, heated to 55°C, and dispersed and stirred under vacuum and light-proof conditions for 40 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of fumed silica, 1 part of silane coupling agent KH 560, and 1 part of dispersant BYK 110 were placed in a 55°C reactor and dispersed and stirred under vacuum and light-proof conditions for 40 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0077] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0078] Example 6: Preparation of a near-infrared light-cured composition with a high filler content:

[0079] Sequentially, 17 parts of 6145-100, 3 parts of HDDA, 22 parts of zirconium oxide, and 60 parts of copper powder were placed in a planetary disperser, heated to 55°C, and dispersed and stirred under vacuum and light-proof conditions for 40 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of fumed silica, 1 part of silane coupling agent KH 550, and 1 part of dispersant BYK 110 were placed in a 55°C reactor and dispersed and stirred under vacuum and light-proof conditions for 40 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0080] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0081] Example 7: Preparation of a near-infrared light-cured composition with a high filler content:

[0082] RY2250 (16 parts), HDDA (4 parts), and copper powder (80 parts) were sequentially placed into a planetary disperser and heated to 55°C. The mixture was dispersed and stirred under vacuum and light-protected conditions for 40 minutes. Then, photoinitiator 819 (1 part), photoinitiator 784 (2 parts), NaYF4 (1 part), gaseous silicon (1 part), silane coupling agent KH 570 (1 part), and dispersant BYK 110 (1 part) were placed into a 55°C reactor and dispersed and stirred under vacuum and light-protected conditions for 40 minutes. After dispersion, the mixture was removed and sealed in a light-protected container for later use.

[0083] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0084] Example 8: Preparation of a near-infrared light-curable composition with a high filler content:

[0085] Sequentially, 28 parts of 6145-100, 2 parts of TMPTA, 40 parts of alumina, and 30 parts of copper powder were placed in a planetary disperser, heated to 50°C, and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of fumed silica, 1 part of silane coupling agent KH 570, and 1 part of dispersant BYK 110 were placed in a 50°C reactor and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0086] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0087] Example 9: Preparation of a near-infrared light-curable composition with a high filler content:

[0088] 28 parts of 6145-100, 2 parts of TMPTA, 40 parts of alumina, and 30 parts of tungsten powder were sequentially placed into a planetary disperser and heated to 50°C. The mixture was then dispersed and stirred under vacuum and light-protected conditions for 30 minutes. Next, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of fumed silica, 1 part of silane coupling agent KH 570, and 1 part of dispersant BYK 110 were placed into a 50°C reactor and dispersed and stirred under vacuum and light-protected conditions for 30 minutes. After dispersion, the mixture was removed and sealed in a light-protected container for later use.

[0089] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0090] Example 10: Preparation of a near-infrared light-curable composition with a high filler content:

[0091] Sequentially, 28 parts of 6145-100, 2 parts of TMPTA, and 70 parts of copper powder were placed in a planetary disperser, heated to 50°C, and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of NaYF4, 1 part of gaseous silicon, 1 part of silane coupling agent KH 560, and 1 part of dispersant BYK 110 were placed in a 50°C reactor and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0092] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0093] Example 11: Preparation of a high filler content composition for near-infrared photothermal synergistic curing:

[0094] Sequentially, 28 parts of 6145-100, 2 parts of TMPTA, and 70 parts of alumina were placed in a planetary disperser and heated to 50°C. The mixture was dispersed and stirred under vacuum and in the dark for 30 minutes. Next, 1 part of photoinitiator 819, 2 parts of photoinitiator-784, 1 part of thermal initiator AIBN, 1 part of NaYF4, 1 part of gaseous silica, 1 part of silane coupling agent KH 550, and 1 part of dispersant BYK 110 were placed in a 50°C reactor and dispersed and stirred under vacuum and in the dark for 30 minutes. After dispersion, the mixture was removed and sealed in a light-proof container for later use.

[0095] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0096] Example 12: Preparation of a high filler content composition for near-infrared photothermal synergistic curing:

[0097] Sequentially, 15 parts of 6145-100, 5 parts of TMPTA, 50 parts of alumina, and 30 parts of copper powder were placed in a planetary disperser, heated to 50°C, and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator-784, 1 part of thermal initiator AIBN, 1 part of NaYF4, 1 part of gaseous silicon, 1 part of silane coupling agent KH 550, and 1 part of dispersant BYK 110 were placed in a 50°C reactor and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. After dispersion, the mixture was removed, sealed in a light-proof container, and stored for later use.

[0098] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0099] Example 13: Preparation of a high filler content composition for near-infrared photothermal synergistic curing:

[0100] 8 parts RY2250, 2 parts HDDA, and 90 parts copper powder were sequentially placed into a planetary disperser and heated to 60°C. The mixture was dispersed and stirred under vacuum and light-protected conditions for 50 minutes. Then, 1 part photoinitiator 819, 2 parts photoinitiator 784, 1 part thermal initiator ABVN, 1 part NaYF4, 1 part gaseous silicon, 1 part silane coupling agent KH 570, and 1 part dispersant BYK 110 were placed into a 60°C reactor and dispersed and stirred under vacuum and light-protected conditions for 50 minutes. After dispersion, the mixture was removed and sealed in a light-protected container for later use.

[0101] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0102] Example 14: Preparation of a high filler content composition for near-infrared photothermal synergistic curing:

[0103] RY2250 (17 parts), HDDA (3 parts), alumina (40 parts), and tungsten powder (40 parts) were sequentially placed into a planetary disperser and heated to 55°C. The mixture was dispersed and stirred under vacuum and light-protected conditions for 40 minutes. Then, photoinitiator 819 (1 part), photoinitiator 784 (2 parts), thermal initiator ABVN (1 part), NaYF4 (1 part), gaseous silicon (1 part), silane coupling agent KH 570 (1 part), and dispersant BYK 110 (1 part) were placed into a 55°C reactor and dispersed and stirred under vacuum and light-protected conditions for 40 minutes. After dispersion, the mixture was removed and sealed in a light-protected container for later use.

[0104] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a near-infrared light source (800nm-1050nm).

[0105] Comparative Example 1:

[0106] Compared with Example 1, this comparative sample did not contain upconversion particles, was cured using a UV light source, and the remaining steps were the same.

[0107] Sequentially, 28 parts of 6145-100, 2 parts of TMPTA, and 70 parts of alumina were placed in a planetary disperser, heated to 50°C, and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. Then, 1 part of photoinitiator 819, 2 parts of photoinitiator 784, 1 part of fumed silica, 1 part of silane coupling agent KH 550, and 1 part of dispersant BYK 110 were placed in a 50°C reactor and dispersed and stirred under vacuum and light-proof conditions for 30 minutes. After dispersion, the mixture was removed and sealed in a light-proof package for later use.

[0108] When using, take out a certain amount of balancing putty, apply it to the position of the motor rotor that needs to be balanced, and then cure it with a UV light source.

[0109] Comparative Example 2:

[0110] Data from Example 1 in patent CN 108504043 A was used.

[0111] Comparative Example 3:

[0112] Data from Example 1 in patent CN 116970365 A was used.

[0113] Comparative Example 4:

[0114] Data from Example 3 of patent CN 117143558 A was used.

[0115] Results analysis:

[0116] The performance test data for each embodiment and comparative example are shown in Table 2.

[0117] Table 2 Performance Tests of Examples and Comparative Examples

[0118] As shown in Table 2, the density of the near-infrared photocurable equilibration mud prepared by this invention is 2.75-8.93 g / cm³. 3 The curing depth can reach over 8mm, and even exceed 10mm. The near-infrared light curing system (Examples 1-10) has a fast curing rate, with a curing time of less than 5 seconds; the near-infrared photothermal synergistic system (Examples 11-14) has an even faster curing rate, with a curing time of less than 3 seconds. Furthermore, the cured equilibrium mud adhesive has high strength, comparable to the compressive strength of existing thermosetting equilibrium mud adhesives. Moreover, the equilibrium mud adhesive system of this invention has a low viscosity, making it suitable for dispensing processes in industrial production.

[0119] As shown in Table 2, the specific gravity of the adhesive mortar of this invention ranges from 2.75 to 8.93, covering a wide density range. This allows for adjustment of the system's specific gravity by modifying the filler type for different application scenarios, making it widely applicable. This characteristic is attributed to both the variation in filler specific gravity and the high filler content of the system. Adjusting the filler type directly affects the system's density, synergistically achieving this effect. In systems with a low filler content, this effect cannot be achieved simply by adjusting the filler type.

[0120] Table 3. Double bond conversion rate of near-infrared curing system

[0121] As shown in Figures 1 and 2 and Table 3, the resin conversion rate data of the near-infrared curing system / near-infrared photothermal curing system of the present invention indicate that a high double bond conversion rate can be achieved in a short time in systems with a high filler content. The double bond conversion rate (44.21%) of the near-infrared photothermal synergistic curing system (Example 11) with the same formulation is higher than that of the near-infrared photocuring system (Example 1) (34.41%), indicating that the near-infrared photothermal synergistic curing system can further promote the resin system reaction and improve the resin conversion rate.

[0122] Table 4. Near-infrared curing system - surface temperature during curing

[0123] As shown in Table 4, the surface temperature during curing of the near-infrared curing system / near-infrared photothermal curing system of the present invention is as follows. Examples 8 and 9, compared to Example 1, added some dark-colored fillers with heat-absorbing effects, which intensified the heat transfer effect, resulting in higher curing temperatures and deeper curing thicknesses. Example 10 used a highly thermally conductive metal filler, which, compared to the mixed filler system, further increased the curing temperature and further deepened the curing thickness.

[0124] Compared to Comparative Example 1, the embodiments of this invention exhibit greater density and deeper cured thickness. Comparative Example 1 only achieved a cured depth of 0.29 mm, due to limited UV light penetration and the absorption or scattering of the light source by molecules in the mortar, resulting in an exponential decrease in light intensity with increasing depth. This light attenuation is even more pronounced in high-filler systems. Compared to Comparative Example 2, the invention demonstrates greater density and a shorter curing time while maintaining comparable compressive strength; furthermore, the process is simpler, eliminating the need for a two-component mixing step. Compared to Comparative Examples 3 / 4, this invention offers significant advantages in specific gravity and cured depth; the overall performance of the specific gravity mortar is significantly superior.

[0125] This invention provides a single-component, fast-curing, wide-density-range, and deep-curing balanced clay adhesive and its preparation method. Compared with the prior art, the balanced clay adhesive of this invention has a low resin content (high filler content) and its density can be easily adjusted according to the application scenario. Moreover, the product is easy to operate and use, and has excellent bonding performance and flexibility.

[0126] The balanced clay adhesive provided by this invention utilizes a near-infrared light curing mechanism: Firstly, near-infrared light has high penetrability and, with the assistance of upconversion particles, is converted into ultraviolet light, enabling deep curing of the balanced clay adhesive. Secondly, the irradiation by the near-infrared light source and the thermal effect generated by the upconversion particles promote further cross-linking and curing of the system, requiring only a small amount of resin for complete curing of the balanced clay adhesive.

[0127] Furthermore, the balanced clay adhesive provided by this invention uses a near-infrared photothermal synergistic curing mechanism: a thermal initiator is added to the near-infrared photocuring system. Due to the thermal effect of near-infrared light, the thermal initiator can be decomposed without heating. Under photothermal synergistic conditions, the balanced clay adhesive can be completely cured in a shorter time and has higher compressive strength.

[0128] Furthermore, the balanced mud adhesive of the present invention has a suitable viscosity, making it suitable for industrial production.

[0129] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the present invention.

Claims

1. A near-infrared curing, high filler content balanced mud adhesive, characterized in that, It includes the following components in parts by weight: Main resin: 5-40 parts; Reactive diluent: 0-15 parts; Filler: 50-95 parts; Photoinitiator: 1-6 parts; Upconversion material: 0.5-4 parts; Thixotropic agent: 1-6 parts; Additives: 1-5 parts; The main resin is a multifunctional acrylate oligomer containing two or more acrylate functional groups.

2. The near-infrared curing high filler content balanced mud adhesive according to claim 1, characterized in that, It includes the following components in parts by weight: Main resin: 5-40 parts; Reactive diluent: 0-15 parts; Filler: 50-95 parts; Photoinitiator: 1-6 parts; Thermal initiator: 1-6 parts; Upconversion material: 0.5-4 parts; Thixotropic agent: 1-6 parts; Additives: 1-5 parts.

3. The near-infrared curing high filler content balanced mud adhesive according to claim 1 or 2, characterized in that, The multifunctional acrylate oligomers are selected from multifunctional epoxy acrylates, multifunctional polyurethane acrylates, multifunctional polyester acrylates, and multifunctional polyether acrylates. And / or, the active diluent contains one or more acrylate groups in its structure; and has a molecular weight of less than 1000 g / mol and a viscosity of less than 500 cps.

4. The near-infrared curing high filler content balanced mud adhesive according to claim 1 or 2, characterized in that, The filler is selected from one or a combination of ceramic powder, metal powder, metal oxide powder, and inorganic non-metallic powder; The ceramic powder includes, but is not limited to: alumina, zirconium oxide, zinc oxide, barium titanate, aluminum titanate, boron nitride, aluminum nitride, silicon nitride, and silicon nitride. The metal powders include, but are not limited to: tungsten powder, magnesium powder, silver powder, tin powder, nickel powder, iron powder, copper powder, and aluminum alloy powder; The metal oxide powders include, but are not limited to: magnesium oxide powder, calcium oxide powder, copper oxide powder, aluminum oxide powder, and titanium oxide. The inorganic non-metallic powders include, but are not limited to: silicon dioxide, mica powder, graphite powder, and kaolin powder.

5. The near-infrared curing high filler content balanced mud adhesive according to claim 4, characterized in that, The filler is a mixture of ceramic powder and a second filler; The second filler is selected from metal powder, metal oxide powder, and inorganic non-metallic powder.

6. The near-infrared curing high filler content balanced mud adhesive according to claim 1 or 2, characterized in that, The upconversion material is selected from one or a combination of NaYF4, BaYF5, NaGdF4, LiYF4, NaYbF4, Na3ScF6, YF3, and GdOF; And / or, the thixotropic agent is selected from one or a combination of fumed silica, hydrogenated castor oil, organobentonite, and polyamide wax; And / or, the additives are selected from silane coupling agents, adhesion promoters, antioxidants, and dispersants.

7. The near-infrared curing high filler content balanced mud adhesive according to claim 1 or 2, characterized in that, The specific gravity of the composition is 2-9 g / cm³. 3 .

8. The method for preparing the near-infrared curing high filler content balanced clay adhesive as described in any one of claims 1-7, characterized in that, The specific steps are as follows: S1. Place the main resin, reactive diluent, and filler into a planetary disperser and disperse them evenly under vacuum and light-proof conditions; S2. Add initiator, upconversion particles, thixotropic agent and additives, and continue to disperse under vacuum and light-proof conditions. After the composition is mixed evenly, take it out and seal it in a light-proof and airtight package for later use.

9. The method of using the near-infrared curing high filler content balanced mud adhesive according to any one of claims 1-7, characterized in that, Apply the composition to the area to be used and cure it using a near-infrared light source.

10. The method of use according to claim 9, wherein the near-infrared light source is a light source with a wavelength in the range of 780nm-2000nm.

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