A single end-capped silicone oil for heat conductive filler treatment and a method for preparing the same

Abstract

The application discloses a single-end capped silicone oil for heat-conducting filler treatment and a preparation method thereof. The silicone oil has a C1-C4 hydrocarbon group at one end and a methoxy group, an ethoxy group or other alkoxy group at the other end. After mixing hexamethylcyclotrisiloxane, organic lithium, silane, a molecular weight regulator and an initiation promoter, the mixture is subjected to reaction, then an end-capping agent and a catalyst are added to perform end-capping reaction, and then the solvent is removed to obtain the single-end capped silicone oil for heat-conducting filler treatment. The single-end capped silicone oil has a large molecular weight and excellent dispersing performance, can endow excellent dispersing performance on heat-conducting fillers such as alumina and magnesia, and can reduce the thixotropy value of the heat-conducting material.

Description

Technical Field

[0001] This invention relates to the field of materials technology for thermally conductive filler treatment agents, and specifically to a method and process for preparing single-end silicone oil for thermally conductive filler treatment. Background Technology

[0002] Due to significant differences in physicochemical properties, organic or organosilicon materials often exhibit poor compatibility with filler surfaces. Therefore, surface treatment of fillers becomes crucial to improve this compatibility.

[0003] Due to their excellent resistance to high and low temperatures, weather resistance, hydrophobicity, and low stress, silicone materials are widely used in the field of thermal conductive materials. Common silicone thermal conductive materials include thermally conductive adhesives, thermally conductive pads, thermally conductive grease, thermally conductive gels, and thermally conductive phase change materials.

[0004] As electronic components become increasingly integrated, the heat generated becomes more concentrated, necessitating improvements in heat dissipation performance. The thermal conductivity of a material depends on both the thermal conductivity of the filler itself and the amount of filler selected. Increasing the amount of filler can improve thermal conductivity, but it also increases viscosity, making the material difficult to apply. Furthermore, the poor compatibility of thermally conductive fillers with silicone can lead to poor dispersion in the silicone, causing filler sedimentation and reducing thermal conductivity. This can further result in poor contact between the thermally conductive material and the device or heat sink, increasing thermal resistance and ultimately reducing overall performance, including mechanical properties.

[0005] To address the aforementioned issues, a conventional approach is to treat the filler surface with a silane coupling agent to improve its compatibility with organosilicon. However, the degree of surface treatment for the filler is limited. When the amount of filler added increases, the thixotropic value of the thermally conductive material increases, making construction impossible and failing to obtain a thermally conductive material with high thermal conductivity. Summary of the Invention

[0006] Existing technologies use silane coupling agents to treat fillers to improve their compatibility with organosilicon, but this increases the thixotropic value of the thermally conductive material, failing to achieve high thermal conductivity. The single-end silicone oil described in this invention for treating thermally conductive fillers offers high operability; a lower dosage imparts excellent dispersion properties, allowing for higher filler addition levels without increasing the thixotropic value of the thermally conductive filler.

[0007] The present invention is achieved through the following technical solution.

[0008] A single-ended silicone oil for thermally conductive filler treatment has the chemical structure shown in Formula 1.

[0009]

[0010] Wherein, X is an alkane group, R is an alkoxy group, and n is a natural number; preferably, X is a substituted or unsubstituted C1-C4 alkane group, and R is a methoxy, ethoxy, or other alkoxy group; 10≤n≤300, more preferably 20≤n≤200, and even more preferably 20≤n≤120. The single-end silicone oil for thermally conductive filler treatment described in this invention has high operability, imparts excellent dispersion performance, requires low dosage and has a low thixotropic value, and has a long service life.

[0011] This invention discloses a method for preparing the above-mentioned single-ended silicone oil for thermally conductive filler treatment, comprising the following steps: mixing hexamethylcyclotrisiloxane with solvent, n-butyllithium, silane, molecular weight regulator and initiator and reacting them; then adding end-capping agent and catalyst to carry out end-capping reaction; and finally removing the solvent to obtain the single-ended silicone oil for thermally conductive filler treatment.

[0012] This invention discloses a method for surface treatment of fillers, comprising the following steps: mixing hexamethylcyclotrisiloxane with solvent, n-butyllithium, silane, molecular weight regulator, and initiator, and then reacting the mixture; adding an end-capping agent and a catalyst to perform an end-capping reaction; then removing the solvent to obtain a single-end capping silicone oil for thermally conductive filler treatment; and then using the single-end capping silicone oil for thermally conductive filler treatment to perform surface treatment on the filler.

[0013] In this invention, the solvent is any one of toluene, xylene, and n-heptane; the molecular weight regulator is trimethylsilanol; the initiator / promoter is any one or more of tetrahydrofuran, N,N-dimethylformamide, acetonitrile, dimethyl sulfoxide, and trimethylurea; the end-capping agent is methyl orthosilicate; the catalyst is one of formic acid, acetic acid, propionic acid, and citric acid; and the silane is trimethylchlorosilane.

[0014] Preferably, when hexamethylcyclotrisiloxane is mixed with n-butyllithium, the temperature is 30-40°C and the time is 10-20 min, then a molecular weight regulator is added, and the mixture is reacted at 10-80°C for 3-8 h.

[0015] Preferably, the mass ratio of solvent to hexamethylcyclotrisiloxane is 0.8–1.0, the mass ratio of n-butyllithium to hexamethylcyclotrisiloxane is 0.2%–1%, the mass ratio of molecular weight regulator to hexamethylcyclotrisiloxane is 0.004–0.12, the mass ratio of initiator to hexamethylcyclotrisiloxane is 0.2–0.5, the mass ratio of end-capping agent to hexamethylcyclotrisiloxane is 0.5–1.0, the mass ratio of catalyst to hexamethylcyclotrisiloxane is 0.2%–1.2%, and the mass ratio of silane to hexamethylcyclotrisiloxane is 0.2%–0.5%.

[0016] This invention discloses the application of the above-mentioned single-end silicone oil used for thermally conductive filler treatment as a surface treatment agent.

[0017] This invention discloses the application of the above-mentioned single-end silicone oil for thermally conductive filler treatment in filler surface treatment.

[0018] This invention discloses the application of the above-mentioned single-end silicone oil for thermally conductive filler treatment in improving filler dispersibility and / or reducing filler thixotropic value.

[0019] When the single-ended silicone oil used for thermally conductive filler treatment is applied to surface treatment, the molecular weight distribution index of the single-ended silicone oil is 1.0-1.5, preferably 1.0-1.2.

[0020] Furthermore, the filler used in the above-mentioned single-end silicone oil surface treatment for thermally conductive filler treatment can be used in organosilicon material systems, such as in vinyl silicone oil systems.

[0021] Therefore, the present invention discloses a thermally conductive organosilicon material, comprising organosilicon raw materials and surface-treated thermally conductive fillers, wherein the surface-treated thermally conductive fillers are the single-end silicone oil surface-treated thermally conductive fillers used for thermally conductive filler treatment.

[0022] As an example, the present invention discloses a method for preparing the above-mentioned single-end silicone oil for thermally conductive filler treatment, comprising the following steps performed sequentially:

[0023] (1) Dissolve hexamethylcyclotrisiloxane (D3) in a solvent, wherein the solvent is any one of toluene, xylene, or n-heptane;

[0024] (2) At a material temperature of 30-40℃, add n-butyllithium as the initiator of the reaction, and react for 10-20 minutes after adding n-butyllithium;

[0025] (3) Add trimethylchlorosilane to the reaction system and react for 60 min;

[0026] (4) Add molecular weight regulator and promoter to the reaction system, and continue the reaction for 3-8 hours. The reaction temperature is 10-50℃, preferably 30-40℃.

[0027] (5) Remove low-boiling substances by vacuum distillation. The vacuum distillation conditions are -90 kPa to -100 kPa and 90-120℃.

[0028] (6) After the de-lowering reaction in step (5) is completed, add end-capping agent and catalyst to carry out end-capping reaction. The reaction time is 3-6 hours and the reaction temperature is 90-120℃.

[0029] (7) After the end-capping reaction in step (6) is completed, low-boiling substances other than silicone oil polymers are removed by vacuum distillation. The vacuum distillation conditions are pressure -90kPa to -100kPa and temperature 160-180℃.

[0030] (8) Filter to remove impurities and obtain a colorless and transparent product, namely the single-end silicone oil used for thermally conductive filler treatment.

[0031] This invention discloses the application of the above-mentioned single-end silicone oil used for thermally conductive filler treatment as a surface treatment.

[0032] This invention discloses the application of the above-mentioned single-end silicone oil for thermally conductive filler treatment in the surface treatment of fillers, especially thermally conductive fillers.

[0033] The beneficial effects of this invention include high reaction yield, with a reaction yield ≥95%.

[0034] The beneficial effects of this invention include uniform molecular weight distribution and narrow molecular weight distribution (PDI < 1.5).

[0035] The beneficial effects of this invention include the ability to customize silicone oils with different numbers of chain segments and different molecular weights (n) between 10 and 300, and the ability to prepare silicone oils with different chain segments according to different usage environments.

[0036] The beneficial effects of this invention include the ability to customize single-ended silicone oils with different functional groups for application in different types of thermally conductive filler treatment fields.

[0037] The advantages of this invention compared to traditional thermally conductive filler treatment agents lie in the fact that its structure and molecular weight can be directionally controlled according to different application environments. Utilizing the advantage of its structure—inert at one end and active at the other—it achieves directional bonding between the surface treatment material and the matrix material. Furthermore, the low molecular weight polysiloxane product can easily penetrate the matrix material, resulting in a more integrated bond between the repeated surface treatment filler and the matrix material. The single-end silicone oil described in this invention, used for thermally conductive filler treatment, imparts excellent dispersion performance at a relatively low dosage, allowing for higher filler addition levels to the thermally conductive material without increasing the thixotropic value of the thermally conductive filler. Attached Figure Description

[0038] Figure 1 The infrared spectrum of the product of Example 1 is shown.

[0039] Figure 2 The infrared spectrum of the product of Example 2 is shown.

[0040] Figure 3 The infrared spectrum of the product of Example 3 is shown.

[0041] Figure 4 The infrared spectrum of the product of Example 4 is shown. Detailed Implementation

[0042] This invention discloses a method for preparing a single-end silicone oil for thermally conductive filler treatment, specifically comprising the following steps:

[0043] (1) Dissolve hexamethylcyclotrisiloxane (D3) in a solvent, wherein the solvent is any one of toluene, xylene, or n-heptane;

[0044] (2) At a material temperature of 20-40℃, add n-butyllithium as the initiator of the reaction, and react for 10-20 minutes after adding n-butyllithium;

[0045] (3) Add trimethylchlorosilane to the reaction system and react for 60 min;

[0046] (4) Add molecular weight regulator and promoter to the reaction system, and continue the reaction for 3-8 hours. The reaction temperature is 10-50℃, preferably 20-40℃.

[0047] (5) Remove low-boiling substances by vacuum distillation. The vacuum distillation conditions are -90 kPa to -100 kPa and 90-120℃.

[0048] (6) After the de-lowering reaction in step (5) is completed, add end-capping agent and catalyst to carry out end-capping reaction. The reaction time is 3-6 hours and the reaction temperature is 90-130℃.

[0049] (7) After the end-capping reaction in step (6) is completed, low-boiling substances other than silicone oil polymers are removed by vacuum distillation. The vacuum distillation conditions are pressure -90kPa to -100kPa and temperature 160-180℃.

[0050] (8) Filter to remove impurities and obtain a colorless and transparent product, namely the single-end silicone oil used for thermally conductive filler treatment.

[0051] Furthermore, the initiator used in step (2) can be any one of organolithium such as methyllithium, n-butyllithium, or sec-butyllithium.

[0052] Furthermore, the initiator used in step (3) is any one or more of tetrahydrofuran, N,N-dimethylformamide, acetonitrile, dimethyl sulfoxide, and trimethylurea.

[0053] Furthermore, the molecular weight regulator used in step (4) is either trimethylsilanol or dimethylvinylsilanol.

[0054] Furthermore, in step (6), the capping agent is any one of tetramethoxysilane, vinyltrimethoxysilane, and tetraethoxysilane.

[0055] Furthermore, the catalyst in step (6) is any one of acetic acid, propionic acid, formic acid, and citric acid.

[0056] To make the technical principles, objectives, and advantages of this invention more easily understood, the invention will be further elaborated below with reference to examples. The example solutions of this invention are only for the purpose of explaining the invention and do not limit the technical solutions of this invention. The raw materials used are existing products, and the specific preparation operations and performance tests are all conventional techniques.

[0057] Example 1

[0058] According to the present invention, the target silicone oil product synthesized in Example 1 is described below with specific examples:

[0059]

[0060] The preparation method is as follows:

[0061] Step 1: Weigh 19 kg of hexamethylcyclotrisiloxane (D3) and 16 kg of toluene and add them to a conventional reaction vessel, then heat to 40°C;

[0062] Step 2: Add 470 mL of n-butyllithium (2.5 mol / L in hexane) to the reactor. After the material in the reactor reacts for 15 min, add 0.057 kg of trimethylchlorosilane to the reactor. After the material in the reactor reacts for 60 min, add a mixed solution of 0.67 kg of trimethylsilanol and 4 kg of N,N-dimethylformamide to the reactor. Keep N2 gas flowing into the reactor, set the oil temperature to 35℃, and start the reaction for 3 h. Step 3: Remove the solvent at 95-100℃ using a negative pressure of -0.1 MPa. Stop the reaction when no solvent is removed.

[0063] Step 4: Weigh 10.6 kg of methyl orthosilicate and 0.18 kg of anhydrous acetic acid, add them through the feeding port, and then carry out the end-capping reaction at 125℃ for 4 hours to complete the reaction;

[0064] Step 5: Remove the solvent at 155-160℃ using a negative pressure of -0.1Mpa until no more solvent is removed;

[0065] Step 6: Filter the product to obtain a colorless and transparent product.

[0066] The obtained product was characterized by gel permeation chromatography: number-average molecular weight was 2516, weight-average molecular weight was 3039, and molecular weight distribution coefficient was 1.208; viscosity (25℃) was 32 mm. 2 / s.

[0067] Figure 1 The infrared spectrum of the obtained product, 801 cm⁻¹ -1 The strong peak appearing at 1023 cm⁻¹ is the absorption peak of the stretching vibration of the Si-C bond. -1 The strong peak at 1261 cm⁻¹ is the absorption peak of the stretching vibration of Si-O-Si.-1 The peak appearing at 2963 cm⁻¹ is the absorption peak of the stretching vibration of Si-CH₃; -1 The peak appearing nearby is the stretching vibration of -CH3, 2844 cm⁻¹. -1 The weak absorption peak is the stretching vibration absorption peak of Si-OCH3.

[0068] Example 2

[0069] According to the present invention, the target silicone oil product synthesized in Example 2 is described below with specific examples:

[0070]

[0071] The preparation method is carried out in the same manner as in Example 1:

[0072] Step 1: Weigh 15 kg of hexamethylcyclotrisiloxane (D3) and 13 kg of toluene and add them to a conventional reaction vessel, then heat to 40°C;

[0073] Step 2: Add 350 mL of n-butyllithium (2.5 mol / L in hexane) to the reactor. After the material in the reactor has reacted for 15 min, add 0.07 kg of trimethylchlorosilane to the reactor. After the material in the reactor has reacted for 60 min, add a mixed solution of 0.29 kg of trimethylsilanol, 2.4 kg of N,N-dimethylformamide, and 1 kg of acetonitrile to the reactor. Keep N2 gas flowing into the reactor, set the oil temperature to 35℃, and start the reaction for 4 h.

[0074] Step 3: Remove the solvent at 95-100℃ using a negative pressure of -0.1Mpa until no more solvent is removed;

[0075] Step 4: Weigh 8.5 kg of methyl orthosilicate and 0.15 kg of anhydrous acetic acid, add them through the feeding port, and then carry out the end-capping reaction at 130℃ for 3 hours to complete the reaction;

[0076] Step 5: Remove the solvent at 155-160℃ using a negative pressure of -0.1Mpa until no more solvent is removed;

[0077] Step 6: Filter the product to obtain a colorless and transparent product.

[0078] The obtained product was characterized by gel permeation chromatography: number-average molecular weight was 3848, weight-average molecular weight was 4568, and molecular weight distribution coefficient was 1.187; viscosity (25℃) was 53 mm. 2 / s.

[0079] Figure 2 The infrared spectrum of the obtained product, 799 cm⁻¹ -1 The strong peak appearing at 1021 cm⁻¹ is the absorption peak of the stretching vibration of the Si-C bond. -1The strong peak at 1261 cm⁻¹ is the absorption peak of the stretching vibration of Si-O-Si. -1 The peak appearing at 2963 cm⁻¹ is the absorption peak of the stretching vibration of Si-CH₃; -1 The peak appearing nearby is the stretching vibration of -CH3, 2844 cm⁻¹. -1 The weak absorption peak is the stretching vibration absorption peak of Si-OCH3.

[0080] Example 3

[0081] According to the present invention, the target silicone oil product synthesized in Example 3 is described below with specific examples:

[0082]

[0083] The preparation method is carried out in the same manner as in Example 1:

[0084] Step 1: Weigh 20 kg of hexamethylcyclotrisiloxane (D3) and 18 kg of toluene and add them to a conventional reaction vessel, then heat to 40°C;

[0085] Step 2: Add 530 mL of n-butyllithium (2.5 mol / L in hexane) to the reactor. After the material in the reactor has reacted for 20 min, add 0.13 kg of trimethylchlorosilane to the reactor. After the material in the reactor has reacted for 60 min, add a mixed solution of 0.19 kg of trimethylsilanol, 2.5 kg of N,N-dimethylformamide, and 1 kg of acetonitrile to the reactor. Keep N2 gas flowing into the reactor, set the oil temperature to 35℃, and start the reaction for 5 h.

[0086] Step 3: Remove the solvent at 95-100℃ using a negative pressure of -0.1Mpa until no more solvent is removed;

[0087] Step 4: Weigh 12 kg of methyl orthosilicate and 0.18 kg of anhydrous acetic acid, add them through the feeding port, and then carry out the end-capping reaction at 120℃ for 6 hours to complete the reaction;

[0088] Step 5: Remove the solvent at 150-155℃ using a negative pressure of -0.1Mpa until no more solvent is removed;

[0089] Step 6: Filter the product to obtain a colorless and transparent product.

[0090] The obtained product was characterized by gel permeation chromatography: number-average molecular weight was 6512, weight-average molecular weight was 7769, and molecular weight distribution coefficient was 1.193; viscosity (25℃) was 85 mm. 2 / s.

[0091] Figure 3 The infrared spectrum of the obtained product, 799 cm⁻¹ -1The strong peak appearing at 1021 cm⁻¹ is the absorption peak of the stretching vibration of the Si-C bond. -1 The strong peak at 1260 cm⁻¹ is the absorption peak of the stretching vibration of Si-O-Si. -1 The peak appearing at 2963 cm⁻¹ is the absorption peak of the stretching vibration of Si-CH₃; -1 The peak appearing nearby is the stretching vibration of -CH3, 2845 cm⁻¹. -1 The weak absorption peak is the stretching vibration absorption peak of Si-OCH3.

[0092] Example 4

[0093] According to the present invention, the target silicone oil product synthesized in Example 4 is described below with specific examples:

[0094]

[0095] The preparation method is carried out in the same manner as in Example 1:

[0096] Step 1: Weigh 16 kg of hexamethylcyclotrisiloxane (D3) and 14 kg of toluene and add them to a conventional reaction vessel, then heat to 40°C;

[0097] Step 2: Add 280 mL of n-butyllithium (2.5 mol / L in hexane) to the reactor. After the material in the reactor reacts for 20 min, add 0.09 kg of trimethylchlorosilane to the reactor. After the material in the reactor reacts for 60 min, add a mixed solution of 0.13 kg of trimethylsilanol and 4 kg of N,N-dimethylformamide to the reactor. Keep N2 gas flowing into the reactor, set the oil temperature to 35℃, and start the reaction for 5 h. Step 3: Remove the solvent at 95-100℃ using a negative pressure of -0.1 MPa. Stop the reaction when no solvent is removed.

[0098] Step 4: Weigh 10 kg of methyl orthosilicate and 0.13 kg of anhydrous acetic acid, add them through the feeding port, and then carry out the end-capping reaction at 125℃ for 4 hours to complete the reaction.

[0099] Step 5: Remove the solvent at 150-155℃ using a negative pressure of -0.1Mpa until no more solvent is removed;

[0100] Step 6: Filter the product to obtain a colorless and transparent product.

[0101] The obtained product was characterized by gel permeation chromatography: number-average molecular weight was 8145, weight-average molecular weight was 9896, and molecular weight distribution coefficient was 1.215; viscosity (25℃) was 115 mm. 2 / s.

[0102] Figure 4 The infrared spectrum of the obtained product, 800 cm⁻¹ -1The strong peak appearing at 1023 cm⁻¹ is the absorption peak of the stretching vibration of the Si-C bond. -1 The strong peak at 1261 cm⁻¹ is the absorption peak of the stretching vibration of Si-O-Si. -1 The peak appearing at 2963 cm⁻¹ is the absorption peak of the stretching vibration of Si-CH₃; -1 The peak appearing nearby is the stretching vibration of -CH3, 2844 cm⁻¹. -1 The weak absorption peak is the stretching vibration absorption peak of Si-OCH3.

[0103] Application Example 5-11

[0104] Component 1: Vinyl silicone oil (model RH-Vi321D, viscosity 100 mPa·s, Ningbo Runhe High-Tech Materials Technology Co., Ltd.)

[0105] Component 2: Alumina (Model: TM-LA-T, Particle size: ≤2.8μm; Specific surface area: 4-7m²) 2 g -1 ).

[0106] Component 3: Single-ended silicone oil 3-1: Example 1;

[0107] Single-ended silicone oil 3-2: Example 2;

[0108] Single-ended silicone oil 3-3: Example 3;

[0109] Single-ended silicone oil 3-4: Example 4.

[0110] Component 4: Coupling agent 4-1: n-Octyltrimethoxysilane (GC content ≥99%, Jiangxi Chenguang New Materials Co., Ltd.);

[0111] Coupling agent 4-2: γ-glycidyl etheroxypropyltrimethoxysilane (GC content ≥99%, Jiangxi Chenguang New Materials Co., Ltd.)

[0112] First, take vinyl silicone oil, alumina, and single-end silicone oil or coupling agent, add them to a 200ml stainless steel cup, stir in a disperser for 10 minutes, test the viscosity of the mixture and calculate the thixotropic value.

[0113] Viscosity test

[0114] Testing instruments: The viscosity of the material system was tested using a Bronispatial viscometer;

[0115] Test conditions: temperature 25±0.1℃, viscometer rotor No. 29, rotation speed 10r / min and 100r / min.

[0116] The formula for calculating thixotropic value is as follows:

[0117]

[0118] Table 1. Dispersion effects of different powder treatment agents in application examples.

[0119]

[0120]

[0121] As can be seen from Examples 5-11 in Table 1, the single-end silicone oil of the present invention, compared with coupling agents 4-1 and 4-2, can impart excellent dispersibility to the thermally conductive filler, and can impart a higher filler addition amount to the thermally conductive material without increasing the thixotropic value of the thermally conductive material. Furthermore, it can be seen that the single-end silicone oil treatment agent with a smaller molecular weight can make the thermally conductive material have lower viscosity and a lower thixotropic value, resulting in good fluidity even in thermally conductive materials with a high filler addition ratio.

[0122] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for surface treatment of fillers, characterized in that, The surface of the filler is treated using a single-end silicone oil for treating thermally conductive fillers; the preparation method of the single-end silicone oil for treating thermally conductive fillers is as follows: Step 1: Weigh 19 kg of hexamethylcyclotrisiloxane (D3) and 16 kg of toluene and add them to a conventional reaction vessel, then heat to 40°C; Step 2: Add 470 mL of a 2.5 mol / L n-butyllithium solution in hexane to the reactor. After the material in the reactor has reacted for 15 min, add 0.057 kg of trimethylchlorosilane to the reactor. After the material in the reactor has reacted for 60 min, add a mixed solution of 0.67 kg of trimethylsilanol and 4 kg of N,N-dimethylformamide to the reactor. Keep N2 gas flowing into the reactor, set the oil temperature to 35℃, and start the reaction for 3 h. Step 3: Remove the solvent at 95-100℃ using a negative pressure of -0.1Mpa until no more solvent is removed; Step 4: Weigh 10.6 kg of methyl orthosilicate and 0.18 kg of anhydrous acetic acid, add them through the feeding port, and then carry out the end-capping reaction at 125℃ for 4 hours to complete the reaction; Step 5: Remove the solvent at 155-160℃ using a negative pressure of -0.1Mpa until no more solvent is removed; Step 6: Filter the product to obtain a colorless and transparent product; The filler is alumina.

2. A thermally conductive silicone material, comprising vinyl silicone oil and surface-treated thermally conductive filler, characterized in that, The surface-treated thermally conductive filler is the single-end silicone oil surface-treated thermally conductive filler as described in claim 1.

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