CN113462165B - Heat-conducting organic silicon pouring sealant for inverter inductor and preparation method thereof - Google Patents
Heat-conducting organic silicon pouring sealant for inverter inductor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a heat-conducting organic silicon pouring sealant for an inverter inductor and a preparation method thereof, wherein the heat-conducting organic silicon pouring sealant is formed by mixing a component A and a component B according to the mass ratio of 1:1, and the component A consists of a base adhesive, low-volatility ultralow-hydroxyl-terminated vinyl polysiloxane, a platinum catalyst and an inhibitor; the component B consists of base glue, low-volatility ultralow-hydroxyl vinyl-terminated polysiloxane, a low-volatility crosslinking agent, a low-volatility chain extender and pigment; the base adhesive is prepared from low-volatility ultralow-hydroxyl vinyl-terminated polysiloxane, a heat conduction material, an environment-friendly flame retardant and a silane coupling agent. The heat-conducting organic silicon pouring sealant is low-viscosity low-volatility addition type liquid silicon rubber, has good fluidity and excellent heat-conducting property, and the inductance device of the poured inverter has good heat dissipation, is high-temperature resistant and free of aging and cracking for a long time, has low system temperature rise and small temperature difference, has no influence on the electrical property of each component in the inverter after long-term high-temperature use, can ensure the stable operation of the inverter, and prolongs the service life of the inverter.
Description
Technical Field
The invention belongs to the field of electronic potting materials, and particularly relates to a heat-conducting organic silicon potting adhesive for an inverter inductor and a preparation method of the heat-conducting organic silicon potting adhesive.
Background
In recent years, with the increasing demand for clean energy in China, the photovoltaic industry receives more and more attention. On a global scale, photovoltaic has become one of the most popular renewable energy sources, with great market potential. The photovoltaic inverter is developed rapidly, the inductor is used as one of key devices in the photovoltaic inverter, and the reliability of the inverter is directly influenced by the type selection and the installation heat dissipation process of the inductor. Inductors with large heat productivity are installed on various inverters in the existing market, and the ambient temperature of the inductors is generally high. These inductors are damaged or have low inductance efficiency and high noise when being in a high temperature state for a long time, so that a heat-conducting silicon rubber material is generally selected for encapsulation and heat dissipation, the temperature of the inductor is reduced, and the reduction of aging cracking capacity when the temperature rises is reduced. Along with the improvement of the inductive power, the requirements of higher heat conduction, temperature resistance and the like are put forward for the heat conduction pouring sealant, and the operation reliability and the service life are further improved.
The heat-conducting pouring sealant has the characteristics of low viscosity, higher heat conductivity, low temperature rise, small temperature difference, long-term resistance to 150 ℃ high-temperature change, no interference to other electronic devices and the like. Patent CN104292843B discloses a preparation method of a bi-component addition type organosilicon heat-conducting pouring sealant, which improves the storage stability of the pouring sealant for sedimentation hardening and high-proportion heat-conducting filler by combining a nano-scale additive and hydroxyl-containing organopolysiloxane and performing high-temperature treatment. The patent CN106833510A discloses a new-energy high-heat-conduction low-specific-gravity organic silicon pouring sealant, and the heat conductivity of the new-energy high-heat-conduction low-specific-gravity organic silicon pouring sealant is more than or equal to 0.95W/m.K through selection and surface modification of a low-specific-gravity heat-conduction filler; the specific gravity is less than or equal to 1.6g/ml. The patent CN109439272A discloses a two-component heat-conducting flame-retardant organic silicon pouring sealant composition for an electric automobile, a pouring sealant and a preparation method thereof, wherein the heat conductivity coefficient of the pouring sealant composition is improved by using a composite heat-conducting filler, the flame retardant property of the pouring sealant composition is improved by using aluminum hydroxide, and the pouring sealant composition is good in fluidity and moderate in elasticity, and is particularly suitable for the packaging requirements of a battery pack of the electric automobile. Patent CN111808571A discloses a high-thermal-conductivity organic silicon pouring sealant for photovoltaic invertersThe material has the advantages of high thermal conductivity (more than or equal to 1.5W/mK), low linear expansion coefficient (less than 200 mu m/(m. DEG C)), good aging resistance and no cracking with an aluminum shell after high temperature; however, the influence of the heat-conducting pouring sealant on the temperature rise and the temperature difference of an inverter system and the influence of the low-molecular polysiloxane ring body on the performance of an electronic device are not involved, and the requirement on the polymer raw material for realizing the low ring body content of the heat-conducting organic silicon pouring sealant is very strict. Patent CN112280039A discloses a preparation method of ultra-low viscosity vinyl silicone oil. The method adopts dimethyl siloxane mixed ring body to react with tetramethyl divinyl disiloxane under the action of an acid catalyst, and then alkali or alkali salt is selected to neutralize the acid catalyst to obtain the ultra-low viscosity vinyl silicone oil, wherein the viscosity of the ultra-low viscosity vinyl silicone oil is lower than 50mm 2 S, up to 20mm below 2 But the volatile component is higher than 3.55-8.15%, and the preparation of the vinyl silicone oil in the patent does not relate to a small amount of hydroxyl silicone oil in a silicone oil system and the influence thereof. A small amount of hydroxyl silicone oil in the vinyl silicone oil system can affect the workability of the pouring sealant and the heat resistance after curing. Generally speaking, as the power of the inverter inductor device increases, higher heat dissipation requirements are provided for the heat-conducting pouring sealant, particularly, the temperature rise and temperature difference change after aging resistance are small, and a severe challenge is provided for the performance stability of the heat-conducting pouring sealant after aging. Meanwhile, after the inverter operates for a period of time, the electrical performance of small electronic module devices in the system can be failed occasionally, and the low-molecular polysiloxane ring bodies contained in the silica gel can be influenced to a certain extent to reach a certain concentration, electromagnetic field effect and the like through multi-part demonstration.
Disclosure of Invention
Aiming at the defects in the prior art and the high requirement of an inverter inductance device, the invention aims to provide the heat-conducting organic silicon pouring sealant for the inverter inductance device and the preparation method thereof, the heat-conducting organic silicon pouring sealant has good fluidity and excellent heat-conducting property, the poured inverter inductance device has good heat dissipation, is high-temperature resistant for a long time and free from aging and cracking, the system temperature rise reaches the standard (the temperature of a high-power inverter device needs to be lower than 120 ℃), the temperature difference in the device is controlled within 5 ℃, and the operation stability of an inverter can be ensured.
In order to achieve the technical effect, the invention adopts the following technical scheme:
a heat-conducting organic silicon pouring sealant for an inverter inductance device comprises a component A and a component B which are used in a mixed mode;
the component A consists of the following materials in parts by weight:
220-720 parts of base rubber;
50 parts of vinyl-terminated polysiloxane;
0.1-0.8 parts of platinum catalyst;
0.01 to 0.3 portion of inhibitor;
the component B comprises the following materials in parts by weight:
220-720 parts of base rubber;
30 parts of vinyl-terminated polysiloxane;
3-9 parts of low-volatility crosslinking agent;
1-20 parts of low-volatility chain extender;
0.5 to 1.5 portions of pigment;
the base rubber in the A, B component is prepared from the following materials in parts by weight:
50 parts of vinyl-terminated polysiloxane;
165-650 parts of heat conduction material;
5-25 parts of an environment-friendly flame retardant;
0.2 to 1.5 portions of silane coupling agent.
The further technical scheme is that the vinyl-terminated polysiloxane is self-made low-volatility ultralow-hydroxyl vinyl-terminated polymethylvinylsiloxane (self-made vinyl-terminated polymethylvinylsiloxane for short), the viscosity of the vinyl-terminated polysiloxane is 100-1000 mPa & s, and the volatile component is less than or equal to 0.3%. Preferably, the viscosity is 100 to 550 mPas.
The further technical proposal is that the low-volatility crosslinking agent is refined side chain hydrogen-containing silicone oil, the viscosity of the low-volatility crosslinking agent is 40-90mPa.s, the hydrogen content is 0.10-0.75%, and the volatile component is less than or equal to 0.5%. Preferably, the viscosity is 45-80mPa.s, the hydrogen content is 0.15-0.50%, and the volatile content is less than or equal to 0.5%.
The further technical scheme is that the low-volatility chain extender is refined hydrogen-terminated silicone oil, the viscosity of the low-volatility chain extender is 20-80mPa.s, the hydrogen content of the low-volatility chain extender is 0.03-0.25%, and the volatile component of the low-volatility chain extender is less than or equal to 0.5%. Preferably, the viscosity is 35 to 65mPa.s, the hydrogen content is 0.05 to 0.18 percent, and the volatile component is less than or equal to 0.5 percent. The end hydrogen-containing silicone oil is used, the low-viscosity vinyl polysiloxane realizes chain growth under the action of a platinum catalyst, and the flexibility of the colloid is better after crosslinking and curing.
The further technical scheme is that the heat conducting material is one or more of spherical alumina, silicon micropowder, zinc oxide, magnesium oxide and aluminum nitride, and the particle size of the heat conducting material is 0.5-70 mu m. Preferably, the particle size of the heat conduction material is 1-70 μm, and a plurality of heat conduction materials such as spherical alumina, spherical alumina and zinc oxide are compounded for use, so that a more effective heat conduction path can be formed.
The further technical proposal is that the environment-friendly flame retardant is at least one or more of aluminum hydroxide, magnesium hydroxide and zinc borate, and the particle size of the environment-friendly flame retardant is 1-15 μm. Preferably, the environment-friendly flame retardant is prepared by aluminum hydroxide and zinc borate according to the mass ratio of 9:1, and the particle size of the environment-friendly flame retardant is 2-10 mu m.
The further technical proposal is that the silane coupling agent is one or more of hexamethyldisilazane, hexadecyl trimethoxy silane, vinyl tri (2-methoxyethoxy) silane and vinyl triethoxy silane. Preferably, the silane coupling agent is hexamethyldisilazane and hexadecyl trimethoxy silane which are compounded according to the mass ratio of 7:3 for use.
The further technical proposal is that the inhibitor is at least one of tetramethyltetravinylcyclotetrasiloxane, methylbutynol and ethynyl cyclohexanol. Preferably, the inhibitor is one of tetramethyltetravinylcyclotetrasiloxane and methylbutinol, wherein tetramethyltetravinylcyclotetrasiloxane is the inhibitor A, and methylbutinol is the inhibitor B. In the invention, the inhibitor is used for controlling the reaction speed of the heat-conducting organic silicon potting adhesive during curing, so that the heat-conducting organic silicon potting adhesive keeps good fluidity before curing, and can well fill the gap in the inverter inductor.
The further technical proposal is that the catalyst is a platinum (0) -divinyl tetramethyl disiloxane complex, and the platinum content is 500-5000 ppm. Preferably, the platinum content is 1500 to 5000ppm.
The invention also provides a preparation method of the heat-conducting organic silicon pouring sealant for the inverter inductor, which comprises the following steps:
(1) Synthesis of Low-volatility ultralow-hydroxyl-terminated vinyl polymethylvinylsiloxane
Adding a vinyl double-end socket, tetramethyl tetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane subjected to fractionation treatment, cation exchange resin subjected to self-purification treatment and a reusable water removal agent into a reaction kettle, balancing for 5-8 hours at 60-80 ℃ under the protection of nitrogen, filtering to obtain filtrate, heating to 165-180 ℃, reducing the pressure to-0.10 Mpa by using a reciprocating Roots vacuum unit device, removing low-boiling-point substances for 3-4 hours, and obtaining self-made low-volatility ultralow-hydroxyl-content vinyl-terminated polymethylvinylsiloxane (called self-made terminal vinyl polymethylvinylsiloxane for short);
(2) Synthesizing refined side chain hydrogen-containing silicone oil and refined end hydrogen-containing silicone oil
Adding tetramethylcyclotetrasiloxane, hexamethyldisiloxane and octamethylcyclotetrasiloxane subjected to fractionation treatment into a reaction kettle, uniformly stirring, slowly dropwise adding a strong acid catalyst into a reaction bottle, carrying out equilibrium reaction at 45-55 ℃ under the protection of nitrogen for 3-4 hours, then adding sodium bicarbonate for neutralization, filtering, heating the filtrate to 140-155 ℃, reducing the pressure to-0.10 Mpa by using a reciprocating Roots vacuum unit device, and removing low-boiling-point substances for 3-5 hours to obtain refined side-chain hydrogen-containing silicone oil;
adding tetramethyldihydro disiloxane and octamethylcyclotetrasiloxane subjected to fractionation treatment into a reaction kettle, uniformly stirring, slowly dropwise adding a strong acid catalyst into a reaction bottle, carrying out equilibrium reaction at 45-55 ℃ under the protection of nitrogen for 3-4 hours, adding sodium bicarbonate for neutralization, filtering, heating filtrate to 140-155 ℃, reducing the pressure to-0.10 Mpa by using a reciprocating Roots vacuum unit device, and removing low-boiling-point substances for 3-5 hours to obtain refined hydrogen-containing silicone oil at the end;
(3) Preparation of the base rubber
Preparing raw materials according to the proportion, kneading the self-made vinyl-terminated polymethylvinylsiloxane, the heat conduction material, the environment-friendly flame retardant and the silane coupling agent at the temperature of 80-90 ℃ for 1-1.5 h under normal pressure, and then evacuating and kneading at the temperature of 140-150 ℃ for 2-2.5 h for later use;
(4) Preparation of A-component and B-component
Preparation of component A: adding the self-made terminal vinyl polymethylvinylsiloxane into high-temperature base glue at the temperature of 140-150 ℃, evacuating and kneading for 1-1.5 h, transferring into a high-speed dispersion machine for cooling and stirring for 40-60 min, cooling to below 50 ℃, adding a platinum catalyst and an inhibitor, fully stirring for 1-1.5 h, and vacuumizing for 5-10 min to obtain a component A;
preparation of the component B: adding the self-made terminal vinyl polymethylvinylsiloxane into high-temperature base glue at the temperature of 140-150 ℃, evacuating and kneading for 1-1.5 h, transferring the mixture into a high-speed dispersion machine for cooling and stirring for 40-60 min, cooling to below 50 ℃, adding the low-volatility crosslinking agent, the low-volatility chain extender and the pigment, fully stirring for 1.5-2 h, and vacuumizing for 5-10 min to obtain a component B;
and mixing the component A and the component B to obtain the heat-conducting organic silicon pouring sealant.
The self-purification treatment of the cation exchange resin can enhance the catalytic efficiency. The reusable water removal agent can be reused after being used and treated at high temperature.
Preferably, the component A and the component B are mixed according to the mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant.
The further technical scheme is that the strong acid catalyst is concentrated sulfuric acid.
Compared with the prior art, the invention has at least the following beneficial effects:
the heat-conducting organic silicon pouring sealant for the inverter inductance device is low-viscosity heat-conducting flame-retardant addition type organic silicon liquid silicone rubber, self-made vinyl-terminated polymethylvinylsiloxane, refined side chain hydrogen-containing silicone oil and refined end hydrogen-containing silicone oil are matched with a heat-conducting material and an environment-friendly flame retardant to prepare the low-viscosity heat-conducting flame-retardant heat-conducting organic silicon pouring sealant, the heat-conducting coefficient is 0.8-2.1W/(m.K), and the flame retardance reaches V-0. The inverter inductor device filled with the heat-conducting pouring sealant has good heat dissipation, and after the inverter inductor device is aged at the high temperature of 150 ℃, the temperature rise of a system is low, the temperature difference is small, the electrical performance of each component in the system is not influenced, and the inverter runs stably.
The heat-conducting organic silicon pouring sealant has good fluidity and excellent heat-conducting flame-retardant performance, can be used for heat management assistance of various inverter inductance devices, controllers, electric tool power supplies and the like, assists stable operation of various electronic devices, has excellent high and low temperature resistance, and protects the overall safety of the devices.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
By adjusting the viscosity of the self-made vinyl-terminated polymethylvinylsiloxane, the using amounts of the heat conduction material and the environment-friendly flame retardant and the using amounts of the low-volatility crosslinking agent and the low-volatility chain extender containing different hydrogen, the heat conduction organic silicon pouring sealant with different comprehensive properties such as low viscosity, higher heat conduction, excellent flame retardance and the like can be obtained.
The specific test method is as follows:
viscosity, mixing viscosity: testing was carried out according to the method specified in GB/T2794 using No. 5 rotor 40 rpm;
tensile strength: testing according to a method specified in GB/T528;
hardness: testing according to the method specified in GB/T531.1;
coefficient of thermal conductivity: testing according to the method specified in ISO 22007-2;
flame retardant rating: adopting a vertical combustion test method in a method specified in GB/T2408 for a flame-retardant strip with the thickness of 3.0mm of a sample piece;
content of low-molecular polysiloxane ring bodies (D3-D10): extracting with solvent, and analyzing and detecting by GC-MS;
the heat conductivity coefficient after aging at 150 ℃ for 1500h is as follows: testing the heat-conducting sample block of the heat-conducting organic silicon pouring sealant according to a method specified by ISO 22007-2 after aging at the high temperature of 150 ℃ for 1500 h;
the inductance device of the glue-pouring inverter can resist the state, temperature rise and temperature difference change before and after aging for 1500h at the high temperature of 150 ℃: arranging a temperature sensing probe at an inductance magnetic core in an inverter inductance device, curing the cured potting adhesive for 7 days, then carrying out a 150 ℃ high-temperature aging test for 1500h, observing whether the potting adhesive cracks or not after the test is finished, and testing the inductance of the inverter to investigate the change of temperature rise and temperature difference in a system.
Self-made low-volatility ultralow-hydroxyl-terminated vinyl polymethylvinylsiloxane
The method comprises the steps of adding metered vinyl double-end sockets (VI-MM), tetramethyl tetravinylcyclotetrasiloxane (D4 Vi), fractionated octamethylcyclotetrasiloxane (D4), self-purification treated cation exchange resin (GLDX-04) and reusable water removal agent (GC 9) into a glass reaction kettle provided with a stirrer, a reflux condenser tube and a temperature sensing device, balancing for 6 hours at 70 ℃ under the protection of nitrogen, filtering to obtain filtrate, heating to 170 ℃, reducing the pressure to-0.10 MPa by using a reciprocating Roots vacuum unit device, removing low-boiling-point substances for 3 hours, and obtaining the different properties of the low-volatility ultralow-hydroxyl terminal vinyl polymethylvinylsiloxane (called self-prepared terminal vinyl polymethylvinylsiloxane for short) with different properties, wherein the results are shown in Table 1.
The mass ratio of D4, VI-MM, D4Vi and GLDX-04 is preferably (94-98): (1-5): (0.5-2): (40 to 50). Preferably, the amount of the reusable water scavenger (GC 9) is 0.6-0.8% of the total mass.
TABLE 1 self-made vinyl-terminated polymethylvinylsiloxanes with different properties
The self-made vinyl terminated polymethylvinylsiloxanes have low volatiles (about 0.5 to 1.5% of commercially available volatiles) compared to commercially available vinyl terminated polysiloxanes. The rapid test of a small amount of hydroxyl silicone oil is carried out by using butyl titanate (butyl titanate and terminal vinyl polysiloxane are mixed according to a proportion, a small amount of hydroxyl silicone oil exists in the system when the viscosity is increased, and almost no hydroxyl silicone oil exists in the system when the viscosity is not increased), the viscosity of the self-made terminal vinyl polymethylvinylsiloxane is almost not increased, the viscosity of the commercially available terminal vinyl silicone oil is obviously increased, and the result shows that almost no hydroxyl silicone oil exists in the self-made terminal vinyl polymethylvinylsiloxane, and the result is shown in table 2.
TABLE 2 results of rapid testing of small amounts of hydroxy silicone oil in terminal vinyl polysiloxanes
Refined side chain hydrogen-containing silicone oil
The method comprises the steps of filling a metered strong acid catalyst concentrated sulfuric acid into a constant pressure funnel, then adding metered tetramethylcyclotetrasiloxane (D4H), hexamethyldisiloxane (MM) and octamethylcyclotetrasiloxane (D4) subjected to fractionation into a four-mouth bottle provided with a stirrer, a reflux condenser tube, a constant pressure dropping funnel and a thermometer, stirring and mixing for 5 minutes at the speed of 150r/min, then slowly dropwise adding the strong acid catalyst from the constant pressure funnel, carrying out equilibrium reaction for 3.5 hours at the temperature of 50 ℃ under the protection of nitrogen, then adding a certain amount of sodium bicarbonate for neutralization for 45 minutes, filtering, heating the filtrate to the temperature of 150 ℃, removing low-boiling substances by using a reciprocating Roots vacuum unit device under reduced pressure for 4 hours, obtaining refined side chain hydrogen-containing silicone oil with different hydrogen contents, and the results are shown in Table 3.
Preferably, when the side chain hydrogen-containing silicone oil is purified, the mass ratio of D4, D4H, MM and the strong acid catalyst is (140-680): 60, (5-35): 2-10).
TABLE 3 refining of side chain hydrogen-containing silicone oils
Refined hydrogen-containing silicone oil
The method comprises the steps of filling a metered strong acid catalyst concentrated sulfuric acid into a constant-pressure funnel, then adding metered tetramethyl dihydro disiloxane (HMM) and fractionated octamethylcyclotetrasiloxane (D4) into a four-mouth bottle provided with a stirrer, a reflux condenser tube, a constant-pressure dropping funnel and a thermometer, stirring and mixing for 5 minutes at a speed of 150r/min, then slowly dripping the strong acid catalyst from the constant-pressure funnel, carrying out equilibrium reaction for 3.5 hours at 50 ℃ under the protection of nitrogen, then adding a certain amount of sodium bicarbonate for neutralization for 45 minutes, filtering, heating the filtrate to 150 ℃, removing low-boiling substances by using a reciprocating Roots vacuum unit device under reduced pressure for 4 hours, and obtaining refined end hydrogen-containing silicone oil with different contents, wherein the results are shown in Table 4.
Preferably, when the hydrogen-containing silicone oil at the end of purification is used, the mass ratio of D4, HMM and the strong acid catalyst is (55-75): 2-8): 1.
TABLE 4 refined end Hydrogen-containing Silicone oils
The prepared refined side chain hydrogen-containing silicone oil or refined end hydrogen-containing silicone oil with different hydrogen contents has lower volatile content than that of the commercially available side chain hydrogen-containing silicone oil (volatile content is about 0.5-3%) or end hydrogen-containing silicone oil (volatile content is about 0.5-5%), and the additive type silicone pouring sealant is used for performance test.
The heat conduction material A is prepared by mixing 5 mu m spherical alumina, 20 mu m spherical alumina and zinc oxide according to a mass ratio of 6; the heat conduction material B is prepared by mixing 5-micron spherical alumina, 40-micron spherical alumina, 70-micron spherical alumina and zinc oxide according to a mass ratio of 4.8.
The environment-friendly flame retardant C is prepared by matching 7 mu m of aluminum hydroxide and zinc borate according to the mass ratio of 9:1.
The silane coupling agent is prepared by compounding hexamethyldisilazane and hexadecyl trimethoxy silane according to the mass ratio of 7:3.
Tetramethyl tetravinylcyclotetrasiloxane is used as an inhibitor A, and methyl butynol is used as an inhibitor B.
Example 1
Based on parts by weight: 50 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-300D), 165 parts of heat conduction material A, 25 parts of environment-friendly flame retardant C and 0.5 part of silane coupling agent are kneaded at 85 ℃ under normal pressure for 1 hour, and then the mixture is used after being pumped out at 150 ℃ and kneaded for 2 hours.
Preparation of component A: adding 50 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-500D) into 240 parts of base rubber at the high temperature of 150 ℃, vacuumizing and kneading for 1h, transferring into a high-speed dispersion machine for cooling and stirring for 45min, cooling to 45 ℃, adding 0.5 part of platinum catalyst with the concentration of 2000ppm and 0.1 part of inhibitor B, fully stirring for 1.5h, vacuumizing for 10min, and preparing the component A rubber material.
Preparation of the component B: adding 30 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-500D) into 240 parts of base rubber at the high temperature of 150 ℃, vacuumizing and kneading for 1h, transferring the mixture into a high-speed dispersion machine for cooling and stirring for 45min to 45 ℃, then adding 7 parts of low-volatility crosslinking agent (GH-50L), 3 parts of low-volatility chain extender (DGH-005) and 0.6 part of black pigment, fully stirring for 1.5h, vacuumizing for 10min, and preparing the B component rubber material.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Example 2
Based on parts by weight: 50 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-300D), 225 parts of heat conducting material A, 15 parts of environment-friendly flame retardant C and 0.7 part of silane coupling agent are kneaded at the temperature of 85 ℃ and normal pressure for 1 hour, and then the mixture is used after being pumped out and kneaded at the temperature of 150 ℃ for 2 hours.
Preparation of component A: 50 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-300D) is added into 290 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1 hour, then transferred into a high-speed dispersion machine to be cooled and stirred for 45 minutes to 45 ℃, 0.6 part of platinum catalyst with the concentration of 2000ppm is added, 0.06 part of inhibitor A is added and stirred for 1.5 hours, pumped out for 10 minutes, and the preparation of the component A rubber material is finished.
Preparation of the component B: adding 30 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-300D) into 290 parts of base rubber at the high temperature of 150 ℃, evacuating, kneading for 1h, transferring to a high-speed dispersion machine for cooling and stirring for 45min, cooling to 45 ℃, adding 5 parts of low-volatility crosslinking agent (GH-50L), 6 parts of low-volatility chain extender (DGH-020) and 0.8 part of black pigment, fully stirring for 1.5h, evacuating for 10min, and preparing the component B rubber material.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Example 3
Based on parts by weight: 50 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-100D), 285 parts of heat conduction material A, 15 parts of environment-friendly flame retardant C and 0.75 part of silane coupling agent are kneaded at the temperature of 85 ℃ and normal pressure for 1.5 hours, and then the mixture is used after being pumped out and kneaded at the temperature of 150 ℃ for 2.5 hours.
Preparation of component A: 50 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-300D) is added into 350 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine to be cooled and stirred for 55min to 45 ℃, 0.3 part of platinum catalyst with the concentration of 5000ppm is added, 0.08 part of inhibitor A is added and stirred for 1.5h, pumped out for 10min, and the preparation of the component A rubber material is finished.
Preparation of the component B: adding 30 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-300D) into 350 parts of base rubber at the high temperature of 150 ℃, evacuating, kneading for 1.5h, transferring to a high-speed dispersion machine for cooling and stirring for 55min, cooling to 45 ℃, adding 8 parts of low-volatility crosslinking agent (GH-36L), 9 parts of low-volatility chain extender (DGH-010) and 1 part of pigment, fully stirring for 1.5h, evacuating for 10min, and completing the preparation of the component B rubber material.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Example 4
Based on parts by weight: 50 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-200D), 370 parts of heat conducting material A, 10 parts of environment-friendly flame retardant C and 0.9 part of silane coupling agent are kneaded at the temperature of 85 ℃ and normal pressure for 1.5 hours, and then the mixture is used after being pumped out and kneaded at the temperature of 150 ℃ for 2.5 hours.
Preparation of component A: 50 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-200D) is added into 430 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine to be cooled and stirred for 55min to 45 ℃, 0.6 part of platinum catalyst with the concentration of 3000ppm and 0.1 part of inhibitor B are added and stirred for 1.5h, pumped out for 10min, and the component A rubber material is prepared.
Preparation of the component B: 30 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-200D) is added into 430 parts of base rubber at the high temperature of 150 ℃, the mixture is pumped out and kneaded for 1.5h, then the mixture is transferred into a high-speed dispersion machine to be cooled and stirred for 55min to 45 ℃, 5.5 parts of low-volatility crosslinking agent (GH-36L), 12 parts of low-volatility chain extender (DGH-010) and 1.2 parts of black pigment are added and stirred for 1.5h, the mixture is pumped out for 10min, and the component B rubber material is prepared.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Example 5
Based on parts by weight: 50 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-100D), 450 parts of heat conduction material A, 5 parts of environment-friendly flame retardant C and 1.15 parts of silane coupling agent are kneaded at 85 ℃ under normal pressure for 1.5 hours, and then the mixture is used after being pumped out at 150 ℃ and kneaded for 2.5 hours.
Preparation of component A: adding 50 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-300D) into 505 parts of base rubber at the high temperature of 150 ℃, evacuating, kneading for 1.5h, transferring to a high-speed dispersion machine for cooling and stirring for 55min, cooling to 45 ℃, adding 0.8 part of platinum catalyst with the concentration of 3000ppm, adding 0.22 part of inhibitor A, fully stirring for 1.5h, evacuating for 10min, and preparing the component A rubber material.
Preparation of the component B: 30 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-500D) is added into 505 parts of base rubber at the high temperature of 150 ℃, the mixture is vacuumized and kneaded for 1.5h, then the mixture is transferred into a high-speed dispersion machine to be cooled and stirred for 55min to 45 ℃, 6 parts of low-volatility crosslinking agent (GH-15L + GH-36L), 16 parts of low-volatility chain extender (DGH-010) and 1.4 parts of pigment are added and fully stirred for 1.5h, and then the preparation is completed after the mixture is vacuumized for 10min and the component B rubber material is mixed.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Example 6
Based on parts by weight: 50 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-100D), 650 parts of heat conduction material B, 5 parts of environment-friendly flame retardant C and 1.15 parts of silane coupling agent are kneaded at the temperature of 85 ℃ and normal pressure for 1.5 hours, and then the mixture is used after being pumped out and kneaded at the temperature of 150 ℃ for 2.5 hours.
Preparation of the component A: 50 parts of self-made terminal vinyl polymethylvinylsiloxane (ViL-100D) is added into 705 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine to be cooled and stirred for 55min to 45 ℃, 0.75 part of platinum catalyst with the concentration of 5000ppm is added, 0.28 part of inhibitor A is added and stirred for 1.5h, pumped out for 10min, and the preparation of the component A rubber material is finished.
Preparation of the component B: 30 parts of self-made vinyl-terminated polymethylvinylsiloxane (ViL-200D) is added into 705 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine to be cooled and stirred for 55min to 45 ℃, 8 parts of low-volatility crosslinking agent (GH-15L + GH-36L), 16 parts of low-volatility chain extender (DGH-010) and 1.5 parts of black pigment are added and fully stirred for 1.5h, pumped out for 10min and component B is used as sizing material to complete the preparation.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Comparative example 1
Based on parts by weight: 50 parts of vinyl-terminated polysiloxane (Vi-100 cs sold in the market), 285 parts of heat conduction material A, 15 parts of environment-friendly flame retardant C and 0.75 part of silane coupling agent are kneaded at 85 ℃ under normal pressure for 1.5 hours, and then are pumped out at 150 ℃ and kneaded for 2.5 hours for use.
Preparation of component A: 50 parts of terminal vinyl polysiloxane (commercially available Vi-300 cs) is added into 350 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine for cooling and stirring for 55min and cooled to 45 ℃, 0.3 part of platinum catalyst with the concentration of 5000ppm is added, 0.08 part of inhibitor A is added and stirred for 1.5h, pumped out for 10min, and the preparation of the component A rubber material is finished.
Preparation of the component B: adding 30 parts of vinyl-terminated polysiloxane (Vi-300 cs sold in the market) into 350 parts of base rubber at the high temperature of 150 ℃, evacuating, kneading for 1.5h, transferring into a high-speed dispersion machine for cooling and stirring for 55min, cooling to 45 ℃, adding 8 parts of low-volatility crosslinking agent (GH-36L), 9 parts of low-volatility chain extender (DGH-010) and 1 part of black pigment, fully stirring for 1.5h, evacuating for 10min, and finishing the preparation of the component B rubber material.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Comparative example 2
Based on parts by weight: 50 parts of vinyl-terminated polysiloxane (Vi-100 cs sold in the market) and 285 parts of heat conducting material A, 15 parts of environment-friendly flame retardant C are kneaded at the high temperature of 85 ℃ and the normal pressure for 1.5h, and then the mixture is pumped out at the high temperature of 150 ℃ and kneaded for 2.5h for use.
Preparation of component A: 50 parts of terminal vinyl polysiloxane (commercially available Vi-300 cs) is added into 350 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine for cooling and stirring for 55min and cooled to 45 ℃, 0.3 part of platinum catalyst with the concentration of 5000ppm is added, 0.08 part of inhibitor A is added and stirred for 1.5h, pumped out for 10min, and the preparation of the component A rubber material is finished.
Preparation of the component B: 30 parts of end vinyl polysiloxane (commercially available Vi-300 cs) is added into 350 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5H, then transferred into a high-speed dispersion machine to be cooled and stirred for 55min to be cooled to 45 ℃, 8 parts of cross-linking agent (commercially available hydrogen-containing silicone oil H0.36%), 9 parts of chain extender (commercially available end hydrogen-containing silicone oil H0.1%) and 1 part of black pigment are added and stirred for 1.5H, pumped out for 10min, and the preparation of the component B sizing material is completed.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
Comparative example 3
Based on parts by weight: 50 parts of vinyl-terminated polysiloxane (Vi-100 cs sold in the market), 450 parts of heat conducting material A, 5 parts of environment-friendly flame retardant C and 1.15 parts of silane coupling agent are kneaded at the temperature of 85 ℃ under normal pressure for 1.5h, and then the mixture is pumped out at the temperature of 150 ℃ and kneaded for 2.5h for use.
Preparation of component A: 50 parts of terminal vinyl polysiloxane (Vi-300 cs sold in the market) is added into 505 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5h, then transferred into a high-speed dispersion machine for cooling and stirring for 55min, cooled to 45 ℃, 0.8 part of platinum catalyst with the concentration of 3000ppm and 0.22 part of inhibitor A are added and fully stirred for 1.5h, pumped out for 10min, and the preparation of the component A rubber material is finished.
Preparation of the component B: 30 parts of terminal vinyl polysiloxane (Vi-500 cs sold in the market) is added into 505 parts of base rubber at the high temperature of 150 ℃, pumped out and kneaded for 1.5H, then transferred into a high-speed dispersion machine for cooling and stirring for 55min, cooled to 45 ℃,5 parts of cross-linking agent (hydrogen-containing silicone oil H0.36% sold in the market), 16 parts of chain extender (hydrogen-containing silicone oil H0.1% sold in the market) and 1.4 parts of black pigment are added and stirred fully for 1.5H, pumped out for 10min, and the rubber material of the component B is prepared.
And mixing the component A and the component B according to a mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant, pouring an inductor of the inverter, curing and maintaining for a certain time, and testing corresponding performance indexes. The test results are shown in Table 5.
TABLE 5 Properties of the examples and comparative examples
As can be seen from table 1, the silicone potting adhesives with different thermal conductivities, prepared by using the self-made vinyl terminated polymethylvinylsiloxane, the refined side chain hydrogen-containing silicone oil and the refined end hydrogen-containing silicone oil in the examples 1 to 6 in combination, have low viscosity, are very beneficial to gap potting of inverter inductance devices, can reduce the generation of bubbles, and have better heat dissipation performance. Compared with the comparative example 1, the comparative example 2 and the comparative example 5, the viscosity of the self-made vinyl terminated polymethylvinylsiloxane is obviously reduced, because the self-made vinyl terminated polymethylvinylsiloxane is controlled by raw material treatment, synthesis process and the like, and the generation of a small amount of hydroxyl silicone oil in the synthesis is avoided, so that the viscosity of the self-made vinyl terminated polymethylvinylsiloxane is obviously reduced. Compared with the comparative example 1 and the comparative example 2, the comparative example 2 has the defects of cracking, abnormal temperature rise and large temperature difference after temperature-resistant aging, which shows that the heat resistance of the refined side chain hydrogen-containing silicone oil and the refined end hydrogen-containing silicone oil is good, and the performance of the prepared heat-conducting organic silicon pouring sealant after aging is more stable. By synthesizing low-volatility polymer raw materials, the volatile components of the raw materials are reduced, so that the content of residual low-molecular polysiloxane ring bodies (D3-D10) in the glue is less than 150ppm, and is obviously reduced compared with the content of low-molecular polysiloxane ring bodies of commercially available raw materials, the inverter inductance device is favorable for stability in long-term thermal operation, and various performances of the inverter inductance device cannot be influenced.
Compared with the heat-conducting pouring sealant prepared from commercially available terminal vinyl polysiloxane and hydrogen-containing silicone oil, the heat-conducting organic silicon pouring sealant has excellent performance, can resist 150 ℃ and 1500h of aging of different inverter inductance devices after pouring, ensures that the temperature rise of an inverter system is in a control range, has the temperature difference within 5 ℃, and is more stable in operation. Therefore, the researched heat-conducting organic silicon pouring sealant for the inverter inductance device can better meet the heat dissipation requirements of each key device of the inverter, the reliability of the inverter is improved, and the service life of an electronic device is prolonged.
Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (5)
1. The preparation method of the heat-conducting organic silicon pouring sealant for the inverter inductance device is characterized by comprising the following steps of:
(1) Synthesis of Low-volatility ultralow-hydroxyl-terminated vinyl polymethylvinylsiloxane
Adding vinyl double end sockets, tetramethyl tetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane subjected to fractionation treatment, cation exchange resin GLDX-04 subjected to self-purification treatment and reusable water removal agent GC9 into a reaction kettle, balancing for 5-8 hours at 60-80 ℃ under the protection of nitrogen, filtering to obtain filtrate, heating to 165-180 ℃, reducing the pressure to-0.10 Mpa by using a reciprocating Roots vacuum unit device, removing low-boiling-point substances for 3-4 hours, and obtaining the self-made low-volatility ultralow-hydroxyl-group-terminated vinyl polymethylvinylsiloxane, wherein the viscosity of the self-made low-volatility ultralow-hydroxyl-group-terminated vinyl polymethylvinylsiloxane is 100-1000 mPas, and the volatile component of the self-made low-volatility ultralow-hydroxyl-group-terminated vinyl polymethylvinylsiloxane is less than or equal to 0.3%;
(2) Refined side chain hydrogen-containing silicone oil and refined end hydrogen-containing silicone oil
Adding tetramethylcyclotetrasiloxane, hexamethyldisiloxane and octamethylcyclotetrasiloxane subjected to fractionation treatment into a reaction kettle, uniformly stirring, slowly dropwise adding a strong acid catalyst, namely concentrated sulfuric acid into a reaction bottle, carrying out equilibrium reaction at 45-55 ℃ under the protection of nitrogen for 3-4 hours, then adding sodium bicarbonate for neutralization, filtering, heating the filtrate to 140-155 ℃, reducing the pressure to-0.10 Mpa by using a reciprocating Roots vacuum unit device, removing low-boiling substances for 3-5 hours, and obtaining refined side chain hydrogen-containing silicone oil with the viscosity of 40-90mPa.s, the hydrogen content of 0.10-0.75% and the volatile component of less than or equal to 0.5%;
adding tetramethyl dihydro disiloxane and octamethylcyclotetrasiloxane which are subjected to fractionation treatment into a reaction kettle, uniformly stirring, slowly dropwise adding a strong acid catalyst, namely concentrated sulfuric acid into a reaction bottle, carrying out equilibrium reaction at 45-55 ℃ under the protection of nitrogen for 3-4 hours, then adding sodium bicarbonate for neutralization, filtering, heating filtrate to 140-155 ℃, reducing the pressure to-0.10 Mpa by using a reciprocating Roots vacuum unit device, removing low-boiling-point substances for 3-5 hours, and obtaining refined end hydrogen-containing silicone oil with the viscosity of 20-80mPa.s, the hydrogen content of 0.03-0.25% and the volatile component of less than or equal to 0.5%;
(3) Preparation of the base rubber
Kneading 50 parts of the self-made low-volatility ultralow-hydroxyl-terminated vinyl polymethylvinylsiloxane, 165-650 parts of heat conduction material, 5-25 parts of environment-friendly flame retardant and 0.2-1.5 parts of silane coupling agent at 80-90 ℃ for 1-1.5 h under normal pressure, and then kneading for 2-2.5 h at high temperature of 140-150 ℃ in a vacuumizing manner for later use;
(4) Preparation of A-component and B-component
Preparation of the component A: adding 50 parts of the self-made low-volatility ultralow-hydroxyl-terminated vinyl polymethylvinylsiloxane into 220-720 parts of high-temperature base adhesive at 140-150 ℃, vacuumizing, kneading, transferring into a high-speed dispersion machine, cooling, stirring, adding 0.1-0.8 part of platinum catalyst and 0.01-0.3 part of inhibitor, fully stirring, and vacuumizing to obtain a component A;
preparation of the component B: adding 30 parts of the self-made low-volatility ultralow-hydroxyl-terminated vinyl polymethylvinylsiloxane into 220-720 parts of high-temperature base adhesive at 140-150 ℃, vacuumizing, kneading, transferring into a high-speed dispersion machine, cooling and stirring, adding 3-9 parts of refined side chain hydrogen-containing silicone oil, 1-20 parts of refined end hydrogen-containing silicone oil and 0.5-1.5 parts of pigment, fully stirring, and vacuumizing to obtain a component B;
and mixing the component A and the component B according to the mass ratio of 1:1 to obtain the heat-conducting organic silicon pouring sealant.
2. The preparation method of the heat-conducting silicone pouring sealant for the inverter inductor device according to claim 1, wherein the heat-conducting material is one or more of spherical alumina, silica micropowder, zinc oxide, magnesium oxide and aluminum nitride, and the particle size of the heat-conducting material is 0.5-70 μm.
3. The preparation method of the heat-conducting silicone pouring sealant for the inverter inductance device according to claim 1, wherein the environment-friendly flame retardant is at least one or more of aluminum hydroxide, magnesium hydroxide and zinc borate, and the particle size of the environment-friendly flame retardant is 1-15 μm.
4. The method for preparing the heat-conducting silicone pouring sealant for the inverter inductance device according to claim 1, wherein the silane coupling agent is one or more of hexamethyldisilazane, hexadecyl trimethoxy silane, vinyl tris (2-methoxyethoxy) silane, and vinyl triethoxy silane.
5. The method for preparing the heat-conducting silicone pouring sealant for the inverter inductance device according to claim 1, wherein the inhibitor is at least one of tetramethyltetravinylcyclotetrasiloxane, methylbutynol and ethynylcyclohexanol; the catalyst is a platinum (0) -divinyl tetramethyl disiloxane complex, and the platinum content is 500-5000 ppm.
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