CN111732932A - Organic silicon material and preparation method and application thereof - Google Patents
Organic silicon material and preparation method and application thereof Download PDFInfo
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Abstract
The invention is applicable to the technical field of materials, and provides an organic silicon material, a preparation method and application thereof, wherein the organic silicon material is prepared by adding modified nano silicon carbide into an organic silicon mixture; the modified nano silicon carbide is obtained by modifying nano silicon carbide with a silicon dioxide film coated on the surface by a coupling agent. The refractive index of the organic silicon material provided by the invention is close to that of a screen body and a curtain wall, so that the transparency of the material is ensured, and the heat conduction performance and the weather resistance of the material are improved, the organic silicon material is used for attaching the screen body and the curtain wall, the light transmittance of a cured bonding layer is more than 95%, the material does not turn yellow after being aged for 1000 hours under the conditions of 85% RH and 85 ℃, the material does not turn crack and yellow after being subjected to cold and hot impact for 1000 cycles at-40 ℃ to 80 ℃, the phenomenon of cracking, embrittlement and yellowing does not occur after a Qsun test for 500 hours, the LED junction temperature in the screen body can be reduced to 56-60 ℃ from the original 70 ℃, and the use requirements are met.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to an organic silicon material, and a preparation method and application thereof.
Background
The development of the LED display technology makes the outdoor lighting engineering become more and more diversified, and the nano screen, the diamond screen, the flexible screen, etc. are endlessly developed, but these various screens need to be combined to form an exquisite display pattern, which has higher requirements for quality and many factors to be considered.
Because of the particularity of the environment of the outdoor LED display screen, two kinds of glue, namely organic silicon potting glue and epoxy resin are generally used, the glue used by the outdoor LED display screen needs to have good heat dissipation performance, high temperature resistance, yellowing resistance and cracking resistance, so the outdoor LED screen generally mainly uses two-component organic silicon potting glue, and epoxy resin with poor weather resistance is rarely selected, however, the existing organic silicon potting glue cannot give consideration to the effects of heat dissipation and seamless bonding of a screen body when in use, can also influence the visual effect of a wall body when the wall body is overlooked from inside to outside to a certain extent, has limited weather resistance, and cannot bear severe weather such as long-term exposure to heat, rain, high altitude, low pressure, typhoon and the like.
Therefore, the problems that the existing organic silicon pouring sealant is poor in visual effect, limited in weather resistance and heat dissipation effect and incapable of meeting the use requirement exist.
Disclosure of Invention
The embodiment of the invention aims to provide an organic silicon material, and aims to solve the problems that the existing organic silicon pouring sealant is poor in visual effect, limited in weather resistance and heat dissipation and incapable of meeting the use requirement.
The embodiment of the invention is realized by that the organic silicon material is prepared by adding modified nano silicon carbide into an organic silicon mixture;
the modified nano silicon carbide is obtained by modifying nano silicon carbide with a silicon dioxide film coated on the surface by a coupling agent.
Another objective of an embodiment of the present invention is to provide a method for preparing the organic silicon material, including:
adding the modified nano silicon carbide into the organic silicon mixture according to the addition amount of 3-8% by weight, and performing planetary dispersing mixing and defoaming treatment to obtain the silicon carbide composite material.
Another object of the embodiments of the present invention is to provide an application of the silicone material in outdoor brightening screens.
According to the organic silicon material provided by the embodiment of the invention, the modified nano silicon carbide is added into the organic silicon mixture, and is obtained by modifying the nano silicon carbide with the surface coated with the silicon dioxide film by the coupling agent, on one hand, the silicon dioxide film and the organic silicon-based adhesive have excellent system compatibility, the light transmittance of an adhesive layer is not influenced, and the heat conductivity coefficient can be improved, meanwhile, the nano silicon carbide with the surface coated with the silicon dioxide film and modified by the coupling agent has excellent hydrophobicity, and the group carried on the surface coated with the silicon dioxide film participates in the reaction of the organic silicon-based adhesive system, so that the body crosslinking is realized by an interpenetrating network structure, the migration cannot occur in the subsequent use process, the transparency of the material is ensured, and the heat conductivity and the weather resistance of the material can also be improved; on the other hand, the refractive index of the organic silicon material is close to that of the screen body and the curtain wall, the organic silicon material is used for adhering the screen body and the curtain wall, the light transmittance of the solidified adhesive layer is larger than 95%, yellowing does not occur after aging for 1000 hours under the conditions of 85% RH and 85 ℃, cracking and yellowing do not occur after 1000 cycles of cold and hot impact at the temperature of-40-80 ℃, cracking, embrittlement and yellowing do not occur after 500 hours of Qsun test, and the LED junction temperature in the screen body can be reduced to 56-60 ℃ from the original 70 ℃.
Drawings
FIG. 1 is a morphology diagram of a modified nano-SiC provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and 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.
The embodiment of the invention aims to meet the following quality requirements in the current LED display technology: 1. seamless bonding of the screen body and the outdoor wall body is realized, and the visual effect of the wall body when the wall body is overlooked from inside to outside cannot be influenced; 2. the screen body is helped to dissipate heat, so that the service life of the LED light source is prolonged; 3. the bonding layer has excellent weather resistance and can bear severe weather such as hot sun, rain, plateau low pressure, typhoon and the like, and an organic silicon material is provided, wherein a modified nano silicon carbide is added into an organic silicon mixture, the modified nano silicon carbide is obtained by modifying nano silicon carbide with a silicon dioxide film coated on the surface through a coupling agent, the refractive index of the organic silicon material is close to that of a screen body and a curtain wall, the organic silicon material is used for bonding the screen body and the curtain wall, the light transmittance of the cured bonding layer is greater than 95%, the bonding layer does not have yellowing after aging for 1000 hours under the conditions of 85% RH and 85 ℃, the bonding layer does not have cracking and yellowing after 1000 cycles of cold and heat shock at the temperature of minus 40-80 ℃, and does not have cracking, embrittlement and yellowing phenomena after a Qsun test for 500 hours, and the LED in the screen body can be reduced to 56-60 ℃ from the original temperature of 70 ℃.
In the embodiment of the invention, the organic silicon material is prepared by adding modified nano silicon carbide into an organic silicon mixture; the modified nano silicon carbide is obtained by modifying nano silicon carbide with a silicon dioxide film coated on the surface by a coupling agent. Because the nano silicon carbide powder is coated, the system compatibility of the silicon dioxide outer membrane and the organic silicon-based adhesive is excellent, the light transmittance of the adhesive layer is not influenced, and the heat conductivity coefficient can be improved.
In the embodiment of the invention, the nano silicon carbide powder coated with the silicon dioxide film on the surface is purchased from combined fertilizer Zhonghang nanotechnology development Co.
In the embodiment of the present invention, the coupling agent is preferably a vinyl silane coupling agent, that is, any coupling agent as long as it is a vinyl group capable of achieving hydrophobic surface treatment, and more preferably one of tetramethyldivinyldisilazane, vinyltriisopropoxysilane, vinyltrimethoxysilane, vinyltri-t-butoxysilane, and vinyltri-t-butoxysilane.
In the embodiment of the invention, the nano silicon carbide with the surface coated with the silicon dioxide film treated by the vinyl silane coupling agent has excellent hydrophobicity, and the silicon dioxide layer coated with the surface also has vinyl which participates in the reaction of an organic silicon-based adhesive system, so that the body crosslinking is realized by an interpenetrating network structure, the migration is not generated in the subsequent use process, the transparency of the material is ensured, and the heat conductivity and the weather resistance of the material are improved.
In the embodiment of the invention, the modified silicon carbide accounts for 3-8% of the weight of the organic silicon mixture; the addition content of the modified silicon carbide has a direct influence on the performance of the organic silicon system, namely the addition amount of the modified silicon carbide is not less than 3%, when the use amount of the modified silicon carbide is too small, the function of forming a heat conduction network cannot be realized, the addition amount of the modified silicon carbide is not more than 8%, and when the addition content of the modified silicon carbide is excessive, the optical performance of the organic silicon system is directly influenced.
In the embodiment of the invention, the modified silicon carbide is obtained by introducing nano silicon carbide with a surface coated with a silicon dioxide film into a fluidized bed, adding a coupling agent, blowing compressed air as a carrier gas at a flow rate of 30-100 mL/min, and reacting for 3-5 h at the temperature of 150-180 ℃. The experimental research of the invention shows that the step process of the coupling agent modification, the reaction time, the reaction temperature, the flow rate of the carrier gas, the type of the carrier gas and the boiling effect of the fluidized bed all have certain influence on the modification effect of the silicon carbide, and directly influence the dispersion and interpenetrating network crosslinking effects of the modified silicon carbide in the using process, thereby influencing the optical and heat-conducting properties of the cured material.
Wherein the weight ratio of the nano silicon carbide coated with the silicon dioxide film on the surface to the coupling agent is 1: 0.02-0.05.
Wherein the compressed air is one of nitrogen and argon.
Wherein, the fluidized bed has one of partial boiling, convection boiling and wave boiling.
In a preferred embodiment of the present invention, the modified silicon carbide is obtained by introducing the nano silicon carbide coated with the silica film into a fluidized bed, adding a coupling agent, blowing compressed air as a carrier gas at a flow rate of 100mL/min, and reacting at a temperature of 170 ℃ for 5 hours.
In the embodiment of the invention, the organic silicon mixture can be organic silicon pouring sealant in the prior art, and can also be prepared by directly and uniformly mixing the following raw materials in parts by weight:
10-65 parts of vinyl silicone oil, 2-15 parts of hydrogen-containing silicone oil, 5-15 parts of long-chain alkyl silicone oil and 8-60 parts of vinyl silicone resin.
In the examples of the present invention, vinyl silicone oil, hydrogen-containing silicone oil, long-chain alkyl silicone oil, and vinyl silicone resin were purchased from Jiangxi Lanxing spark Silicone Co., Ltd.
The embodiment of the invention also provides a preparation method of the organic silicon material, which comprises the following steps:
adding the modified nano silicon carbide into the organic silicon mixture according to the addition amount of 3-8% by weight, and performing planetary dispersing mixing and defoaming treatment to obtain the silicon carbide composite material. The dispersing and defoaming processes are conventional means, and are not described in detail herein.
The embodiment of the invention also provides application of the organic silicon material in an outdoor brightening screen.
In the embodiment of the invention, according to the construction requirements of the LED brightening screen, the screen body and the curtain wall glass can be assembled for use after being attached in advance in a plane blade coating/spraying mode, and the screen body can also be pre-fixed on the periphery of the finished curtain wall and then poured and attached.
The technical effects of the organosilicon material of the present invention will be further described with reference to specific examples, wherein, unless otherwise specified, "parts" and "%" in the examples refer to "parts by weight" and "percent by mass", respectively; however, the specific implementation methods mentioned in these examples are only illustrative of the technical solutions of the present invention, and do not limit the implementation scope of the present invention.
Example 1
Introducing 2kg of nano silicon carbide powder coated with a silicon dioxide film on the surface into a fluidized bed, adding 40g of tetramethyl divinyl disilazane, blowing compressed air (nitrogen) as carrier gas at the flow rate of 30mL/min, rapidly heating to 150 ℃, wherein the boiling effect is local boiling, reacting for 3 hours, stopping the carrier gas, and emptying the gas in the carrier gas to obtain the modified nano silicon carbide 1.
Adding the modified nano silicon carbide 1 into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 10 parts by weight of vinyl silicone resin) according to the addition amount of 3%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide composite material.
Example 2
Introducing 2kg of nano silicon carbide powder coated with a silicon dioxide film on the surface into a fluidized bed, adding 40g of tetramethyl divinyl disilazane, blowing compressed air (argon) as a carrier gas at the flow rate of 70mL/min, rapidly heating to 170 ℃, reacting for 4 hours with the boiling effect of convection boiling, stopping the carrier gas, and emptying the gas in the carrier gas to obtain the modified nano silicon carbide 2.
Adding the modified nano silicon carbide 2 into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin) according to the addition of 5%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide composite material.
Example 3
Introducing 2kg of nano silicon carbide powder coated with a silicon dioxide film on the surface into a fluidized bed, then adding 100g of tetramethyl divinyl disilazane, blowing compressed air (argon) as carrier gas at the flow rate of 80mL/min, rapidly heating to 180 ℃, wherein the boiling effect is wave boiling, reacting for 5 hours, then stopping the carrier gas, and emptying the gas in the carrier gas to obtain the modified nano silicon carbide 3.
Adding the modified nano silicon carbide 3 into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin) according to the addition amount of 8%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide composite material.
Example 4
Introducing 2kg of nano silicon carbide powder coated with a silicon dioxide film on the surface into a fluidized bed, then adding 100g of tetramethyl divinyl disilazane, blowing compressed air (nitrogen) as carrier gas at the flow rate of 70mL/min, rapidly heating to 180 ℃, wherein the boiling effect is wave boiling, reacting for 3h, then stopping the carrier gas, and emptying the gas in the carrier gas to obtain the modified nano silicon carbide 4.
Adding the modified nano silicon carbide 4 into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin) according to the addition amount of 5%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide composite material.
Comparative example 1
Adding unmodified nano silicon carbide powder with a surface coated with a silicon dioxide film into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 10 parts by weight of vinyl silicone resin) according to the addition amount of 3%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide nano silicon carbide composite material.
Comparative example 2
Adding unmodified nano silicon carbide powder with a surface coated with a silicon dioxide film into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin) according to the addition amount of 5%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide nano silicon carbide composite material.
Comparative example 3
Adding unmodified nano silicon carbide powder with a surface coated with a silicon dioxide film into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin) according to the addition amount of 8%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide nano silicon carbide composite material.
Comparative example 4
The preparation method comprises the following steps of sequentially adding unmodified nano silicon carbide powder with a surface coated with a silicon dioxide film and tetramethyl divinyl disilazane (the amount is the same as that in example 3) into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin), performing planetary dispersion mixing, defoaming and packaging.
Comparative example 5
Adding commercially available single nano silicon carbide powder (which is not modified by a coupling agent and is not coated with a silicon dioxide film) into an organic silicon mixture (the organic silicon mixture is prepared by directly and uniformly mixing 65 parts by weight of vinyl silicone oil, 15 parts by weight of hydrogen-containing silicone oil, 7 parts by weight of long-chain alkyl silicone oil and 8 parts by weight of vinyl silicone resin) according to the addition amount of 8%, performing planetary dispersion mixing, defoaming and packaging to obtain the silicon carbide composite material.
Blank group
The single organic silicon mixture system is prepared by directly and uniformly mixing the following raw materials in parts by weight: 65 parts of vinyl silicone oil, 15 parts of hydrogen-containing silicone oil, 7 parts of long-chain alkyl silicone oil and 8 parts of vinyl silicone resin.
The morphology of the modified nano silicon carbide 1 prepared in the example 1 is observed through an optical microscope, and the result is shown in fig. 1, wherein the obtained modified nano silicon carbide is spherical, and the particle size is 3-10 micrometers; the silicone materials prepared in the above examples 1-3 and comparative examples 1-4, and the blank group, and the existing commercial product (silicone potting adhesive) were subjected to density (GB/T13354-.
TABLE 1
To sum up, as can be seen from table 1 above, in the organic silicon material prepared in embodiments 1 to 4 of the present invention, by adding a vinyl coupling agent-modified nano silicon carbide with a surface coated with a silicon dioxide film in an organic silicon-based adhesive system, not only is the light transmittance of the cured adhesive layer greater than 95%, no yellowing occurs after aging for 1000 hours at 85% RH and 85 ℃, no cracking or yellowing occurs after 1000 cycles of cold and heat shock at-40 ℃ to 80 ℃, no cracking, embrittlement, and yellowing occur after 500 hours of Qsun test, but also the thermal conductivity is increased to 0.52 to 0.8W/(m · K), and the thermal conductivity gradually increases with the increase of the content of the modified nano silicon carbide; the thermal conductivity of the organosilicon material prepared in comparative examples 1-3 shows that the addition of the nano silicon carbide with the surface coated with the silicon dioxide film, which is not modified by the vinyl coupling agent, to the organosilicon-based adhesive system does not increase the thermal conductivity of the organosilicon material due to the increase of the nano silicon carbide, and the thermal conductivity is only 0.2-0.3W/(m.k), and in addition, the tendency of light transmittance and weather resistance deterioration occurs with the increase of the nano silicon carbide; in contrast, in comparative example 4, the unmodified nano silicon carbide powder with the surface coated with the silicon dioxide film and the tetramethyl divinyl disilazane are sequentially added into the organic silicon mixture, so that the light transmittance, the heat conductivity and the weather resistance of the prepared organic silicon material are not improved due to the addition of the tetramethyl divinyl disilazane; in contrast, in comparative example 5, a single nano silicon carbide powder available on the market was directly added to the silicone mixture, and the silicone material obtained was also poor in light transmittance, thermal conductivity and weather resistance. The main reason is that the nano silicon carbide powder coated with the silicon dioxide film on the surface and the single nano silicon carbide powder have poor compatibility with an organic silicon system and migrate in the using process; the nano silicon carbide with the surface coated with the silicon dioxide film modified by the vinyl coupling agent has excellent hydrophobicity, and the silicon dioxide layer coated with the surface also has vinyl which participates in the reaction of an organic silicon-based adhesive system, so that the body crosslinking is realized by an interpenetrating network structure, the migration cannot occur in the subsequent use process, the transparency of the material is ensured, and the heat conductivity and the weather resistance of the material can be improved.
Further, according to the construction requirements of the LED brightening screen, the organic silicon materials prepared in the embodiments 1-4 and the comparative examples 2-3 and the existing commercial products (organic silicon pouring sealant) are assembled and used after the screen body and the curtain wall glass are attached in advance in a plane blade coating mode, the LED junction temperature, the light transmittance and the outdoor aging condition are tested and analyzed, and the results are shown in Table 2.
The LED junction temperature test method comprises the following steps: testing by adopting a TRA-300 LED thermal structure analysis testing system; light transmittance: according to ASTM D1003-61 Standard Test Method for Haze and lumineous Transmission of Transparent Plastics (Transparent Plastics light transmittance and Haze Test Method); temperature and humidity resistance reliability, cold and hot impact stability, high temperature and low temperature reliability tests are carried out according to GB/T2423.3-2006 part 2 of test method test cab of environment test of electrical and electronic products: constant damp heat test execution; the outdoor aging condition test method comprises the following steps: and directly placing the product on an outdoor balcony for aging after the product is manufactured.
TABLE 2
In summary, as can be seen from table 2, the refractive index of the organosilicon material prepared in embodiments 1 to 4 of the present invention is close to that of the screen body and the curtain wall, when the organosilicon material is used for bonding the screen body and the curtain wall, the light transmittance of the cured bonding layer is greater than 95%, no yellowing occurs after aging for 1000 hours under 85% RH and 85 ℃, no cracking and yellowing occur after 1000 cycles of cold and heat shock at-40 ℃ to 80 ℃, no cracking, embrittlement and yellowing phenomena occur after 500 hours of Qsun test, no yellowing, cracking and hardening phenomena occur in 30 days outdoors, and the LED junction temperature in the screen body can be reduced from 70 ℃ to 56-60 ℃.
Further, in the research and development process, the addition content of the modified silicon carbide directly affects the performance of the organic silicon system, only the addition content of the modified silicon carbide is changed based on the process conditions of the embodiment 3 of the invention, the related performance of the obtained organic silicon system is tested, and the test results are shown in table 3.
TABLE 3 Effect of the amount of modified silicon carbide added on System Performance
In summary, as can be seen from table 3, in the embodiment of the present invention, the addition amount of the modified silicon carbide directly affects the performance of the organic silicon system, that is, the addition amount of the modified silicon carbide is not less than 3%, when the amount of the modified silicon carbide is too small, the modified silicon carbide cannot form a heat conducting network, and the addition amount of the modified silicon carbide is not more than 8%, when the addition amount of the modified silicon carbide is too large, the optical performance of the organic silicon system is directly affected, and the modified silicon carbide is agglomerated, so that the thermal conductivity is not significantly increased, but the weather resistance is reduced.
Furthermore, in the research and development process, the step process of modifying the coupling agent, the reaction time, the reaction temperature, the flow rate of the carrier gas, the type of the carrier gas and the boiling effect of the fluidized bed all have certain influence on the modification effect of the silicon carbide, the dispersion and interpenetrating network crosslinking effects of the modified silicon carbide in the using process are directly influenced, and further the optical and heat-conducting properties of the cured material are influenced, and on the basis of the process conditions of the embodiment 3 of the invention, only part of process parameters (the reaction time, the reaction temperature, the boiling effect and the flow rate of the carrier gas) are changed, and the related properties of the obtained organic silicon system are tested, and the test results are shown in tables 4-7.
TABLE 4 Effect of reaction time on System Performance
TABLE 5 Effect of reaction temperature on System Performance
TABLE 6 Effect of boiling effect on System Performance
TABLE 7 Effect of carrier gas flow Rate on System Performance
In summary, from tables 4-5, when the reaction time is too short or the reaction temperature is too low, the light transmittance, thermal conductivity and weather resistance of the system are poor, and when the reaction time is too long or the reaction temperature is too high, the weather resistance of the system is rather poor, mainly because the short reaction time or the too low reaction temperature leads to incomplete coating of the system and poor dispersion of the heat conductive filler; and the excessively long reaction time or the excessively high reaction temperature is not favorable for reducing the cost, and the excessive decomposition of the coupling agent can influence the stability of the coating and the subsequent interpenetrating network crosslinking structure. From tables 6-7, it can be seen that when the flow rate of the carrier gas is too low, the nano powder cannot be completely boiled, resulting in incomplete coating of the nano powder and poor dispersion of the heat conductive filler; the high flow rate of the carrier gas is not favorable for reducing the cost, and the excessive decomposition of the coupling agent can influence the stability of the coating and the subsequent interpenetrating network crosslinking structure.
It can be seen from the above tables 4-7 that in the process of modifying nano-silicon carbide with a silica film coated on the surface by a coupling agent, convection boiling can be formed only when the reaction time, reaction temperature and air flow rate are appropriate, so as to ensure the full coating modification of nano-silicon carbide, and the best performance can be formed only when the powder with complete surface modification is added into the system. Experiments prove that when argon is blown in at the flow rate of 100mL/min as carrier gas and the light transmittance reaches and reacts for 5 hours at the temperature of 170 ℃, the obtained modified silicon carbide is added into an organic silicon system to obtain the organic silicon material, the organic silicon material has the advantages that the light transmittance is as high as 97.5 percent and the thermal conductivity is as high as 0.85W/(m.K) while the excellent weather resistance is ensured.
In addition, in the development process of the invention, other coupling agents (such as vinyl triisopropoxysilane, vinyl trimethoxy silane, vinyl tri-tert-butoxysilane, vinyl triethoxy silane, gamma-glycidoxypropyl trimethoxy silane, gamma-aminopropyl triethoxy silane and the like) are used for modifying the nano silicon carbide, and the scheme of replacing only the coupling agent by using types based on the process conditions of the embodiment 3 of the invention is shown below, and the relevant performances of the obtained organosilicon system are tested, and as shown in table 8, the relevant experiments with large differences of the performance influence effects are shown below.
TABLE 8 influence of the kind of silane coupling agent
From Table 8, it is understood that when the coupling agent is selected from vinyltriisopropoxysilane, vinyltrimethoxysilane, vinyltri-t-butoxysilane, and vinyltri-t-butoxysilane, the obtained silicone material has good thermal conductivity, light transmittance, and weather resistance; when the type of the coupling agent is vinyltriethoxysilane, although the thermal conductivity, light transmittance and weather resistance of the obtained organosilicon material are superior to those of the scheme that the type of the coupling agent is gamma-glycidoxypropyltrimethoxysilane or gamma-aminopropyltriethoxysilane, the obtained organosilicon material is still inferior to the relevant performances of the organosilicon material obtained in the embodiment of the invention, mainly because the vinyltriethoxysilane cannot completely coat the powder in a fluidized bed, and the generated hydrolysate ethanol also remains in the system and deteriorates the performances after curing after being added into the system; the powder modified by gamma-glycidoxypropyltrimethoxysilane can not react with an organic silicon substrate to form an interpenetrating network structure, so that the optical performance is influenced and the reliability is reduced after long-term use; and the gamma-aminopropyltriethoxysilane modified powder can not react with an organic silicon substrate to form an interpenetrating network structure, so that the optical performance is influenced, the reliability is reduced after long-term use, and the yellowing is obvious.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (12)
1. An organic silicon material is characterized in that the organic silicon material is prepared by adding modified nano silicon carbide into an organic silicon mixture;
the modified nano silicon carbide is obtained by modifying nano silicon carbide with a silicon dioxide film coated on the surface by a coupling agent.
2. The organosilicon material of claim 1, wherein the modified silicon carbide is present in an amount of 3-8% by weight of the organosilicon mixture.
3. The silicone material according to claim 1, wherein the coupling agent is a vinyl silane coupling agent.
4. The silicone material of claim 3, wherein the vinyl silane coupling agent is one of tetramethyldivinyldisilazane, vinyltriisopropoxysilane, vinyltrimethoxysilane, vinyltri-tert-butoxysilane, and vinyltri-tert-butoxysilane.
5. The organosilicon material according to claim 1, wherein the modified silicon carbide is obtained by introducing nano silicon carbide coated with a silica film on the surface into a fluidized bed, adding a coupling agent, blowing compressed air as a carrier gas at a flow rate of 30 to 100mL/min, and reacting at a temperature of 150 to 180 ℃ for 3 to 5 hours.
6. The organosilicon material of claim 5, wherein the weight ratio of the nano-silicon carbide and the coupling agent of the surface-coated silicon dioxide film is 1: 0.02-0.05.
7. The silicone material of claim 5, wherein the boiling effect of the fluidized bed is one of partial boiling, convective boiling, and wavy boiling.
8. The organosilicon material of claim 5, wherein the modified silicon carbide is prepared by introducing the nano silicon carbide coated with the silicon dioxide film into a fluidized bed, adding a coupling agent, blowing compressed air as a carrier gas at a flow rate of 100mL/min, and reacting at a temperature of 170 ℃ for 5 hours.
9. The silicone material of claim 5, wherein the compressed air is nitrogen or argon.
10. The silicone material according to claim 1, wherein the silicone mixture comprises the following raw materials in parts by weight:
10-65 parts of vinyl silicone oil, 2-15 parts of hydrogen-containing silicone oil, 5-15 parts of long-chain alkyl silicone oil and 8-60 parts of vinyl silicone resin.
11. A method for preparing a silicone material according to any one of claims 1 to 10, comprising:
adding the modified nano silicon carbide into the organic silicon mixture according to the addition amount of 3-8% by weight, and performing planetary dispersing mixing and defoaming treatment to obtain the silicon carbide composite material.
12. Use of a silicone material according to any one of claims 1 to 10 in outdoor glazing screens.
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