CN116083041A - Anti-overload organic silicon pouring sealant based on nano microspheres and preparation method thereof - Google Patents
Anti-overload organic silicon pouring sealant based on nano microspheres and preparation method thereof Download PDFInfo
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- 239000004005 microsphere Substances 0.000 title claims abstract description 74
- 239000000565 sealant Substances 0.000 title claims abstract description 44
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 100
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 47
- 239000002904 solvent Substances 0.000 claims abstract description 47
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229920002545 silicone oil Polymers 0.000 claims abstract description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910008051 Si-OH Inorganic materials 0.000 claims abstract description 6
- 229910006358 Si—OH Inorganic materials 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical group C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 4
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000000839 emulsion Substances 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- -1 polydimethylsiloxane Polymers 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 claims description 5
- 125000001165 hydrophobic group Chemical group 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 3
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 claims 2
- 239000004945 silicone rubber Substances 0.000 abstract description 15
- 229910052697 platinum Inorganic materials 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 8
- 239000006229 carbon black Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000004382 potting Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005489 elastic deformation Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012974 tin catalyst Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention provides a preparation method of anti-overload organic silicon pouring sealant based on nano microspheres, which comprises the following steps: preparing a first mixture of silicone rubber, solvent and nano-silica microspheres or surface-modified nano-silica microspheres; preparing a second mixture of a curing agent and a catalyst; and stirring and defoaming the first mixture and the second mixture, pouring and defoaming, and solidifying to form the overload-resistant organic silicon pouring sealant. The nanometer silicon dioxide microsphere is a silicon dioxide microsphere with a monodisperse surface group of Si-OH in a range of 50-500nm, or a compound mixture is formed by a plurality of monodisperse microspheres; the organic silicon rubber is methyl vinyl silicon rubber or hydroxyl silicon rubber; the solvent is one or more of ethyl acetate solvent, cyclohexane solvent or absolute ethyl alcohol; or one or more of benzene, cyclohexane or n-hexane solvents; the curing agent is organosilicate or hydrogen-containing silicone oil; the catalyst comprises an organotin catalyst or an organic platinum catalyst; corresponding anti-overload organic silicon pouring sealant is also disclosed.
Description
Technical Field
The invention relates to the technical field of preparation of potting materials, in particular to an overload-resistant organic silicon potting adhesive based on nano microspheres and a preparation method thereof.
Background
The organosilicon potting material has been widely used in missile-borne electronic devices due to excellent high-low temperature performance, no corrosiveness, good fluidity, mild curing conditions, simple and easily controlled process. The overload impact energy generated during the emission is absorbed through the elastic deformation of the circuit board fixing frame and the potting adhesive, so that the normal operation of the missile-borne circuit can be ensured. In general, impact overload applied to a missile-borne electronic device in the process of transmitting and penetrating is about 5000-10000g, even 5-10 ten thousand g of overload is achieved in a penetrating weapon, and the traditional pouring sealant for pouring a circuit board under the overload impact of 5000-20000 g is insufficient in strength and overload resistance and energy absorption capacity, so that the circuit board is easy to distort and deform, and the circuit function is invalid and cannot play a role. In addition to the design of the protection structure of the missile-borne electronic device under the condition, the composition and the strength of the pouring sealant, particularly the dynamic strength under the loading condition, and whether the interference signals in the penetration process can be attenuated and filtered become key factors influencing the normal performance of the function of the missile-borne electronic device.
The existing elastic loading organic silicon pouring sealant generally adopts particles such as micron-scale silica micropowder, white carbon black and the like to adjust the compression strength, hardness and energy absorption capacity of the pouring sealant; the organic silicon rubber matrix is usually a dealcoholized silicon rubber system or an addition type organic silicon system, the dealcoholized organic silicon is prepared from hydroxyl silicon rubber base rubber, an organic silicate curing agent and an organic tin catalyst, the strength and the hardness of the organic silicon rubber system are low, and white carbon black is often required to be added as a reinforcing filler; even so, there are disadvantages of low hardness and breakage. The organic silicon rubber is composed of vinyl silicon rubber matrix, hydrogen-containing silicon rubber and platinum catalyst, the mechanical strength and toughness of the organic silicon rubber system are better than those of dealcoholized organic silicon rubber, but in the aspect of overload protection application, a certain amount of solid powder filler such as white carbon black and silicon micropowder is still required to be added into the organic silicon rubber to strengthen the mechanical strength and regulate the hardness, and usually only 2500-5000 g of overload protection can be met. Because the inorganic filler is generally between micrometers and tens of micrometers in size and the particle size is not uniform, the surface interface between the organic silicon pouring sealant matrix and particles is not rich enough, the synergistic energy absorption capability is weak, the dynamic strength is not high, and the application requirement of overload resistance of the missile-borne electronic system under the condition of high overload of 5000-200000g cannot be met.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the anti-overload organic silicon pouring sealant based on the nano-microspheres and the preparation method thereof are provided, the nano-silica microspheres and the like are used for replacing the traditional silica micropowder, white carbon black and other inorganic fillers, and a solvent-assisted and ultrasonic dispersion process is adopted, so that the uniform dispersion of the nano-microspheres in a silicon rubber matrix with higher viscosity is realized, and the application problems of insufficient dynamic impact energy absorption and insufficient signal highlighting of the traditional micro-particle filled anti-overload pouring sealant are solved; meanwhile, the nano silicon dioxide microspheres and the nano silicon dioxide microspheres modified by the surface groups have the characteristics of uniform particle size, high sphericity, smooth surface and the like, and the scale smaller than 1um can be more beneficial to reflecting the rigid-flexible synergistic energy absorption effect on the microstructure of the organic silicon composite system under the dynamic overload impact effect.
The invention aims to provide a preparation method of anti-overload organic silicon pouring sealant based on nano microspheres, which comprises the following steps:
s1, preparing a first mixture formed by organic silicon rubber, a solvent and nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres;
s2, preparing a second mixture formed by a curing agent and a catalyst;
and S3, stirring and defoaming the first mixture and the second mixture, casting and defoaming, and solidifying to form the overload-resistant organic silicon pouring sealant.
Preferably, the organic silicone rubber is methyl vinyl silicone rubber or hydroxyl silicone rubber, the hydroxyl silicone rubber comprises hydroxyl-terminated methyl silicone rubber, and the hydroxyl-terminated methyl silicone rubber is omega-dihydroxymethyl silicone rubber.
Preferably, the solvent is one or more of ethyl acetate solvent, cyclohexane solvent or absolute ethanol; or one or more of benzene, cyclohexane or n-hexane solvents.
Preferably, the surface-modified nano-silica microspheres are nano-silica microspheres with surfaces modified to hydrophobic groups (-CH 3); the nano silicon dioxide microsphere or the surface modified nano silicon dioxide microsphere is a silicon dioxide microsphere with a monodisperse surface group of Si-OH within a range of 50-500nm, or a compound mixture formed by a plurality of monodisperse microspheres, wherein the monodisperse microsphere comprises a compound mixture of silicon dioxide microspheres with surface groups of Si-OH, methyl and alkyl.
Preferably, the S1 includes:
s11, ultrasonically stirring and dispersing metered nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres in the solvent until no precipitate exists, so as to form uniform white emulsion;
s12, adding a metered matrix of the organic silicon rubber into the white emulsion, and continuing ultrasonic stirring and dispersing for 0.5-3 hours to form a first mixed solution;
s13, removing the solvent from the first mixed solution at the temperature of 40-60 ℃ to obtain a first mixture of uniformly dispersed nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres in a matrix of the organic silicon rubber; the solvent removal is a reduced pressure distillation solvent removal method, a rotary evaporation solvent removal method or a heating stirring vacuumizing solvent removal method.
Preferably, the curing agent is organosilicate or hydrogen-containing silicone oil, and the organosilicate comprises an ethyl orthosilicate cross-linking agent or vinyl polydimethylsiloxane; the hydrogen-containing silicone oil is a hydrogen-containing silicone oil cross-linking agent and a cross-linking inhibitor.
Preferably, the catalyst comprises an organotin catalyst or an organo-platinum group catalyst.
Preferably, the S2 includes: and stirring and mixing the curing agent and the catalyst according to a metering proportion at room temperature to obtain a second mixed solution of the curing system.
Preferably, the S3 includes:
s31, stirring and defoaming the metered first mixed solution and the metered second mixed solution by using a mechanical stirring or planetary stirring deaerator for 3-5 minutes;
s32, pouring the material into a device to be encapsulated, and performing vacuum defoamation again for 1-3 minutes;
s33, curing for 2-4 hours at the temperature of 40-80 ℃ to form the overload-resistant organic silicon pouring sealant.
The second aspect of the invention provides a nano-microsphere-based overload-resistant organic silicon pouring sealant, which is prepared by a preparation method of the nano-microsphere-based overload-resistant organic silicon pouring sealant.
The invention has the beneficial effects that:
the traditional silica micropowder, white carbon black and other inorganic fillers are replaced by nano silica microspheres and the like, and a solvent-assisted and ultrasonic dispersion process is adopted, so that the uniform dispersion of the nano microspheres in a silicon rubber matrix with higher viscosity is realized, and the application problems of insufficient dynamic impact energy absorption and insufficient signal salient of the traditional micron particle filled overload-resistant pouring sealant are solved; meanwhile, the nano silicon dioxide microspheres and the nano silicon dioxide microspheres modified by the surface groups have the characteristics of uniform particle size, high sphericity, smooth surface and the like, and the scale smaller than 1um can be more beneficial to reflecting the rigid-flexible synergistic energy absorption effect on the microstructure of the organic silicon composite system under the dynamic overload impact effect.
The above, as well as additional objectives, advantages, and features of the present invention will become apparent to those skilled in the art from the following detailed description of a specific embodiment of the present invention when read in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the invention will be described in detail hereinafter by way of example and not by way of limitation with reference to the accompanying drawings. The same reference numbers will be used throughout the drawings to refer to the same or like parts or portions. It will be appreciated by those skilled in the art that the drawings are not necessarily drawn to scale. The objects and features of the present invention will become more apparent in view of the following description taken in conjunction with the accompanying drawings in which:
fig. 1 is a schematic flow chart of a preparation method of an anti-overload organic silicon pouring sealant based on nano microspheres according to an embodiment of the invention.
Detailed Description
In order to better understand the above technical solutions, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, the embodiment provides a preparation method of an anti-overload organic silicon pouring sealant based on nano microspheres, which comprises the following steps:
s1, preparing a first mixture formed by organic silicon rubber, a solvent and nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres;
s2, preparing a second mixture formed by a curing agent and a catalyst;
and S3, stirring and defoaming the first mixture and the second mixture, casting and defoaming, and solidifying to form the overload-resistant organic silicon pouring sealant.
As a preferred embodiment, the organic silicone rubber is methyl vinyl silicone rubber or hydroxy silicone rubber, the hydroxy silicone rubber includes a hydroxy-terminated methyl silicone rubber, and the hydroxy-terminated methyl silicone rubber is ω -dihydroxy methyl silicone rubber.
As a preferred embodiment, the solvent is one or more of ethyl acetate solvent, cyclohexane solvent or absolute ethanol; or one or more of benzene, cyclohexane or n-hexane solvents.
As a preferred embodiment, the surface-modified nano-silica microspheres are nano-silica microspheres surface-modified to hydrophobic groups (-CH 3); the nano silicon dioxide microsphere or the surface modified nano silicon dioxide microsphere is a silicon dioxide microsphere with a monodisperse surface group of Si-OH in a range of 50-500nm, and can also be a compound mixture formed by a plurality of monodisperse microspheres, and in order to realize rapid and uniform dispersion, the silicon dioxide microsphere with a surface of methyl or other alkyl is preferable.
As a preferred embodiment, the S1 includes:
s11, ultrasonically stirring and dispersing metered nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres in the solvent until no precipitate exists, so as to form uniform white emulsion;
s12, adding a metered matrix of the organic silicon rubber into the white emulsion, and continuing ultrasonic stirring and dispersing for 0.5-3 hours to form a first mixed solution;
s13, removing the solvent from the first mixed solution at the temperature of 40-60 ℃ to obtain a first mixture of uniformly dispersed nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres in a matrix of the organic silicon rubber; the solvent removal is a reduced pressure distillation solvent removal method, a rotary evaporation solvent removal method or a heating stirring vacuumizing solvent removal method.
As a preferred embodiment, the curing agent is an organosilicate or a hydrogen-containing silicone oil, the organosilicate comprising an ethyl orthosilicate cross-linking agent or a vinyl polydimethylsiloxane; the hydrogen-containing silicone oil is a hydrogen-containing silicone oil cross-linking agent and a cross-linking inhibitor.
As a preferred embodiment, the catalyst comprises an organotin catalyst or an organoplatinum-based catalyst.
As a preferred embodiment, the S2 includes: and stirring and mixing the curing agent and the catalyst according to a metering proportion at room temperature to obtain a second mixed solution of the curing system.
As a preferred embodiment, the S3 includes:
s31, stirring and defoaming the metered first mixed solution and the metered second mixed solution by using a mechanical stirring or planetary stirring deaerator for 3-5 minutes;
s32, pouring the material into a device to be encapsulated, and performing vacuum defoamation again for 1-3 minutes;
s33, curing for 2-4 hours at the temperature of 40-80 ℃ to form the overload-resistant organic silicon pouring sealant.
The second aspect of the embodiment provides a nano-microsphere-based anti-overload organic silicon pouring sealant, which is prepared by a preparation method of the nano-microsphere-based anti-overload organic silicon pouring sealant.
Example 1
(1) Adding 10-50 parts of nano silicon dioxide microspheres into 200-300 parts of ethyl acetate solvent, stirring, and performing ultrasonic dispersion for 3-5 hours until a white emulsion without precipitate is formed;
(2) Adding 50-100 parts of alpha, omega-dihydroxyl polydimethylsiloxane into the white emulsion, stirring, ultrasonically dispersing for 10-30min, and then heating at 40-60 ℃ and decompressing to remove solvent ethyl acetate to obtain a viscous white liquid component A;
(3) Adding 0.1-1 part of catalyst into 5-10 parts of tetraethoxysilane cross-linking agent to form a component B;
(4) Mixing the prepared A, B components for 3-5min at a stirring speed of 100-500rpm, defoaming for 30-50s at a pressure of 50-70kPa, pouring into a mold or a device to be encapsulated, and vulcanizing for 24-6h at a temperature of 20-80 ℃ under the condition of RH 40-60%.
The obtained nano silica microsphere reinforced overload-resistant potting material is white opaque solid, has Shore A hardness of 25-50, tensile strength of more than 3MPa and loss factor of 0.1-0.3 at 25 ℃, and can meet the application of overload-resistant potting of 5000-10000 g.
Example 2
(1) 10-50 parts of nano silicon dioxide microsphere with the surface modified into a hydrophobic group (-CH 3) are added into 200-300 parts of cyclohexane solvent, stirred and dispersed for 3-5 hours by ultrasonic until white emulsion without sediment is formed;
(2) Adding 50-100 parts of vinyl polydimethylsiloxane into the white emulsion, stirring, ultrasonically dispersing for 10-30min, heating at 40-60 ℃ and decompressing to remove solvent cyclohexane, adding 5-20 parts of hydrogen-containing silicone oil crosslinking agent and crosslinking inhibitor, and fully and uniformly stirring to obtain a viscous white liquid component A;
(3) Adding 0.5-1 part of platinum catalyst into 10-50 parts of vinyl polydimethylsiloxane, and fully stirring for 3-5min to obtain a component B;
(4) 100 parts of the component A and 5-10 parts of the component B are stirred and mixed for 3-5min at 100-300rpm, and defoamed under the vacuum degree of 0.06-0.1 MPa to obtain the high-strength overload-resistant organosilicon pouring sealant. The pouring sealant has excellent fluidity, the room temperature operation time is longer than 1.5h, and the curing time is 48h at 25 ℃. The obtained solidified material is white opaque solid, the Shore A hardness is 35-50, the tensile strength is more than 6MPa, the using temperature is between-45 ℃ and 200 ℃, and the loss factor is 0.25-0.3 at 0-120 ℃.
The pouring sealant is widely applied to the pouring of overload-resistant electronic devices in a high-low temperature wide-temperature range, has good mechanical property and dynamic impact energy absorption performance, and can meet the application of overload-resistant pouring of 5000-25000 g.
Example 3
(1) 10-50 parts of nano silicon dioxide microsphere with the surface modified into a hydrophobic group (-CH 3) are added into 200-300 parts of cyclohexane solvent, stirred and dispersed for 3-5 hours by ultrasonic until white emulsion without sediment is formed;
(2) Adding 50-100 parts of vinyl polydimethylsiloxane into the white emulsion, stirring, ultrasonically dispersing for 10-30min, heating at 40-60 ℃ and decompressing to remove solvent cyclohexane, adding 5-20 parts of hydrogen-containing silicone oil crosslinking agent and crosslinking inhibitor, and fully and uniformly stirring to obtain a viscous white liquid component A;
(3) Adding 0.1-0.3 part of platinum catalyst into 10-50 parts of vinyl polydimethylsiloxane, and fully stirring for 3-5min to obtain a component B;
(4) 100 parts of the component A and 5-10 parts of the component B are stirred and mixed for 3-5min at 100-300rpm, and defoamed under the vacuum degree of 0.06-0.1 MPa to obtain the high-strength overload-resistant organosilicon pouring sealant. The pouring sealant has excellent fluidity, the room temperature operation time is longer than 1.5h, and the curing time is 4h at 80 ℃. The obtained solidified material is white opaque solid, the Shore A hardness is 35-50, the tensile strength is more than 6MPa, the using temperature is between-45 ℃ and 200 ℃, and the loss factor is 0.25-0.3 at 0-120 ℃.
The pouring sealant is widely applied to the pouring of overload-resistant electronic devices in a high-low temperature wide-temperature range, has good mechanical property and dynamic impact energy absorption performance, and can meet the application of overload-resistant pouring of 5000-25000 g.
The traditional silica micropowder, white carbon black and other inorganic fillers are replaced by nano silica microspheres and the like, and a solvent-assisted and ultrasonic dispersion process is adopted, so that the uniform dispersion of the nano microspheres in a silicon rubber matrix with higher viscosity is realized, and the application problems of insufficient dynamic impact energy absorption and insufficient signal salient of the traditional micron particle filled overload-resistant pouring sealant are solved; meanwhile, the nano silicon dioxide microspheres and the nano silicon dioxide microspheres modified by the surface groups have the characteristics of uniform particle size, high sphericity, smooth surface and the like, and the scale smaller than 1um can be more beneficial to reflecting the rigid-flexible synergistic energy absorption effect on the microstructure of the organic silicon composite system under the dynamic overload impact effect.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (10)
1. The preparation method of the anti-overload organic silicon pouring sealant based on the nano microspheres is characterized by comprising the following steps of:
s1, preparing a first mixture formed by organic silicon rubber, a solvent and nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres;
s2, preparing a second mixture formed by a curing agent and a catalyst;
and S3, stirring and defoaming the first mixture and the second mixture, casting and defoaming, and solidifying to form the overload-resistant organic silicon pouring sealant.
2. The method for preparing the overload-resistant organic silicon pouring sealant based on the nano microspheres according to claim 1, wherein the organic silicon rubber is methyl vinyl silicon rubber or hydroxyl silicon rubber, the hydroxyl silicon rubber comprises hydroxyl-terminated methyl silicon rubber, and the hydroxyl-terminated methyl silicon rubber is omega-dihydroxymethyl silicon rubber.
3. The method for preparing the anti-overload organic silicon pouring sealant based on the nano microspheres according to claim 2, wherein the solvent is one or more of ethyl acetate solvent, cyclohexane solvent and absolute ethyl alcohol; or one or more of benzene, cyclohexane or n-hexane solvents.
4. The method for preparing the anti-overload organic silicon pouring sealant based on the nano-microspheres according to claim 3, wherein the surface-modified nano-silica microspheres are nano-silica microspheres with surfaces modified into hydrophobic groups (-CH 3); the nano silicon dioxide microsphere or the surface modified nano silicon dioxide microsphere is a silicon dioxide microsphere with a monodisperse surface group of Si-OH within a range of 50-500nm, or a compound mixture formed by a plurality of monodisperse microspheres, wherein the monodisperse microsphere comprises a compound mixture of silicon dioxide microspheres with surface groups of Si-OH, methyl and alkyl.
5. The method for preparing the anti-overload organic silicon pouring sealant based on the nano microspheres according to claim 4, wherein the step S1 comprises the following steps:
s11, ultrasonically stirring and dispersing metered nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres in the solvent until no precipitate exists, so as to form uniform white emulsion;
s12, adding a metered matrix of the organic silicon rubber into the white emulsion, and continuing ultrasonic stirring and dispersing for 0.5-3 hours to form a first mixed solution;
s13, removing the solvent from the first mixed solution at the temperature of 40-60 ℃ to obtain a first mixture of uniformly dispersed nano silicon dioxide microspheres or surface modified nano silicon dioxide microspheres in a matrix of the organic silicon rubber; the solvent removal is a reduced pressure distillation solvent removal method, a rotary evaporation solvent removal method or a heating stirring vacuumizing solvent removal method.
6. The method for preparing the anti-overload organic silicon pouring sealant based on the nano microspheres according to claim 5, wherein the curing agent is organic silicate or hydrogen-containing silicone oil, and the organic silicate comprises an ethyl orthosilicate cross-linking agent or vinyl polydimethylsiloxane; the hydrogen-containing silicone oil is a hydrogen-containing silicone oil cross-linking agent and a cross-linking inhibitor.
7. The method for preparing the anti-overload organic silicon pouring sealant based on the nano microspheres according to claim 6, wherein the catalyst comprises an organotin catalyst or an organic platinum group catalyst.
8. The method for preparing the anti-overload organic silicon pouring sealant based on the nano microspheres according to claim 7, wherein the step S2 comprises the following steps: and stirring and mixing the curing agent and the catalyst according to a metering proportion at room temperature to obtain a second mixed solution of the curing system.
9. The method for preparing the anti-overload organic silicon pouring sealant based on the nano microspheres according to claim 8, wherein the step S3 comprises the following steps:
s31, stirring and defoaming the metered first mixed solution and the metered second mixed solution by using a mechanical stirring or planetary stirring deaerator for 3-5 minutes;
s32, pouring the material into a device to be encapsulated, and performing vacuum defoamation again for 1-3 minutes;
s33, curing for 2-4 hours at the temperature of 40-80 ℃ to form the overload-resistant organic silicon pouring sealant.
10. The anti-overload organic silicon pouring sealant based on the nano-microspheres is characterized by being prepared by the preparation method of the anti-overload organic silicon pouring sealant based on the nano-microspheres according to any one of claims 1-9.
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