CN110819297B - Condensed type heat-conducting pouring sealant capable of being quickly vulcanized at room temperature and preparation method thereof - Google Patents

Condensed type heat-conducting pouring sealant capable of being quickly vulcanized at room temperature and preparation method thereof Download PDF

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CN110819297B
CN110819297B CN201911274500.3A CN201911274500A CN110819297B CN 110819297 B CN110819297 B CN 110819297B CN 201911274500 A CN201911274500 A CN 201911274500A CN 110819297 B CN110819297 B CN 110819297B
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guanidine
pouring sealant
flame retardant
parts
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CN110819297A (en
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姬振行
王少华
王宇川
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Cetc Baoli Beijing Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a condensed heat-conducting flame-retardant pouring sealant fast vulcanized at room temperature and a preparation method thereof, wherein the pouring sealant comprises the following raw materials: the flame retardant is prepared from hydroxyl-terminated polysiloxane, SH-MQ organic silicon resin, modified fumed silica, an organic guanidine flame retardant, a heat conducting agent, a crosslinking agent, an organic guanidine catalyst and a diluent, wherein the organic guanidine flame retardant is a compound of guanidine sulfamate and guanidine polyphosphate. The invention leads the acetone-free type organic silicon pouring sealant to have excellent flame retardant performance by introducing the organic guanidine flame retardant into the raw materials, and simultaneously, the unexpected discovery shows that when the organic guanidine flame retardant is the compound of guanidine sulfamate and poly guanidine phosphate, the flame retardant and the organic guanidine catalyst can play a catalytic role in cooperation with the catalyst, at the moment, the pouring sealant can realize rapid curing, and the deep curing thickness is large. The pouring sealant prepared by the invention has excellent mechanical properties, and the preparation method is simple, low in production cost, easy for mass production, environment-friendly and pollution-free, and is suitable for industrial large-scale production.

Description

Condensed type heat-conducting pouring sealant capable of being quickly vulcanized at room temperature and preparation method thereof
Technical Field
The invention belongs to the field of organic silicon pouring sealant, and particularly relates to a room-temperature fast-vulcanization condensed type heat-conducting flame-retardant pouring sealant and a preparation method thereof.
Background
In the electronic industry, in order to improve the stability and reliability of components and complete machines, electronic components or assembled parts are often encapsulated, except for lead-out wires or connecting pieces, the whole parts are wrapped and sealed by encapsulating glue and isolated from the outside atmosphere, so that the complete machine can still normally work in environments of vibration, high humidity, severe temperature change, air pollution and the like. The most commonly used potting materials are the three main classes of epoxy, polyurethane and silicone rubber. Because the organic silicon rubber has excellent performances of high and low temperature resistance, weather resistance, moisture resistance, electric insulation, biological inertia, chemical stability and the like, the organic silicon rubber is recognized as a potting material for the electronic industry with great research potential and development prospect at home and abroad.
From the angle of a crosslinking mechanism, the organic silicon encapsulating material is divided into a condensation type and an addition type. The reaction principle of the addition type organic silicon pouring sealant is that siloxane containing vinyl and siloxane containing Si-H bonds are subjected to hydrosilylation reaction under the catalysis of an eighth-group transition metal compound (such as Pt) to form new Si-C bonds, so that linear siloxane is crosslinked into a network structure. The condensed type organosilicon pouring sealant takes hydroxyl-terminated polydiorganosiloxane as a basic polymer and multifunctional silane or siloxane as a cross-linking agent, and can perform condensation reaction when meeting moisture or being uniformly mixed at room temperature under the action of a catalyst to form a network-shaped elastomer. The condensed type organosilicon pouring sealant is inferior to the addition type organosilicon pouring sealant in overall comprehensive performance, but the condensed type organosilicon pouring sealant is far ahead of the addition type organosilicon pouring sealant in application field and dosage, because the condensed type organosilicon pouring sealant has lower cost, although the performance is inferior to the addition type organosilicon pouring sealant, the condensed type organosilicon pouring sealant can still meet the industries of building, electronics, automobiles, packaging, medical sanitation and the like, and most of people can select the condensed type organosilicon pouring sealant in order to save cost. Therefore, in the field of organic silicon pouring and sealing materials, the condensed organic silicon pouring and sealing glue has remarkable research potential and great application prospect compared with the addition type organic silicon pouring and sealing glue.
With the progress of science and technology, the line width of an integrated circuit is smaller and smaller, the integration level is higher and higher, and higher requirements are also put forward on the performance of the potting material, and particularly the potting material is required to have excellent heat resistance, thermal conductivity, flame retardant property and the like. The acetone-removing type organic silicon pouring sealant is the organic silicon pouring sealant with the best heat resistance in the condensed type organic silicon pouring sealant, has short-term temperature resistance of over 300 ℃, has high vulcanization speed, has stronger caking property on most base materials, can be widely used in high-temperature resistant environment, and most particularly is not like harmful gas with corrosivity and odor discharged like the traditional RTV silicon rubber. Although the acetone-free type organic silicon pouring sealant has the advantages, improvement of other properties is urgently needed, for example, the heat conductivity of the silicone pouring sealant is relatively poor, the flame retardant property of the silicone pouring sealant cannot meet the requirements of increasingly strict use environments, the mechanical property of the silicone pouring sealant is poor, the requirements of people on the work environments cannot be met, and the like. For example, patent CN201210588518.2 discloses a halogen-free flame retardant, high temperature resistant, fast curing, de-acetonized silicone rubber and a preparation method thereof, the silicone rubber uses hydroxyl-terminated polydimethylsiloxane as a main body, and is matched with a heat-resistant additive and a flame-retardant additive, including 100 parts of hydroxyl-terminated polydimethylsiloxane, 1-50 parts of polydimethylsiloxane, 5-18 parts of silicon dioxide, 5-15 parts of the heat-resistant additive, 50-200 parts of the flame-retardant additive, 0.5-2.5 parts of a tackifier, 0.5-1 part of an organoguanidine catalyst, and 5-8 parts of a de-acetonized silicone cross-linking agent, the de-acetonized silicone rubber has good heat resistance, but the defect in the beauty is that although the de-acetonized silicone rubber has excellent flame retardant performance, the mechanical performance of deep silicone rubber is seriously reduced due to excessive use amount, and the curing thickness is limited. Patent CN201010278350.6 discloses a silicone rubber with acetone removed and a preparation method thereof, which comprises the following raw materials by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 20-50 parts of plasticizer, 5-10 parts of acetone-removing type cross-linking agent, 500-1000 parts of spherical heat-conducting filler, 1-5 parts of needle-shaped heat-conducting filler, 6-10 parts of thixotropic agent, 1-2 parts of tackifier and 0.5-2 parts of organic guanidine catalyst, wherein the spherical heat-conducting filler is one or a mixture of any more of spherical alumina, spherical aluminum nitride, spherical boron nitride or spherical silicon carbide; the needle-shaped heat-conducting filler is zinc oxide whisker and carbon nano tube, although the heat-conducting capacity of the acetone-removed silicone rubber disclosed by the patent is improved, in order to improve the heat-conducting coefficient, the elongation at break of the acetone-removed silicone pouring sealant is greatly reduced due to the use of a large amount of heat-conducting filler, and the requirement of the pouring sealant on the mechanical property cannot be met.
In summary, there is a need to develop a de-acetone type silicone pouring sealant which has high thermal conductivity, good flame retardant property, and simultaneously, the comprehensive properties such as mechanical properties and the like are not greatly reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a room temperature fast vulcanization condensed type heat conduction flame retardant pouring sealant and a preparation method thereof, so as to improve the overall comprehensive performance of the existing deacetone type organic silicon pouring sealant, and particularly overcome the problem that the overall mechanical performance is reduced due to the improvement of the flame retardant performance or the heat conduction performance of the deacetone type organic silicon pouring sealant in the prior art.
In order to realize the purpose of the invention, the adopted specific technical scheme is as follows:
the condensed heat-conducting flame-retardant pouring sealant fast vulcanized at room temperature comprises the following raw materials: the flame retardant is prepared from hydroxyl-terminated polysiloxane, SH-MQ organic silicon resin, modified fumed silica, an organic guanidine flame retardant, a heat conducting agent, a crosslinking agent, an organic guanidine catalyst and a diluent, wherein the organic guanidine flame retardant is a compound of guanidine sulfamate and guanidine polyphosphate.
When the polymer of the organic guanidine flame retardant is heated, a uniform carbon foam layer can be generated on the surface, the layer can insulate heat, isolate oxygen, inhibit smoke and prevent the phenomenon of molten drop, has good flame retardant performance, and meets the development trend of the current flame retardant with less smoke and low toxicity.
In the preferred technical scheme of the invention, the condensed heat-conducting flame-retardant pouring sealant is provided, which comprises the following raw materials in parts by weight: 40-65 parts of hydroxyl-terminated polysiloxane, 1-5 parts of SH-MQ organic silicon resin, 5-10 parts of organic silicon modified fumed silica, 20-30 parts of organic guanidine flame retardant, 10-15 parts of heat conducting agent, 3-6 parts of cross-linking agent, 0.1-1 part of catalyst, 0.1-5 parts of diluent and 0.5-3 parts of silane coupling agent, wherein the organic guanidine flame retardant is compounded by guanidine sulfamate or guanidine polyphosphate.
Preferably, the organic guanidine flame retardant is a compound of guanidine sulfamate and guanidine polyphosphate according to the mass ratio of 2-4: 1-2.
The inventors have unexpectedly found that, with organic guanidine flame retardants, not only can the flame retardancy of the resulting product be satisfactory, but also the cure rate can be increased. Particularly, after the organic guanidine flame retardant is compounded by guanidine sulfamate and guanidine polyphosphate, a synergistic catalyst is generated to play a catalytic role, and at the moment, the pouring sealant can realize rapid curing and complete curing.
The heat-conducting agent can enable the pouring sealant to have good heat-conducting performance, and the heat-conducting agent is at least one of metal compounds such as aluminum nitride, aluminum oxide and zinc oxide.
Preferably, graphene can be further added into the heat conducting agent, and the mass ratio of the graphene to the metal nitride is 1: 5-8. The graphene is one or two mixtures of single-layer graphene and multi-layer graphene nanosheets, and the thickness of the graphene is 1-100 nm.
The viscosity of the hydroxyl-terminated polysiloxane is 500 to 10 ten thousand mps.
The modified fumed silica is modified by organic silicon, and the specific surface area of the modified fumed silica is 100-500m2And/g, the organosilicon modifying agent used for the organosilicon modified gas-phase silica is at least one selected from hexamethyldisilazane and octamethylcyclotetrasilazane.
The crosslinking agent is at least one selected from vinyl tri (isopropenyloxy) silane, methyl tri (isopropenyloxy) silane and phenyl tri (isopropenyloxy) silane.
The SH-MQ organic silicon resin has an MQ ratio of 0.5-0.8:1 and a solid content of 50% (150 ℃ C. 2H).
The organic guanidine catalyst is a compound containing guanidine and siloxane groups, and is specifically selected from at least one of 1, 1, 3, 3-tetramethylguanidinopropyltrimethoxysilane or 1, 1, 3, 3-tetramethylguanidinopropyltriethoxysilane.
The diluent is not an innovative point of the present invention, and examples thereof include, but are not limited to, at least one of 1, 4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether, o-tolyl glycidyl ether, hydroxy silicone oil, and white oil.
The silane coupling agent comprises at least one of KH550 or KH 560.
The pouring sealant can also comprise functional auxiliary materials, such as an ultraviolet light stabilizer, a heat stabilizer, a structure control agent, a silane coupling agent, a defoaming agent and the like, wherein the dosage of the functional auxiliary materials can be flexibly mastered by a person skilled in the art according to actual requirements, such as 0.01-2 parts of the ultraviolet light stabilizer, 0.1-5 parts of the heat stabilizer, 0.1-5 parts of the structure control agent and 0.1-8 parts of the defoaming agent.
The ultraviolet light stabilizer is a hindered amine light stabilizer, and examples thereof include, but are not limited to, at least one of bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate or pentamethylpiperidinol 2- (4 ' -hydroxy-3 ', 5 ' -di-tert-butyl) benzyl-2-n-butylmalonate.
The heat stabilizer is at least one selected from nano ferric oxide, nano cerium dioxide and nano tin dioxide, and the particle size of the heat stabilizer is 10-100 nm.
The structure control agent is selected from at least one of methyl phenyl diethoxysilane, tetramethyl ethylene dimethyl silane, low molecular weight hydroxyl silicone oil and silazane.
The defoaming agent is a siloxane defoaming agent, and examples include but are not limited to at least one of XP-008, BYK-141 and BYK-A530.
The invention also provides a preparation method of the pouring sealant, which comprises the following steps:
a. cleaning and preheating vacuum mixing equipment;
b. adding hydroxyl-terminated polysiloxane, SH-MQ organic silicon resin, organic silicon modified fumed silica, organic guanidine flame retardant and heat conducting agent, stirring, heating and vacuumizing;
c. mixing, stopping stirring, heating, and storing in sealed condition;
d. adding a diluent under the protection of dry nitrogen to adjust the viscosity, cooling, and filtering by a filter screen;
e. sequentially adding a cross-linking agent and a catalyst under the protection of dry nitrogen, wherein the raw material is added after being uniformly stirred under a vacuum condition every time;
f. and finally, transferring the mixture into a filling machine for extrusion and subpackage.
The preheating temperature of the step a is 50-80 ℃.
The heating temperature in the step b is 100-150 ℃, and the vacuum degree is 0.1-0.8 mpa.
The mixing time of the step c is 1-5 h.
In the step d, the viscosity is 1000-5000mps, the temperature reduction temperature is room temperature, and the mesh number of the filter screen is 100-500 meshes.
And e, stirring for 0.5-2 h.
The invention also provides application of the pouring sealant in serving as an electronic pouring sealant.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a de-acetone type organic silicon pouring sealant which is prepared by introducing an organic guanidine flame retardant into raw materials, and has excellent flame retardant performance.
The pouring sealant prepared by the invention has excellent mechanical properties, and the preparation method is simple, low in production cost, easy for mass production, environment-friendly and pollution-free, and is suitable for industrial large-scale production.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the descriptions in the following. Unless otherwise specified, "parts" in the examples of the present invention are parts by weight. All reagents used are commercially available in the art.
Example 1
a. Cleaning and preheating vacuum banburying equipment to 60 ℃;
b. adding 35 parts of hydroxyl-terminated polysiloxane with the viscosity of 1500mps.s and 15 parts of hydroxyl-terminated polysiloxane with the viscosity of 2 mps.s, 5 parts of SH-MQ organic silicon resin with the solid content of 50 percent (150 ℃ C. 2H) and the MQ ratio of 0.5-0.8:1 and the specific surface area of 300m25 parts of hexamethyldisilazane-modified fumed silica per gram, 30 parts of a compound of guanidine sulfamate and guanidine polyphosphate, and the weight ratio of the compound to the compound is 4:1, 12.5 parts of aluminum nitride, 1 part of ultraviolet light stabilizer bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, 2 parts of heat stabilizer nano ferric oxide with the particle size of 40nm, 2 parts of structure control agent methyl phenyl diethoxysilane and 0082 parts of defoaming agent XP-0082, stirring, heating to 120 ℃, and vacuumizing to 0.6 mpa;
c. mixing for 2h, stopping stirring and heating, and storing in a sealed manner;
d. adding 2 parts of 1, 4-butanediol diglycidyl ether serving as a diluent under the protection of dry nitrogen, adjusting the viscosity to 4500mps, cooling to room temperature, and filtering by using a 150-mesh filter screen;
e. adding 5 parts of cross-linking agent vinyl tri (isopropenyloxy) silane under the protection of dry nitrogen, stirring for 15min under vacuum, adding 0.8 part of catalyst 1, 1, 3, 3-tetramethylguanylpropyltriethoxysilane, stirring for 15min under vacuum, adding 1 part of KH-550 and 1 part of KH-560, and further stirring for 15min under vacuum;
f. and finally, transferring the mixture into a filling machine for extrusion and subpackage.
Example 2
The rest was the same as example 1 except that the weight ratio of guanidine sulfamate to guanidine polyphosphate was 2: 1.
Example 3
The rest was the same as example 1 except that the weight ratio of guanidine sulfamate to guanidine polyphosphate was 1: 1.
Example 4
The process was repeated as in example 1 except that the amount of the guanidine sulfamate-polyphosphoric acid mixture was 20 parts.
Example 5
The rest was the same as example 1 except that the weight ratio of guanidine sulfamate to guanidine polyphosphate was 1: 2.
Example 6
The rest was the same as example 1 except that the weight ratio of guanidine sulfamate to guanidine polyphosphate was 6: 1.
Example 7
The process was the same as in example 1 except that no graphene was added.
Comparative example 1
The procedure was as in example 1 except that the flame retardant was 30 parts of guanidine sulfamate.
Comparative example 2
The procedure was as in example 1 except that the flame retardant was 30 parts of guanidine sulfamate.
Application example
The potting compound prepared in the examples was subjected to the following performance tests:
time to surface dry
The tack-free time is tested with reference to the standard GB/T13477.5-2002.
And 24h deep curing thickness:
pouring the same amount of pouring sealant into a disposable cup with the same specification, then placing the cup in a constant humidity room, taking out after 24h, quickly drying the cured layer on the glass surface by using a clean and dry cloth strip, and measuring the thickness of the cured layer by using a vernier caliper, namely the 24h deep curing thickness of the sample. A total of 10 sets of data were measured and then averaged.
Limiting oxygen index
The determination of the Limiting Oxygen Index (LOI) is carried out using an oxygen index apparatus, according to the method of ASTM D2863.
Vertical combustion performance
The test is carried out by referring to American ANSI/UL94-2010, and the phenomenon A is that the combustion is violent, and the dropping object exists, so that the original shape can not be maintained; the phenomenon B is slow combustion, has no drop and can keep the original shape.
Coefficient of thermal conductivity
The thermal conductivity is measured according to the standard ASTM D5470.
Tensile Properties
The reference standard GB/T528-.
TABLE 1
Figure BDA0002315169840000061
The above table shows that the prepared acetone-free type organic silicon pouring sealant has excellent flame retardant property, wherein UL94 tests show that the silicone pouring sealant is V-0 grade, limit oxygen indexes are all over 27, the silicone pouring sealant belongs to a flame retardant material, the dosage of the flame retardant is moderate, and the mechanical property of the pouring sealant is not damaged; meanwhile, unexpected discovery is also found that when the organic guanidine flame retardant is compounded by amino guanidine sulfonate and poly guanidine phosphate, the flame retardant can play a catalytic role in cooperation with a catalyst, and can play an optimal synergistic catalytic effect when the ratio of the amino guanidine sulfonate to the poly guanidine phosphate is adjusted to be 2-4:1-2, at the moment, the pouring sealant can realize rapid curing, the deep curing thickness is greatly increased, the surface drying time can be as short as 5min, and the maximum deep curing thickness of 24h can reach 11.0mm and break through 10.0 mm; finally, the pouring sealant prepared by the invention has excellent mechanical property and heat conductivity, and the preparation method of the pouring sealant is simple, low in production cost, easy for mass production, environment-friendly and pollution-free, and is suitable for industrial large-scale production.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.

Claims (12)

1. The condensed heat-conducting flame-retardant pouring sealant fast vulcanized at room temperature is characterized by comprising the following raw materials in parts by weight: 40-65 parts of hydroxyl-terminated polysiloxane, 1-5 parts of SH-MQ organic silicon resin, 5-10 parts of organic silicon modified fumed silica, 20-30 parts of organic guanidine flame retardant, 10-15 parts of heat conducting agent, 3-6 parts of cross-linking agent, 0.1-1 part of catalyst and 0.1-5 parts of diluent, wherein the organic guanidine flame retardant is a compound of guanidine sulfamate and guanidine polyphosphate;
the mass ratio of the compound of guanidine sulfamate and guanidine polyphosphate is 2-4: 1-2.
2. The potting adhesive of claim 1, wherein the thermal conductive agent is at least one of aluminum nitride, aluminum oxide, and zinc oxide metal compounds.
3. The pouring sealant as claimed in claim 2, wherein the heat conducting agent further comprises graphene, and the mass ratio of the graphene to the metal compound is 1: 5-8; the graphene is one or two mixtures of single-layer graphene and multi-layer graphene nanosheets, and the thickness of the graphene is 1-100 nm.
4. The potting adhesive of claim 1, wherein the hydroxyl terminated polysiloxane has a viscosity of 1 to 5 ten thousand mps.
5. The pouring sealant as claimed in claim 1, wherein the specific surface area of the organosilicon-modified fumed silica is 100-500m2/g。
6. The pouring sealant according to claim 5, wherein the organosilicon-modified fumed silica is prepared by using an organosilicon modifier selected from at least one of hexamethyldisilazane and octamethylcyclotetrasilazane.
7. The potting adhesive of claim 1, wherein the cross-linking agent is selected from at least one of vinyltris (isopropenyloxy) silane, methyltris (isopropenyloxy) silane, and phenyltris (isopropenyloxy) silane; the diluent is glycidyl ether.
8. The potting adhesive of claim 7, wherein the glycidyl ether is selected from at least one of 1, 4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether, and o-tolyl glycidyl ether.
9. The potting adhesive of claim 1, wherein the organoguanidine catalyst is selected from at least one of 1, 1, 3, 3-tetramethylguanidinopropyltrimethoxysilane and 1, 1, 3, 3-tetramethylguanidinopropyltriethoxysilane.
10. The pouring sealant of claim 1, further comprising functional auxiliary materials: ultraviolet light stabilizer, heat stabilizer, structure control agent, silane coupling agent and defoaming agent.
11. A method for the preparation of the potting adhesive of any of claims 1 to 9, comprising the steps of:
a. cleaning and preheating vacuum mixing equipment;
b. adding hydroxyl-terminated polysiloxane, SH-MQ organic silicon resin, organic silicon modified fumed silica, organic guanidine flame retardant and heat conducting agent, stirring, heating and vacuumizing;
c. mixing, stopping stirring, heating, and storing in sealed condition;
d. adding a diluent under the protection of dry nitrogen to adjust the viscosity, cooling, and filtering by a filter screen;
e. sequentially adding a cross-linking agent and a catalyst under the protection of dry nitrogen, wherein the raw material is added after being uniformly stirred under a vacuum condition every time;
f. finally, transferring the mixture into a filling machine for extrusion and subpackage;
the preheating temperature of the step a is 50-80 ℃;
the heating temperature in the step b is 100-;
the mixing time of the step c is 1-5 h;
in the step d, the viscosity is 1000-5000mps, the temperature reduction temperature is room temperature, and the mesh number of the filter screen is 100-500 meshes;
and e, stirring for 0.5-2 h.
12. Use of the potting adhesive of any of claims 1 to 10 as an electronic potting adhesive.
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