CN116640550A - Low-density foaming silica gel and preparation method thereof - Google Patents
Low-density foaming silica gel and preparation method thereof Download PDFInfo
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- CN116640550A CN116640550A CN202211211321.7A CN202211211321A CN116640550A CN 116640550 A CN116640550 A CN 116640550A CN 202211211321 A CN202211211321 A CN 202211211321A CN 116640550 A CN116640550 A CN 116640550A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000741 silica gel Substances 0.000 title claims abstract description 34
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005187 foaming Methods 0.000 title claims abstract description 14
- 229920002545 silicone oil Polymers 0.000 claims abstract description 100
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 40
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003063 flame retardant Substances 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000003112 inhibitor Substances 0.000 claims abstract description 17
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000006260 foam Substances 0.000 claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 22
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 8
- 229940083037 simethicone Drugs 0.000 claims description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- OTJZCIYGRUNXTP-UHFFFAOYSA-N but-3-yn-1-ol Chemical compound OCCC#C OTJZCIYGRUNXTP-UHFFFAOYSA-N 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000000565 sealant Substances 0.000 abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- 238000005538 encapsulation Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229940008099 dimethicone Drugs 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920001558 organosilicon polymer Polymers 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of organic silicon pouring sealant, in particular to low-density foaming silica gel and a preparation method thereof, wherein the low-density foaming silica gel comprises a component A and a component B; the preparation raw materials of the component A at least comprise the following components in parts by weight: 1-10 parts of dimethyl silicone oil, 20-50 parts of hydroxyl-containing silicone oil A, 10-30 parts of heat conducting powder, 10-35 parts of flame retardant powder and 0.05-0.5 part of catalyst; the preparation raw materials of the component B at least comprise: 1-10 parts of dimethyl silicone oil, 30-60 parts of hydroxyl-containing silicone oil B, 5-30 parts of curing agent, 10-30 parts of heat conducting powder, 10-35 parts of flame retardant powder, 0.01-0.05 part of inhibitor and 0.01-0.1 part of foam stabilizer, so that the density of the product is effectively reduced to 0.2g/cm under the conditions of excellent low viscosity, high heat conduction, high temperature resistance and high flame retardance 3 ～0.6g/cm 3 Meets the use requirement of strict encapsulation of electronic components.
Description
Technical Field
The invention relates to the technical field of organic silicon pouring sealant, in particular to low-density foaming silica gel and a preparation method thereof.
Background
The organic silicon pouring sealant is generally composed of two components, the two components are liquid before mixing, the liquid is liquid in a short time after mixing, the liquid is low in viscosity and good in fluidity, and can be filled in a gap of a small electronic component, and after being placed for 1 hour, the two components are gradually reacted and crosslinked to become solid, so that the organic silicon pouring sealant plays a role in protecting the electronic component, and is generally used as a pouring sealing protection material between the electronic components. Along with the development of electronic appliances, large-scale integrated circuit boards and electronic components are more and more refined, lighter and higher in power, the heating value is more and more high, the service life of the electronic components is reduced due to high temperature, and the potting adhesive is required to have the properties of low viscosity, low density, high heat conduction and high temperature resistance.
The organic silicon polymer material contains a large number of silicon-oxygen bonds and has the special properties of high temperature resistance and aging resistance. At present, most of the pouring sealants on the market are prepared by adding heat conducting fillers (aluminum oxide, aluminum hydroxide and the like) into organic silicon polymer materials to increase heat conductivity, for example, chinese application patent CN112480863A discloses a preparation method of the organic silicon pouring sealant, specifically adopts dopamine modified organic silicon resin, vinyl silicone oil, aluminum oxide and white carbon black as raw materials, improves the bonding force of the organic silicon gel and electronic components to a certain extent, but the density of the produced pouring sealant is very high (generally 1.5g/cm due to the high density of the aluminum oxide and the aluminum hydroxide adopted by the pouring sealant 3 ～2.0g/cm 3 ) This results in an increase in the overall weight of the electronic device. Chinese patent CN112480864A discloses a low-density organic silicon electronic pouring sealant and a preparation method thereof, and specifically, carbon fibers are introduced into the organic silicon pouring sealant to reduce the addition of aluminum oxide and aluminum hydroxide serving as heat conducting fillers, so that the density of the provided organic silicon pouring sealant is reduced to 0.8-1.1 g/cm 3 However, the density is reduced by reducing the addition amount of the aluminum oxide and the aluminum hydroxide, and meanwhile, new carbon fibers are introduced, so that the density of the organic silicon pouring sealant cannot be effectively reduced fundamentally, and the dispersion compatibility of the carbon fibers in the pouring sealant greatly influences the thermal conductivity, the high temperature resistance and the bonding performance of the product.
Disclosure of Invention
In one aspect, the invention provides a low-density foamed silica gel, comprising a component A and a component B; the preparation raw materials of the component A at least comprise the following components in parts by weight: 1-10 parts of dimethyl silicone oil, 20-50 parts of hydroxyl-containing silicone oil A, 10-30 parts of heat conducting powder, 10-35 parts of flame retardant powder and 0.05-0.5 part of catalyst; the preparation raw materials of the component B at least comprise: 1-10 parts of dimethyl silicone oil, 30-60 parts of hydroxyl-containing silicone oil B, 5-30 parts of curing agent, 10-30 parts of heat conducting powder, 10-35 parts of flame retardant powder, 0.01-0.05 part of inhibitor and 0.01-0.1 part of foam stabilizer.
As a preferable technical scheme, the viscosity (25 ℃) of the simethicone is 50-500mpa.s; preferably, the viscosity (25 ℃) of the simethicone is 50-100mpa.s. Based on the system, the dimethyl silicone oil with the viscosity (25 ℃) of 50-100mpa.s is respectively introduced into the component A and the component B, so that the raw materials in the component A and the component B are fully mixed, the viscosity of the mixed component A and the mixed component B is in a proper range, the component A and the component B fully react, and the tensile strength of the low-density foamed silica gel is ensured. The inventors analyzed the cause may be: the dimethyl silicone oil with the viscosity (25 ℃) of 50-100mpa.s is introduced into the system, the heat conducting powder and the flame retardant powder are well dispersed in the system, the free flowing space of the dimethyl silicone oil outside the heat conducting powder and the flame retardant powder is increased, the viscosity of the mixed component A and the mixed component B is effectively reduced, and meanwhile, the component A and the component B are fully reacted, so that the tensile strength of the low-density foamed silica gel is ensured.
As a preferable technical scheme, the viscosity (25 ℃) of the hydroxyl-containing silicone oil A and the hydroxyl-containing silicone oil B is 500-20000mpa.s. Preferably, the hydroxyl-containing silicone oil A and the hydroxyl-containing silicone oil B are respectively selected from one or a combination of a plurality of hydroxyl-containing silicone oils (alpha, omega-dihydroxypolysiloxane) with the viscosity of 500mpa.s, 1000mpa.s, 2000mpa.s and 20000mpa.s. Further preferably, the hydroxyl-containing silicone oil A is a hydroxyl-containing silicone oil (alpha, omega-dihydroxypolysiloxane) having a viscosity of 500mpa.s or 1000 mpa.s; the hydroxyl-containing silicone oil B is hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with viscosity of 1000mpa.s or 2000 mpa.s.
Based on the system of the invention, hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) is respectively introduced into the component A and the component B, especially when hydroxyl silicone oil A containing hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with the viscosity of 500mpa.s or 1000mpa.s is matched with hydroxyl silicone oil B containing hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with the viscosity of 1000mpa.s or 2000mpa.s, the hydroxyl silicone oil A containing hydroxyl silicone oil and the component B react specifically with the curing agent under the action of the catalyst, and the density of the organosilicon pouring sealant is greatly reduced on the premise of not affecting the low viscosity, high heat conduction, high temperature resistance and high flame retardance of the product. The inventor analyzes that the reasons probably are that after the component A and the component B are mixed, under the action of a platinum catalyst, oxygen hydrogen bonds in hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) are broken, silicon oxygen bonds in curing agent hydrogen silicone oil are broken, two powerful hydrogens are combined into hydrogen gas in the reaction process to generate bubbles, meanwhile, the hydroxyl silicone oil A is matched with hydroxyl silicone oil B to increase the crosslinking viscosity of the hydrogen silicone oil to form a three-dimensional network structure, the generated bubbles are stably and uniformly fixed in the foaming silicone product, the foaming silicone product after full crosslinking curing reaction is in a spongy shape with certain pore distribution, the product density is effectively reduced from the material structure, and the provided low-density foaming silicone product meets the use requirement of severe electronic component encapsulation.
As a preferable technical scheme, the curing agent is hydrogen-containing silicone oil; preferably, the hydrogen content of the hydrogen-containing silicone oil is at least one of 0.1%, 0.5%, 1%, 1.3%, and 1.6%. Preferably, the hydrogen content of the hydrogen-containing silicone oil is 1.3%. Based on the hydroxyl-containing silicone oil A and the hydroxyl-containing silicone oil B introduced into the system, the hydrogen-containing silicone oil with the hydrogen content of 1.3% is introduced to realize the full crosslinking reaction during mixing, so that the product density is effectively reduced, and the comprehensive performance of the product is ensured. If the hydrogen content is too low, under a certain hydrogen-containing silicone oil dosage, the balance of a cross-linked network between the hydroxyl-containing silicone oil A and the hydroxyl-containing silicone oil B and the hydrogen-containing silicone oil is broken, the density of the product cannot be effectively reduced, and meanwhile, the mechanical property of the product is also reduced. The hydrogen content of the hydrogen-containing silicone oil in the system is too high or the addition amount is too high, so that the contact thermal resistance is increased, and the heat conducting property of the product is influenced.
As a preferable technical scheme, the heat conducting powder is at least one of aluminum oxide, boron nitride and silicon nitride. Preferably, the particle size of the heat conducting powder is 10-20 mu m.
As a preferable technical scheme, the flame retardant powder is aluminum hydroxide and/or magnesium hydroxide. Preferably, the particle size of the flame retardant powder is 10-20 mu m.
As a preferable technical scheme, the catalyst is a platinum catalyst; preferably, the platinum content in the platinum catalyst is one of 1000ppm, 3000ppm and 5000 ppm. Preferably, the platinum content in the platinum catalyst is 3000ppm.
As a preferred technical scheme, the inhibitor is at least one of methylbutynol, 1-ethynyl cyclohexanol and 3-butyn-1-ol; preferably, the inhibitor is 1-ethynyl cyclohexanol. Based on the system, the stability of the raw materials of the component B before the component A is mixed is ensured by adding the 1-ethynyl cyclohexanol as an inhibitor, and the crosslinking reaction between the component A and the component B is ensured to be sufficiently and stably carried out.
As a preferable technical scheme, the foam stabilizer is German winning DC2525 silicone oil.
In another aspect, the invention provides a method for preparing a low-density foamed silica gel, which at least comprises the following steps:
(1) Adding the raw materials except the catalyst in the component A into a planetary disperser according to parts by weight, controlling the temperature to be 80-120 ℃, stirring for 1.8-2.5 hours under the condition of 1800-2500 rpm, then cooling to 20-30 ℃, adding the catalyst, controlling the temperature to be 20-40 ℃, stirring for 0.5 hour under the condition of 300-500 rpm, and sealing and preserving to obtain the component A;
(2) Adding the raw materials except the inhibitor in the component B into a planetary disperser according to parts by weight, controlling the temperature to be 80-120 ℃, stirring for 1.8-2.5 hours under the condition of 1800-2500 rpm, then cooling to 20-30 ℃, adding the inhibitor, controlling the temperature to be 20-40 ℃, stirring for 0.5 hour under the condition of 300-500 rpm, and hermetically preserving;
(3) When in use, the component A and the component B are mixed and stirred uniformly at the temperature of 25-30 ℃, and then are kept stand for 15-30 minutes at the temperature of 25-30 ℃ to obtain the composite material.
As a preferable technical scheme, the mass ratio of the component A to the component B in the step (3) is 1:1.
Advantageous effects
1. The invention provides a low-density foaming silica gel, which adopts specific hydrogen-containing silicone oil and hydroxyl-containing silicone oil to ensure that the density of the product is effectively reduced to 0.2g/cm under the conditions of excellent low viscosity, high heat conduction, high temperature resistance and high flame retardance 3 ～0.6g/cm 3 Meets the use requirement of strict encapsulation of electronic components.
2. Based on the system, the dimethyl silicone oil with the viscosity (25 ℃) of 50-100mpa.s is respectively introduced into the component A and the component B, so that the raw materials in the component A and the component B are fully mixed, the viscosity of the mixed component A and the mixed component B is in a proper range, the component A and the component B fully react, and the tensile strength of the low-density foamed silica gel is ensured.
3. Based on the system of the invention, hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) is respectively introduced into the component A and the component B, especially when hydroxyl silicone oil A containing hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with the viscosity of 500mpa.s or 1000mpa.s is matched with hydroxyl silicone oil B containing hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with the viscosity of 1000mpa.s or 2000mpa.s, the hydroxyl silicone oil A containing hydroxyl silicone oil and the component B react specifically with the curing agent under the action of the catalyst, and the density of the organosilicon pouring sealant is greatly reduced on the premise of not affecting the low viscosity, high heat conduction, high temperature resistance and high flame retardance of the product.
4. Based on the hydroxyl-containing silicone oil A and the hydroxyl-containing silicone oil B introduced into the system, the hydrogen-containing silicone oil with the hydrogen content of 1.3% is introduced to realize the full crosslinking reaction during mixing, so that the product density is effectively reduced, and the comprehensive performance of the product is ensured.
Drawings
FIG. 1 is a diagram of an actual low-density foamed silica gel product prepared in example 1 of the present invention.
Detailed Description
Example 1
Referring to fig. 1, in one aspect, example 1 of the present invention provides a low density foamed silica gel comprising component a and component B; the preparation raw materials of the component A are as follows in parts by weight: 10 parts of dimethyl silicone oil, 40 parts of hydroxyl-containing silicone oil A, 20 parts of heat conducting powder, 29.5 parts of flame retardant powder and 0.5 part of catalyst; the preparation raw materials of the component B comprise 5 parts of dimethyl silicone oil, 40 parts of hydroxyl-containing silicone oil B, 25 parts of curing agent, 10 parts of heat conducting powder, 20 parts of flame retardant powder, 0.01 part of inhibitor and 0.05 part of foam stabilizer.
The viscosity (25 ℃) of the dimethicone was 50mpa.s. The model number of the simethicone is 201-50, and the simethicone is from Shanghai Chu Yijia organosilicon materials Co.
The hydroxyl-containing silicone oil A is hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with viscosity of 1000mpa.s (25 ℃), the model is V1000, and the hydroxyl-containing silicone oil A is from Anhui Ai Yaoda silicone oil Co., ltd; the hydroxyl-containing silicone oil B is hydroxyl silicone oil (alpha, omega-dihydroxypolysiloxane) with the viscosity of 2000mpa.s (25 ℃), the model is V2000, and the hydroxyl-containing silicone oil B is from Anhui Ai Yaoda silicone oil Co.
The curing agent is hydrogen-containing silicone oil; the hydrogen content of the hydrogen-containing silicone oil is 1.3%, and the hydrogen-containing silicone oil is from Shandong Dayi chemical industry limited company.
The heat conducting powder is alumina. The particle size of the heat conducting powder is 10 mu m, the model is Brofos-AlO3-W10, and the heat conducting powder is from BoHuasi nanotechnology (Ningbo) Co.
As a preferable technical scheme, the flame retardant powder is aluminum hydroxide. The grain diameter of the flame retardant powder is 10 mu m, and the flame retardant powder is from the Hefeizhong flame retardant new material Co.
The catalyst is a platinum catalyst; the platinum catalyst has a platinum content of 3000ppm and is derived from Anhui Ai Yaoda silicone oil Co.
The inhibitor is 1-ethynyl cyclohexanol.
The foam stabilizer is Germany winning DC2525 silicone oil.
In another aspect, embodiment 1 of the present invention provides a method for preparing a low-density foamed silica gel, comprising the steps of:
(1) Adding the raw materials except the catalyst in the component A into a planetary disperser according to parts by weight, controlling the temperature to be 100 ℃, stirring for 2 hours under the condition of 2000 revolutions per minute, then cooling to 25 ℃, adding the catalyst, controlling the temperature to be 30 ℃, stirring for 0.5 hour under the condition of 400 revolutions per minute, and hermetically preserving to obtain the component A;
(2) Adding the raw materials except the inhibitor in the component B into a planetary disperser according to parts by weight, controlling the temperature to be 100 ℃, stirring for 2 hours under the condition of 2000 revolutions per minute, then cooling to 25 ℃, adding the inhibitor, controlling the temperature to be 30 ℃, stirring for 0.5 hour under the condition of 400 revolutions per minute, and sealing for preservation;
(3) When in use, the component A and the component B are mixed and stirred uniformly at 25 ℃, and then are kept stand at 25 ℃ for 20 minutes, thus obtaining the composite material.
And in the step (3), the mass ratio of the component A to the component B is 1:1.
Example 2
The embodiment 2 of the invention provides a low-density foaming silica gel and a preparation method thereof, wherein the low-density foaming silica gel comprises a component A and a component B; the specific embodiment is the same as in example 1, except that the preparation raw materials of the component A are as follows in parts by weight: 10 parts of dimethyl silicone oil, 50 parts of hydroxyl-containing silicone oil A, 15 parts of heat conducting powder, 29.5 parts of flame retardant powder and 0.5 part of catalyst; the preparation raw materials of the component B comprise 5 parts of dimethyl silicone oil, 50 parts of hydroxyl-containing silicone oil B, 30 parts of curing agent, 10 parts of heat conducting powder, 20 parts of flame retardant powder, 0.01 part of inhibitor and 0.05 part of foam stabilizer. The viscosity (25 ℃) of the dimethicone was 100mpa.s. The model number of the simethicone is 201-100, and the simethicone is from Shanghai Chu Yijia organosilicon materials Co.
Example 3
The embodiment 3 of the invention provides a low-density foaming silica gel and a preparation method thereof, wherein the low-density foaming silica gel comprises a component A and a component B; the specific embodiment is the same as in example 1, except that the preparation raw materials of the component A are as follows in parts by weight: 5 parts of dimethyl silicone oil, 30 parts of hydroxyl-containing silicone oil A, 18 parts of heat conducting powder, 29.5 parts of flame retardant powder and 0.5 part of catalyst; the preparation raw materials of the component B comprise 5 parts of dimethyl silicone oil, 50 parts of hydroxyl-containing silicone oil B, 25 parts of curing agent, 10 parts of heat conducting powder, 20 parts of flame retardant powder, 0.01 part of inhibitor and 0.05 part of foam stabilizer.
Comparative example 1
Comparative example 1 of the present invention provides a low density foamed silica gel and a method for preparing the same, and a specific embodiment thereof is the same as example 1, except that the simethicone has a model number of 201-1000 and is derived from Shanghai Chu Yijia organosilicon materials Co.
Comparative example 2
Comparative example 2 of the present invention provides a low density foamed silica gel, the specific embodiment of which is the same as example 1, except that the hydroxyl-containing silicone oil a is a hydroxyl-containing silicone oil (α, ω -dihydroxypolysiloxane) having a viscosity (25 ℃) of 3000mpa.s, model V3000, from the company anhui Ai Yaoda silicone oil limited; the hydroxyl-containing silicone oil B is hydroxyl-containing silicone oil (alpha, omega-dihydroxypolysiloxane) with the viscosity (25 ℃) of 3000mpa.s, and the model is V3000.
Comparative example 3
Comparative example 3 of the present invention provides a low density foamed silica gel, which is different from example 1 in that the hydrogen content of the hydrogen-containing silicone oil is 0.5%, which is obtained from Shanghai Chu Yijia silicone materials Co., ltd.
Performance test method
Performance test method
(1) The viscosities of the components A and B in the examples and comparative examples after mixing were measured at 25℃using a viscometer, and the results are shown in Table 1.
(2) The thermal conductivity of the low density foamed silica gels obtained in the examples and comparative examples of the present invention was measured with reference to the standard ASTM D5470-2001, and the results are shown in Table 1.
(3) The densities of the low-density foamed silica gels obtained in the examples and comparative examples of the present invention were measured with reference to the national standard GB/T533-1991, and the results are shown in Table 1.
(4) The hardness of the low density foamed silica gel obtained in the examples and comparative examples of the present invention was measured by using a durometer with reference to the standard ASTM D2240-2015, and the results are shown in Table 1.
(5) The flame retardant rating of the low density foamed silica gel obtained in examples and comparative examples of the present invention was measured with reference to the standard UL-94, and the results are shown in table 1.
(6) The tensile strength of the low density foamed silica gel obtained in examples and comparative examples of the present invention was measured with reference to national standard GB/T6344-2008, and the results are shown in Table 1.
TABLE 1,
Claims (10)
1. The low-density foaming silica gel is characterized by comprising a component A and a component B; the preparation raw materials of the component A at least comprise the following components in parts by weight: 1-10 parts of dimethyl silicone oil, 20-50 parts of hydroxyl-containing silicone oil A, 10-30 parts of heat conducting powder, 10-35 parts of flame retardant powder and 0.05-0.5 part of catalyst; the preparation raw materials of the component B at least comprise: 1-10 parts of dimethyl silicone oil, 30-60 parts of hydroxyl-containing silicone oil B, 5-30 parts of curing agent, 10-30 parts of heat conducting powder, 10-35 parts of flame retardant powder, 0.01-0.05 part of inhibitor and 0.01-0.1 part of foam stabilizer.
2. The low density foamed silica gel according to claim 1, wherein said simethicone has a viscosity of 50-500mpa.s.
3. The low-density foamed silica gel according to claim 1, wherein the viscosity of the hydroxyl-containing silicone oil a and the hydroxyl-containing silicone oil B is 500 to 20000mpa.s.
4. A low density foamed silica gel according to claim 3 wherein said hydroxyl-containing silicone oil a, hydroxyl-containing silicone oil B is selected from the group consisting of one or more of hydroxyl-containing silicone oils (α, ω -dihydroxypolysiloxanes) having a viscosity of 500mpa.s, 1000mpa.s, 2000mpa.s, 20000mpa.s, respectively.
5. The low-density foamed silica gel according to claim 4, wherein the curing agent is hydrogen-containing silicone oil; the hydrogen content of the hydrogen-containing silicone oil is at least one of 0.1%, 0.5%, 1%, 1.3% and 1.6%.
6. The low-density foamed silica gel according to claim 5, wherein the heat conductive powder is at least one of aluminum oxide, boron nitride, and silicon nitride.
7. The low-density foamed silica gel according to claim 6, wherein the flame retardant powder is aluminum hydroxide and/or magnesium hydroxide.
8. The low density foamed silica gel according to claim 7, wherein the catalyst is a platinum catalyst, and the platinum content in the platinum catalyst is one of 1000ppm, 3000ppm, and 5000 ppm.
9. The low density foamed silica gel according to claim 8, wherein said inhibitor is at least one of methylbutynol, 1-ethynyl cyclohexanol, 3-butyn-1-ol.
10. A method for preparing a low density foamed silica gel according to any one of claims 1 to 9, comprising at least the steps of:
(1) Adding the raw materials except the catalyst in the component A into a planetary disperser according to parts by weight, controlling the temperature to be 80-120 ℃, stirring for 1.8-2.5 hours under the condition of 1800-2500 rpm, then cooling to 20-30 ℃, adding the catalyst, controlling the temperature to be 20-40 ℃, stirring for 0.5 hour under the condition of 300-500 rpm, and sealing and preserving to obtain the component A;
(2) Adding the raw materials except the inhibitor in the component B into a planetary disperser according to parts by weight, controlling the temperature to be 80-120 ℃, stirring for 1.8-2.5 hours under the condition of 1800-2500 rpm, then cooling to 20-30 ℃, adding the inhibitor, controlling the temperature to be 20-40 ℃, stirring for 0.5 hour under the condition of 300-500 rpm, and hermetically preserving;
(3) When in use, the component A and the component B are mixed and stirred uniformly at the temperature of 25-30 ℃, and then are kept stand for 15-30 minutes at the temperature of 25-30 ℃ to obtain the composite material.
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