CN112322048A - Organic silicon gel composition and preparation method and application thereof - Google Patents
Organic silicon gel composition and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a silicone gel composition, which comprises the following components in percentage by mass: (0.8-1.2) component A and component B; the component A comprises: 96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups; 0.5-2 parts of toughening and softening agent; 0.01-0.1 part by weight of a metal catalyst; the component B comprises: 78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups; 8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms; 0.01-0.1 parts by weight of a gel curing inhibitor; 0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent; the transparent high-temperature-resistant auxiliary agent is selected from one or more of a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound. Compared with the prior art, the organic silicon gel composition provided by the invention adopts specific content components, realizes better interaction, and obtains a high-transparency high-temperature-resistant organic silicon gel composition; the product has higher high-transparency high-temperature resistance than the conventional silica gel.
Description
Technical Field
The invention relates to the technical field of low-hardness silicone gel compositions, in particular to an organic silicone gel composition and a preparation method and application thereof.
Background
The IGBT module generally comprises a red copper base plate, a heat-conducting insulating ceramic copper-clad plate, a chip, a connecting guide beam, an electrode, a control terminal, a PBT plastic shell and an organic silicon soft gel layer. The high-temperature-resistant silica gel has excellent temperature resistance, can be used for a long time at-60 ℃ to +250 ℃, has waterproof, moistureproof and electric insulating properties, and is an indispensable packaging material for electronic devices. The soft silica gel is a material used in the most widely applied packaging process, and the power semiconductor packaging process will develop towards more excellent high-transparency high-heat-resistance and high-adhesion silica gel packaging.
The IGBT module and the circuit board electronic module for the electric automobile and the high-speed rail are easy to generate heat in the long-term working process, the local high temperature can exceed 250 ℃, and the semiconductor module can generate an aging effect on common gel in the long-term high-temperature working state; therefore, the high-temperature resistant gel is adopted, the limitation that the module works in a high-temperature state can be effectively solved, the high-temperature service time of the module is effectively prolonged, and the failure of the module is reduced.
Disclosure of Invention
In view of the above, the present invention provides a silicone gel composition and a preparation method thereof, and the silicone gel composition provided by the present invention has excellent high temperature resistance and high light transmittance.
The invention provides a silicone gel composition, which comprises the following components in percentage by mass: (0.8-1.2) component A and component B;
the component A comprises:
96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups;
0.5-2 parts of toughening and softening agent;
0.01-0.1 part by weight of a metal catalyst;
the component B comprises:
78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups;
8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms;
0.01-0.1 parts by weight of a gel curing inhibitor;
0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent;
the transparent high-temperature-resistant auxiliary agent is selected from one or more of a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound.
Preferably, the compound containing at least two aliphatic unsaturation is an organosilicon compound containing at least two aliphatic unsaturation;
the base unit of the organosilicon compound containing at least two aliphatic unsaturation has the general formula shown in formula (I):
RaR1 bSiO(4-a-b)/2formula (I);
in the formula (I), R is selected from organic groups without aliphatic carbon-carbon multiple bonds; r1Selected from the group consisting of monovalent unsubstituted or substituted, SiC-bonded hydrocarbon radicals having aliphatic carbon-carbon multiple bonds;
a is more than or equal to 0 and less than or equal to 3, b is more than or equal to 0 and less than or equal to 2, and a + b is less than or equal to 3.
Preferably, the toughening and softening agent is selected from single-ended vinyl polysiloxane and/or vinyl trimethylsilane.
Preferably, the compound comprising at least two aliphatic unsaturation has a kinematic viscosity at 25 ℃ of 102～105mPa.s; the dynamic viscosity of the toughening and softening agent at 25 ℃ is 0.01-300 mPa.s.
Preferably, the metal catalyst is selected from one or more of a platinum catalyst, a rhodium catalyst and a palladium catalyst.
Preferably, the basic unit of the organopolysiloxane having silicon-bonded hydrogen atoms has the general formula shown in formula (II):
R2 cHdSiO(4-c-d)/2formula (II);
in the formula (II), R2Selected from organic radicals free of aliphatic carbon-carbon multiple bonds;
c is more than or equal to 0 and less than or equal to 3, d is more than or equal to 0 and less than or equal to 2, and c + d is less than or equal to 3.
Preferably, the gel-curing inhibitor is selected from one or more of an alkenyl-containing organosiloxane compound, an alkynyl-containing organosiloxane compound, an alkynol, cumene hydroperoxide, an organic peroxide, an organic sulfone, an organic amine, an amide, a phosphate, a nitrile, and a diaziridine.
Preferably, the component a or the component B further comprises:
0.1-5 parts by weight of a polysiloxane reinforcing agent;
the polysiloxane reinforcing agent has a general formula of a basic unit shown in formula (III):
R3 pR4 q[SiO]zformula (III);
in the formula (III), R3Selected from methyl or phenyl; r4Selected from vinyl or silicon hydride;
0.6≤p≤0.9，0＜q≤0.1，z＝1。
the invention also provides a preparation method of the organic silicon gel composition, which comprises the following steps:
a) adding a toughening softening agent and a metal catalyst into a compound containing at least two aliphatic unsaturated groups, and uniformly stirring to obtain a component A;
b) uniformly mixing a compound containing at least two aliphatic unsaturated groups, organopolysiloxane with silicon-bonded hydrogen atoms, a gel curing inhibitor and a transparent high-temperature-resistant auxiliary agent at room temperature to obtain a component B;
c) mixing the component A and the component B according to the mass ratio of 1: (0.8-1.2) uniformly mixing to obtain an organic silicon gel composition;
the step a) and the step b) are not limited in order.
The invention also provides a using method of the organic silicon gel composition, which comprises the following steps:
mixing the component A and the component B according to the mass ratio of 1: (0.8-1.2), and then drying for 13-16 min at 110-130 ℃ for full curing.
The invention provides a silicone gel composition, which comprises the following components in percentage by mass: (0.8-1.2) component A and component B; the component A comprises: 96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups; 0.5-2 parts of toughening and softening agent; 0.01-0.1 part by weight of a metal catalyst; the component B comprises: 78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups; 8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms; 0.01-0.1 parts by weight of a gel curing inhibitor; 0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent; the transparent high-temperature-resistant auxiliary agent is selected from one or more of a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound. Compared with the prior art, the organic silicon gel composition provided by the invention adopts specific content components, realizes better interaction, and obtains a high-transparency high-temperature-resistant organic silicon gel composition; the product has higher high-transparency high-temperature resistance than the conventional silica gel. Experimental results show that the penetration degree of the organic silicon gel composition is 360-380 mm/10 after the organic silicon gel composition is cured at the temperature of 120 ℃ for 15min, and the penetration degree is 260-300 mm/10 after the organic silicon gel composition is baked at the temperature of 250 ℃ for 300 h; the UV-VIS transmittance is 99 percent; the high temperature resistance can reach 250 ℃ multiplied by 500h, the colloid is not brittle and does not crack; the adhesive shear force is 3.3 to 3.5Kgf/cm2(ii) a Therefore, the silicon gel has lower hardness, higher light transmittance, higher high-temperature resistance for a longer time than common silicon gel, and stronger bonding and stretching force.
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application; meanwhile, the use method of the organic silicon gel composition provided by the invention is simple and easy to control, is suitable for being used in various working condition environments, and has a wide application prospect.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a silicone gel composition, which comprises the following components in percentage by mass: (0.8-1.2) component A and component B;
the component A comprises:
96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups;
0.5-2 parts of toughening and softening agent;
0.01-0.1 part by weight of a metal catalyst;
the component B comprises:
78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups;
8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms;
0.01-0.1 parts by weight of a gel curing inhibitor;
0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent;
the transparent high-temperature-resistant auxiliary agent is selected from one or more of a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound.
In the present invention, the silicone gel composition includes, by mass, 1: (0.8-1.2), preferably, the component A and the component B are prepared from the following components in a mass ratio of 1: (0.8-1.2), and more preferably, the component A and the component B are mixed in a mass ratio of 1: 1, component A and component B.
In the present invention, the a component is an organopolysiloxane composition comprising:
96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups;
0.5-2 parts of toughening and softening agent;
0.01-0.1 part by weight of a metal catalyst;
preferably comprising:
96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups;
0.5-2 parts of toughening and softening agent;
0.05 part by weight of a metal catalyst.
In the present invention, the component a preferably further includes:
0.1-5 parts by weight of a polysiloxane reinforcing agent;
more preferably, the method further comprises:
2 parts by weight of polysiloxane reinforcing agent.
In the present invention, the compound containing at least two aliphatic unsaturated groups is preferably an organosilicon compound containing at least two aliphatic unsaturated groups, more preferably a linear organosilicon compound containing at least two aliphatic unsaturated groups. In the present invention, the basic unit of the organosilicon compound containing at least two aliphatic unsaturated groups preferably has the general formula shown in formula (I):
RaR1 bSiO(4-a-b)/2formula (I);
in formula (I), R is preferably selected from organic radicals which do not contain aliphatic carbon-carbon multiple bonds, more preferably from monovalent, SiC-bonded, unsubstituted or substituted hydrocarbon radicals having from C1 to C18 carbon atoms and which do not contain carbon-carbon multiple bonds; r1Preferably selected from monovalent unsubstituted or substituted, SiC-bonded hydrocarbon radicals having aliphatic carbon-carbon multiple bonds, more preferably from C2-C10 alkylene radicals or C2-C10 alkynylene radicals; a is more than or equal to 0 and less than or equal to 3, b is more than or equal to 0 and less than or equal to 2, and a + b is less than or equal to 3.
In the invention, R is selected from organic radicals without aliphatic carbon-carbon multiple bonds, preferably selected from monovalent organic radicals without aliphatic carbon-carbon multiple reconstruction; the monovalent organic radicals which are free of aliphatic carbon-carbon multiple reconstruction are preferably selected from the group consisting of-F, -Cl, -CN, -SCN, -NCO groups, SiC-bonded unsubstituted hydrocarbon radicals or SiC-bonded substituted hydrocarbon radicals; the monovalent organic groups not containing aliphatic carbon-carbon multiple reconstruction are more preferably selected from monovalent, SiC-bonded unsubstituted or substituted C1-C18 hydrocarbon groups; if monovalent, SiC-bonded substituted C1-C18 hydrocarbon radicals, where the substituents are preferably selected from halogen atoms, phosphorus-containing groups, cyano groups; most preferably selected from monovalent, SiC-bonded unsubstituted or substituted C1-C6 hydrocarbon groups; the SiC-bonded unsubstituted hydrocarbon groups are preferably selected from saturated alkyl groups; the saturated alkyl group is preferably selected from methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, n-butyl, isobutyl, isopentane, neopentyl, tert-pentyl, hexyl, heptyl, octyl, nonyl, decylphenyl or tolyl, more preferably from methyl or phenyl. In the present invention, the compound containing at least two aliphatic unsaturated groups preferably further includes one or more of 1,3, 5-trivinylcyclohexane, 2, 3-dimethyl-1, 3-butadiene, 2-methyl-1, 3-butadiene, 1, 5-hexadiene, 1, 7-octadiene, 1, 4-divinylcyclohexane, 1,3, 5-triallylbenzene, vinyl-containing polybutadiene, 1,2, 4-trivinylcyclohexane, 1,3, 5-tripropylene benzene, 1, 4-divinylbenzene, 3-methyl-1, 5-heptadiene, and triphenyl-1, 5-hexadiene.
In the present invention, said R1Selected from monovalent unsubstituted or substituted, SiC-bonded hydrocarbon radicals having aliphatic carbon-carbon multiple bonds, more preferably from C2-C10 alkenes or C2-C10 alkynes; specifically, the R is1Selected from the group consisting of vinyl, propenyl, allyl, 1-propenyl, ethynyl, butadienyl, ethenyl, vinylphenyl or styryl. In the present invention, the organosilicon compound containing at least two aliphatic unsaturated groups contains an average of at least 2R per molecule1A group.
In the present invention, the molecular weight of the organosilicon compound containing at least two aliphatic unsaturated groups is preferably 102～105g/mol; component A which is prepared may be an alkenylpolysiloxane of relatively low molecular weight, or may be a highly polymerized polydimethylsiloxane having silicon-bonded vinyl groups in the chain or at the ends of the chain, the structure of the oligomeric or highly polymerized siloxane being linear, cyclic, branched or resin-like or network-like; the linear or cyclic polysiloxane is mainly represented by the formula R3SiO1/2、R1R2SiO1/2、R1R1SiO2/2And R2SiO2/2The unit composition of (a); branched or network-like polysiloxanes also comprising trifunctional or tetrafunctional units, e.g. RSiO3/2、R1SiO3/2、SiO4/2。
In a preferred embodiment of the invention, the compound comprising at least two aliphatic unsaturation is a vinyl terminated Polydimethylsiloxane (PDMS) or a vinyl silicone oil.
In the present invention, the compound containing at least two aliphatic unsaturated groups preferably has a kinematic viscosity at 25 ℃ of 102～105mpa.s, more preferably 1000 mpa.s.
In the present invention, the toughening softener is preferably selected from single-terminal vinyl polysiloxane and/or vinyl trimethylsilane, more preferably single-terminal vinyl polysiloxane or vinyl trimethylsilane. The source of the toughening softener is not particularly limited in the present invention, and commercially available products of the above-mentioned single-terminal vinyl polysiloxane and vinyltrimethylsilane known to those skilled in the art may be used.
In the invention, due to the linear chain monofunctional property of the single-end vinyl polymethylsiloxane structure, the curable organopolysiloxane composition is endowed with remarkable effect, not only can the functional group with a vinyl group and hydrogen-containing polysiloxane undergo hydrosilylation reaction, but also the other end of the pendant chain end which does not participate in the hydrosilylation reaction can play a role in increasing toughness, reducing the flexibility of the organopolysiloxane composition and increasing the surface viscosity of the composition. In the invention, the dynamic viscosity of the toughening and softening agent at 25 ℃ is preferably 0.01-300 mPa.s, and more preferably 100 mPa.s.
In the present invention, the metal catalyst is preferably selected from one or more of a platinum catalyst, a rhodium catalyst and a palladium catalyst, and more preferably a platinum catalyst; the platinum catalyst is compatible with polyorganosiloxanes. The source of the metal catalyst is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art may be used.
In the present invention, the platinum catalyst is preferably selected from platinum, platinum-olefin complexes, platinum-cyclopropane complexes ((PtCl)2C3H6)2) One or more of a platinum-vinylsiloxane complex, a reaction product of hexachloroplatinic acid and an alcohol, a reaction product of hexachloroplatinic acid and an ether, a reaction product of hexachloroplatinic acid and an aldehyde, a complex of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane and platinum, and a complex of 1,3,5, 7-tetravinyl-1, 3,5, 7-tetramethylcyclosiloxane and platinum; wherein, the olefin in the platinum-olefin complex is preferably selected from linear olefins of C2-C6 or cycloolefins of C5-C7, and the linear olefins of C2-C6 are preferably ethylene or propylene; the cycloolefine of C5-C7 is preferably cyclopentene, cyclohexene or cycloheptene; the platinum in the platinum-olefin complex is preferably PtCl. In a preferred embodiment of the present invention, the metal catalyst is a complex of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane and platinum (prepared from platinum and divinyltetramethyldisiloxane), a complex of 1,3,5, 7-tetravinyl-1, 3,5, 7-tetramethylcyclotetrasiloxane and platinum, a platinum-cyclopentene complex or a platinum-cyclohexene complex (a reaction product of hexachloroplatinic acid and methylvinyltetrasiloxane in the presence of sodium bicarbonate in an ethanol solution).
In the present invention, the platinum content in the platinum catalyst is preferably 0.1 wt% to 0.5 wt%, more preferably 0.3 wt%.
In the present invention, the base unit of the polysiloxane reinforcing agent preferably has a general formula represented by formula (III):
R3 pR4 q[SiO]zformula (III);
in the formula (III), R3Preferably selected from methyl or phenyl; r4Preferably selected from vinyl or silicon hydride groups; p is more than or equal to 0.6 and less than or equal to 0.9, q is more than 0 and less than or equal to 0.1, and z is equal to 1. In the present invention, R is as defined above3 pAnd/or R4 qDenoted as M, [ SiO ]]zDenoted as Q. In a preferred embodiment of the present invention, the silicone reinforcing agent in component a is a vinyl MQ silicone resin.
In the present invention, the B component is an organopolysiloxane composition comprising:
78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups;
8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms;
0.01-0.1 parts by weight of a gel curing inhibitor;
0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent;
preferably comprising:
78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups;
8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms;
0.03-0.04 parts by weight of a gel curing inhibitor;
1-2 parts of transparent high-temperature-resistant auxiliary agent.
In the present invention, the component B preferably further comprises:
0.1-5 parts by weight of a polysiloxane reinforcing agent;
more preferably, the method further comprises:
2 parts by weight of polysiloxane reinforcing agent.
In the present invention, the compound containing at least two aliphatic unsaturated groups is preferably an organosilicon compound containing at least two aliphatic unsaturated groups, more preferably a linear organosilicon compound containing at least two aliphatic unsaturated groups. In the present invention, the basic unit of the organosilicon compound containing at least two aliphatic unsaturated groups preferably has the general formula shown in formula (I):
RaR1 bSiO(4-a-b)/2formula (I);
in formula (I), R is preferably selected from organic radicals which do not contain aliphatic carbon-carbon multiple bonds, more preferably from monovalent, SiC-bonded, unsubstituted or substituted hydrocarbon radicals having from C1 to C18 carbon atoms and which do not contain carbon-carbon multiple bonds; r1Preferably selected from monovalent unsubstituted or substituted, SiC-bonded hydrocarbon radicals having aliphatic carbon-carbon multiple bonds, more preferably from C2-C10 alkylene radicals or C2-C10 alkynylene radicals; a is more than or equal to 0 and less than or equal to 3, b is more than or equal to 0 and less than or equal to 2, and a + b is less than or equal to 3.
In the present invention, the compound containing at least two aliphatic unsaturated groups in component B and the compound containing at least two aliphatic unsaturated groups in component a are in the same range of species, and may or may not be the same when selecting the specific species.
In a preferred embodiment of the invention, the compound comprising at least two aliphatic unsaturation is a vinyl terminated Polydimethylsiloxane (PDMS).
In the present invention, the compound containing at least two aliphatic unsaturated groups preferably has a kinematic viscosity at 25 ℃ of 102～105mpa.s, more preferably 1000 mpa.s.
In the present invention, the basic unit of the organopolysiloxane having silicon-bonded hydrogen atoms preferably has a general formula shown in formula (II):
R2 cHdSiO(4-c-d)/2formula (II);
in the formula (II), R2Preferably selected from organic radicals which do not contain aliphatic carbon-carbon multiple bonds, in accordance with the selection range of R, which is not described in detail herein2When R is specifically selected from the group consisting of the same or different groups; c is more than or equal to 0 and less than or equal to 3, d is more than or equal to 0 and less than or equal to 2, and c + d is less than or equal to 3.
In the present invention, the molecular weight of the organopolysiloxane having silicon-bonded hydrogen atoms is preferably 102～105g/mol; the organopolysiloxane having silicon-bonded hydrogen atoms may be a relatively low molecular weight SiH-functional oligosiloxane, such as tetramethyldisiloxane, but also a highly polymerized polydimethylsiloxane having SiH groups in the chain or at the ends, or a silicone resin having SiH groups; the structure constituting the organopolysiloxane having silicon-bonded hydrogen atoms may be a linear, cyclic, branched, dendritic-like or net-like structure; linear and cyclic organopolysiloxanes having silicon-bonded hydrogen atoms are preferably of the formula R23SiO1/2、HR2 2SiO1/2Or R2 2SiO2/2The unit composition of (a); the branched or network-like organopolysiloxanes having silicon-bonded hydrogen atoms also comprise trifunctionalOr tetrafunctional units, it being of course also possible to use different siloxane mixtures which meet the criteria for properties after curing. In the present invention, in the case of the present invention,
in the present invention, the organopolysiloxane having silicon-bonded hydrogen atoms has a structure comprising an SiH group and an aliphatic unsaturated group R2Wherein the SiH/Sivi molar ratio is (0.4-20): 1, the organopolysiloxane composition can have stable penetration performance after being cured.
In the present invention, the organosilicon compound containing at least two aliphatic unsaturated groups contains an average of at least 2 silicon-bonded hydrogen atoms per molecule. In the present invention, the hydrogen content of the organopolysiloxane having silicon-bonded hydrogen atoms is preferably 0.01 to 1.6 wt%, more preferably 0.4 wt%; the organopolysiloxane having silicon-bonded hydrogen atoms preferably has a dynamic viscosity of 1 to 100mPa.s, more preferably 4 to 80mPa.s, at 25 ℃.
In a preferred embodiment of the invention, the organopolysiloxane having silicon-bonded hydrogen atoms is a polydimethylsiloxane, a hydrogen-terminated polydimethylsiloxane or a terminal side chain hydrogen-containing polymethylhydrosiloxane.
In the present invention, the gel curing inhibitor is preferably selected from one or more of an alkenyl-containing organosiloxane compound, an alkynyl-containing organosiloxane compound, an alkynol, cumene hydroperoxide, an organic peroxide, an organic sulfone, an organic amine, an amide, a phosphate, a nitrile, and diaziridine; the alkynol is preferably selected from one or more of 1-ethynyl-1-cyclohexanol, 2-methyl-3-butyn-2-ol and 3, 5-dimethyl-1-hexyn-3-ol; the alkenyl-containing organosiloxane compound is preferably selected from polymethylvinylcyclosiloxanes; the methylvinylcyclosiloxane is preferably 1,3,5, 7-tetravinyltetramethylcyclosiloxane, divinyltetramethyldisiloxane or tetravinyldimethyldisiloxane. The source of the gel curing inhibitor is not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used.
In the present invention, the gel curing inhibitor can adjust the working time, the initial temperature and the crosslinking speed of the composition. In a preferred embodiment of the invention, the gel-curing inhibitor is 1,3,5, 7-tetravinyltetramethylcyclosiloxane, ethynylcyclohexanol, or an alkynyl-containing polysiloxane.
In the present invention, the transparent high temperature resistant auxiliary is one or more selected from a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound, and more preferably a cerium-containing compound or a neodymium-containing compound. In the present invention, the compound includes an acetic acid compound and a silicon polymer; on the basis, the cerium-containing compound can be cerium acetate or a cerium-containing compound in a silicon polymer; the praseodymium-containing compound can be cerium acetate or a praseodymium-containing compound in a silicon polymer, and the neodymium-containing compound can be neodymium acetate or a neodymium-containing compound in a silicon polymer. The source of the transparent high temperature resistant auxiliary agent is not particularly limited in the present invention, and commercially available products well known to those skilled in the art can be used. The compound containing the specific rare earth element is added, the compound is a transparent compound, and a product obtained after the compound is added into gel has low hardness, high light transmittance and excellent high temperature resistance, is particularly not hardened and cracked after being baked at the high temperature of 250 ℃ for 500 hours for a long time, and can protect a microelectronic device from normal operation under the high temperature condition.
In the present invention, the base unit of the polysiloxane reinforcing agent preferably has a general formula represented by formula (III):
R3 pR4 q[SiO]zformula (III);
in the formula (III), R3Preferably selected from methyl or phenyl; r4Preferably selected from vinyl or silicon hydride groups; p is more than or equal to 0.6 and less than or equal to 0.9, q is more than 0 and less than or equal to 0.1, and z is equal to 1. In a preferred embodiment of the present invention, the polysiloxane reinforcing agent in component B is a polymonovinylpolysiloxane.
The organic silicon gel composition provided by the invention adopts specific content components, realizes better interaction, and obtains a high-transparency high-temperature-resistant organic silicon gel composition; the product has higher high-transparency high-temperature resistance than the conventional silicone gel, thereby solving the current situations that the conventional silicone gel becomes hard and the colloid cracks after being baked for 100 hours at 220 ℃ and the technical problems that the conventional high-temperature resistant silicone gel is opaque.
The invention also provides a preparation method of the organic silicon gel composition, which comprises the following steps:
a) adding a toughening softening agent and a metal catalyst into a compound containing at least two aliphatic unsaturated groups, and uniformly stirring to obtain a component A;
b) uniformly mixing a compound containing at least two aliphatic unsaturated groups, organopolysiloxane with silicon-bonded hydrogen atoms, a gel curing inhibitor and a transparent high-temperature-resistant auxiliary agent at room temperature to obtain a component B;
c) mixing the component A and the component B according to the mass ratio of 1: (0.8-1.2) uniformly mixing to obtain an organic silicon gel composition;
the step a) and the step b) are not limited in order.
Firstly, adding a toughening softening agent and a metal catalyst into a compound containing at least two aliphatic unsaturated groups, and uniformly stirring to obtain a component A;
and simultaneously, uniformly mixing a compound containing at least two aliphatic unsaturated groups, organopolysiloxane with silicon-bonded hydrogen atoms, a gel curing inhibitor and a transparent high-temperature-resistant auxiliary agent at room temperature to obtain a component B.
In the present invention, the compound containing at least two aliphatic unsaturated groups, the toughening softener, the metal catalyst, the organopolysiloxane having a silicon-bonded hydrogen atom, the gel curing inhibitor, and the transparent high temperature resistant auxiliary are the same as those in the above technical solution, and are not described herein again.
The stirring and mixing at room temperature are not particularly limited, and the technical scheme of manual stirring or mechanical stirring known to those skilled in the art can be adopted.
After the component A and the component B are obtained, the component A and the component B are mixed according to the mass ratio of 1: (0.8-1.2) uniformly mixing to obtain the organic silicon gel composition.
The preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
The invention also provides a using method of the organic silicon gel composition, which comprises the following steps:
mixing the component A and the component B according to the mass ratio of 1: (0.8-1.2) uniformly mixing, and then drying for 13-16 min at 110-130 ℃ for full curing;
preferably:
mixing the component A and the component B according to the mass ratio of 1: 1, and then baking the mixture at 120 ℃ for 15min to fully cure the mixture.
The application method of the organic silicon gel composition provided by the invention is simple and easy to control, is suitable for being used in various working condition environments, and has a wide application prospect.
The invention provides a silicone gel composition, which comprises the following components in percentage by mass: (0.8-1.2) component A and component B; the component A comprises: 96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups; 0.5-2 parts of toughening and softening agent; 0.01-0.1 part by weight of a metal catalyst; the component B comprises: 78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups; 8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms; 0.01-0.1 parts by weight of a gel curing inhibitor; 0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent; the transparent high-temperature-resistant auxiliary agent is selected from one or more of a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound. Compared with the prior art, the organic silicon gel composition provided by the invention adopts specific content components, realizes better interaction, and obtains a high-transparency high-temperature-resistant organic silicon gel composition; the product has higher high-transparency high-temperature resistance than the conventional silica gel. Experimental results show that the penetration degree of the organic silicon gel composition is 360-380 mm/10 after the organic silicon gel composition is cured at the temperature of 120 ℃ for 15min, and the penetration degree is 260-300 mm/10 after the organic silicon gel composition is baked at the temperature of 250 ℃ for 300 h; the UV-VIS transmittance is 99 percent; the high temperature resistance can reach 250 ℃ multiplied by 500h, the colloid is not brittle and does not crack; the adhesive shear force is 3.3 to 3.5Kgf/cm2(ii) a Therefore, the silicon gel has lower hardness, higher light transmittance, higher high-temperature resistance for a longer time than common silicon gel, and stronger bonding and stretching force。
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application; meanwhile, the use method of the organic silicon gel composition provided by the invention is simple and easy to control, is suitable for being used in various working condition environments, and has a wide application prospect.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available products.
Example 1
(1) The component A comprises: adding 2 parts by mass of single-ended vinyl polysiloxane with the dynamic viscosity of 100mPa.s (25 ℃), 2 parts by mass of vinyl MQ silicone resin and 0.05 part by mass of a complex of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane and platinum (the Pt content is 0.3 wt%) into 96 parts by mass of vinyl-terminated Polydimethylsiloxane (PDMS) with the dynamic viscosity of 1000mPa.s (25 ℃), and uniformly stirring to obtain a component A;
(2) and B component: uniformly mixing 91 parts by mass of vinyl-terminated Polydimethylsiloxane (PDMS) having a kinematic viscosity of 1000mpa.s (25 ℃), 2 parts by mass of polydimethylsiloxane (H% ═ 0.4 wt%, kinematic viscosity of 80mpa.s at 25 ℃), 6 parts by mass of hydrogen-terminated polydimethylsiloxane, 0.03 parts by mass of gel curing inhibitor 1,3,5, 7-tetravinyltetramethylcyclosiloxane and 1 part by mass of cerium acetate at room temperature to obtain component B;
(3) mixing the component A and the component B according to the mass ratio of 1: 1, uniformly mixing to obtain a curable silicone gel composition; finally, the mixture is baked for 15min at 120 ℃ to be fully cured.
Example 2
(1) The component A comprises: adding 2 parts by mass of a single-ended vinyl polysiloxane having a kinematic viscosity of 100mPa.s (25 ℃) and 0.05 part by mass of a complex of 1,3,5, 7-tetravinyl-1, 3,5, 7-tetramethylcyclotetrasiloxane and platinum (Pt content of 0.3 wt%) to 98 parts by mass of a vinyl-terminated Polydimethylsiloxane (PDMS) having a kinematic viscosity of 1000mPa.s (25 ℃), and uniformly stirring to obtain a component A;
(2) and B component: mixing 78 parts by mass of vinyl-terminated Polydimethylsiloxane (PDMS) having a kinematic viscosity of 1000mpa.s (25 ℃), 18 parts by mass of polydimethylsiloxane (H% ═ 0.25 wt%, kinematic viscosity at 25 ℃ of 30mpa.s), 2 parts by mass of polyterminal vinyl polysiloxane having a kinematic viscosity of 100mpa.s (25 ℃), 0.035 parts by mass of ethynylcyclohexanol, and 2 parts by mass of cerium acetate, uniformly at room temperature, to obtain component B;
(3) mixing the component A and the component B according to the mass ratio of 1: 1, uniformly mixing to obtain a curable silicone gel composition; finally, the mixture is baked for 15min at 120 ℃ to be fully cured.
Example 3
(1) The component A comprises: adding 2 parts by mass of single-ended vinyl polysiloxane with the dynamic viscosity of 100mPa.s (25 ℃) and 0.05 part by mass of platinum catalyst platinum-cyclopentene complex (the Pt content is 0.3 wt%) into 98 parts by mass of vinyl silicone oil with the dynamic viscosity of 1000mPa.s (25 ℃), and uniformly stirring to obtain a component A;
(2) and B component: 83 parts by mass of vinyl-terminated Polydimethylsiloxane (PDMS) having a kinematic viscosity of 1000mpa.s (25 ℃), 16 parts by mass of hydrogen-containing polymethylhydrosiloxane having a terminal side chain (H% ═ 0.17 wt%, kinematic viscosity of 5mpa.s at 25 ℃), 0.04 part by mass of alkynyl-containing polysiloxane, and 1 part by mass of cerium zirconate were uniformly mixed at room temperature to obtain component B;
(3) mixing the component A and the component B according to the mass ratio of 1: 1, uniformly mixing to obtain a curable silicone gel composition; finally, the mixture is baked for 15min at 120 ℃ to be fully cured.
Example 4
(1) The component A comprises: adding 0.5 part by mass of vinyltrimethylsilane and 0.05 part by mass of platinum catalyst platinum-cyclohexene complex (Pt content is 0.3 wt%) into 99.5 parts by mass of vinyl silicone oil with dynamic viscosity of 1000mPa.s (25 ℃), and uniformly stirring to obtain a component A;
(2) and B component: mixing 78 parts by mass of vinyl-terminated Polydimethylsiloxane (PDMS) having a kinematic viscosity of 1000mpa.s (25 ℃), 20 parts by mass of hydrogen-containing polymethylhydrosiloxane having a terminal side chain (H% ═ 0.15 wt%, kinematic viscosity of 4mpa.s at 25 ℃), 0.04 part by mass of alkynyl-containing polysiloxane, and 2 parts by mass of neodymium acetate uniformly at room temperature to obtain component B;
(3) mixing the component A and the component B according to the mass ratio of 1: 1, uniformly mixing to obtain a curable silicone gel composition; finally, the mixture is baked for 15min at 120 ℃ to be fully cured.
The silicone gel compositions provided in examples 1-4 were tested for various properties and the results are shown in table 1.
Table 1 performance data for silicone gel compositions provided in examples 1-4
As can be seen from Table 1, the penetration of the silicone gel compositions provided in embodiments 1 to 4 of the present invention after curing at 120 ℃ for 15min is 360 to 380mm/10, and the penetration after baking at 250 ℃ for 300h is 260 to 300 mm/10; the UV-VIS transmittance is 99 percent; the high temperature resistance can reach 250 ℃ multiplied by 500h, the colloid is not brittle and does not crack; the adhesive shear force is 3.3 to 3.5Kgf/cm2. Thus, the present invention provides curable silicone gel compositions having lower hardness; and the silicon gel has higher light transmittance, higher high-temperature resistance for a longer time than common silicon gel, and stronger bonding and stretching force.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A silicone gel composition comprising, by mass, 1: (0.8-1.2) component A and component B;
the component A comprises:
96-99.5 parts by weight of a compound containing at least two aliphatic unsaturated groups;
0.5-2 parts of toughening and softening agent;
0.01-0.1 part by weight of a metal catalyst;
the component B comprises:
78-91 parts by weight of a compound containing at least two aliphatic unsaturated groups;
8-20 parts by weight of organopolysiloxane having silicon-bonded hydrogen atoms;
0.01-0.1 parts by weight of a gel curing inhibitor;
0.5-5 parts by weight of a transparent high-temperature-resistant auxiliary agent;
the transparent high-temperature-resistant auxiliary agent is selected from one or more of a cerium-containing compound, a praseodymium-containing compound and a neodymium-containing compound.
2. The silicone gel composition of claim 1, wherein the compound comprising at least two aliphatic unsaturation is a silicone compound comprising at least two aliphatic unsaturation;
the base unit of the organosilicon compound containing at least two aliphatic unsaturation has the general formula shown in formula (I):
RaR1 bSiO(4-a-b)/2formula (I);
in the formula (I), R is selected from organic groups without aliphatic carbon-carbon multiple bonds; r1Selected from the group consisting of monovalent unsubstituted or substituted, SiC-bonded hydrocarbon radicals having aliphatic carbon-carbon multiple bonds;
a is more than or equal to 0 and less than or equal to 3, b is more than or equal to 0 and less than or equal to 2, and a + b is less than or equal to 3.
3. The silicone gel composition of claim 1, wherein the toughening softener is selected from the group consisting of single-ended vinyl polysiloxane and/or vinyl trimethylsilane.
4. The silicone gel composition of claim 1, wherein the compound comprising at least two aliphatic unsaturation has a kinematic viscosity at 25 ℃ of 102～105mPa.s; the dynamic viscosity of the toughening and softening agent at 25 ℃ is 0.01-300 mPa.s.
5. The silicone gel composition of claim 1, wherein the metal catalyst is selected from one or more of a platinum catalyst, a rhodium catalyst, and a palladium catalyst.
6. The silicone gel composition according to claim 1, wherein the base unit of the organopolysiloxane having silicon-bonded hydrogen atoms has a general formula represented by formula (II):
R2 cHdSiO(4-c-d)/2formula (II);
in the formula (II), R2Selected from organic radicals free of aliphatic carbon-carbon multiple bonds;
c is more than or equal to 0 and less than or equal to 3, d is more than or equal to 0 and less than or equal to 2, and c + d is less than or equal to 3.
7. The silicone gel composition of claim 1, wherein the gel cure inhibitor is selected from one or more of an alkenyl-containing organosiloxane compound, an alkynyl-containing organosiloxane compound, an acetylenic alcohol, cumene hydroperoxide, an organic peroxide, an organic sulfone, an organic amine, an amide, a phosphate, a nitrile, and a diaziridine.
8. The silicone gel composition according to any one of claims 1 to 7, further comprising, in the component A or the component B:
0.1-5 parts by weight of a polysiloxane reinforcing agent;
the polysiloxane reinforcing agent has a general formula of a basic unit shown in formula (III):
R3 pR4 q[SiO]zformula (III);
in the formula (III), R3Selected from methyl or phenyl; r4Selected from vinyl or silicon hydride;
0.6≤p≤0.9，0＜q≤0.1，z＝1。
9. a method of preparing a silicone gel composition as set forth in any one of claims 1 to 7 comprising the steps of:
a) adding a toughening softening agent and a metal catalyst into a compound containing at least two aliphatic unsaturated groups, and uniformly stirring to obtain a component A;
b) uniformly mixing a compound containing at least two aliphatic unsaturated groups, organopolysiloxane with silicon-bonded hydrogen atoms, a gel curing inhibitor and a transparent high-temperature-resistant auxiliary agent at room temperature to obtain a component B;
c) mixing the component A and the component B according to the mass ratio of 1: (0.8-1.2) uniformly mixing to obtain an organic silicon gel composition;
the step a) and the step b) are not limited in order.
10. A method of using the silicone gel composition of any one of claims 1 to 7, comprising the steps of:
mixing the component A and the component B according to the mass ratio of 1: (0.8-1.2), and then drying for 13-16 min at 110-130 ℃ for full curing.
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