CN108410416A - A kind of embedding silica gel and its preparation method and application - Google Patents
A kind of embedding silica gel and its preparation method and application Download PDFInfo
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- CN108410416A CN108410416A CN201810295063.2A CN201810295063A CN108410416A CN 108410416 A CN108410416 A CN 108410416A CN 201810295063 A CN201810295063 A CN 201810295063A CN 108410416 A CN108410416 A CN 108410416A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
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- 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
- C09J11/08—Macromolecular additives
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/296—Organo-silicon compounds
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The present invention provides a kind of embedding silica gel and its preparation method and application.The embedding silica gel of the present invention, is made of component A and B component, wherein the component A, by weight, including following component：20~45 parts of vinyl silicone oil, 2~7 parts of containing hydrogen silicone oil, 40~80 parts of surface modifying stuffing, 0.01~0.1 part of inhibitor；The B component, by weight, including following component：20~45 parts of vinyl silicone oil, 30~70 parts of surface modifying stuffing, 0.05~0.2 part of catalyst.Embedding silica gel made from the preparation method of the present invention, the coefficient of expansion is low, and the good leveling property in solidification, surfacing is beautiful, good embedding effect can be kept under severe cold and heat climatic environment, cracking or the damage for preventing component can be widely applied to the embedding of the electronic component more demanding to temperature stability such as LED power, dry-type transformer.
Description
Technical field
The invention belongs to silicon rubber technical field, be related to a kind of embedding silica gel and preparation method thereof, more particularly to it is a kind of low
Expand the preparation method and application of high-leveling embedding silica gel.
Background technology
Currently, in the fields such as electric, communication and space flight, in order to ensure that product can be under the larger environment of temperature change
Steady operation, or reliably used in the larger different regions of the temperature difference, the low-expansion material of generally use is so that product obtains
Obtain excellent dimensional stability.And protect the silicon rubber of component also to have same requirement embedding, otherwise in heated or drop
Wen Hou, sizing material expansion or contraction, cause volume change to cause the thermal matching between component inconsistent, not only cannot be effective
Prevent the intrusion of moisture, dust and pernicious gas to electronic component, and there is a possibility that generated between device and sizing material internal
Stress, so as to cause the damage or failure of electronic component.The thermal expansion coefficients of existing usual silicone rubber are larger, therefore how
It is the critical issue that silicone rubber applications face to reduce the coefficient of expansion.
In order to effectively reduce the expansion rate of silicon rubber, the lower inorganic filler of the coefficient of expansion can be used as filler, it is inorganic
Filler can be graphite, silica flour, calcium carbonate, titanium dioxide, silicon powder, alumina powder, magnesia etc., wherein graphite and silicon
Powder is notable to the reducing effect of the coefficient of expansion.Meanwhile the dosage of filler is also depended on to the improvement of the expansion rate of silicon rubber,
The coefficient of expansion of sizing material can be reduced by improving proportion of filler.But when amount of filler is larger, the viscosity of colloid is got higher,
Levelability is deteriorated, and surface irregularity when embedding, aesthetics is poor, and therefore, the contradiction between low thermal expansion and high-leveling is to be badly in need of
It solves the problems, such as.
CN103242799A discloses a kind of low viscosity and cures high flexibility two-component condensed type embedding silica gel and its preparation soon
The low viscosity of method, the invention cures high flexibility two-component condensed type embedding silica gel soon, is grouped as two groups by A, B, two groups of A, B
The mass ratio divided is 8-12：1；Wherein component A is made of the raw material of following mass parts：100 parts of hydroxy-terminated polysiloxanes, 20~
100 parts of fillers, 5~50 parts of plasticizer, 0.1~5 part of colorant；B component is made of the raw material of following mass parts：1~5 part of crosslinking
Agent, 1~5 part of coupling agent, 0.01~0.5 part of catalyst, 5~10 parts of plasticizer, 0.5~5 part of chain extender.The invention is prepared double
Component condensed type embedding silica gel has the performance of low viscosity, fast solidification, high flexibility, can meet the high luminous density of LED industry, high
Production efficiency demand, levelability is improved, but the coefficient of thermal expansion of sizing material needs to be further increased.
CN105623593A discloses a kind of two-component embedding silica gel, including two component of A and B, and the component A includes following
The raw material of mass parts：100 parts of vinyl silicone oil, 0~100 part of non-reactive silicone oil, 0.05~10 part of hollow powder, transition metal
0.01~1.5 part of complex compound catalyst, 0~3 part of stock white；The B component includes the raw material of following mass parts：Vinyl silicone oil
100 parts, 0~100 part of non-reactive silicone oil, 0.05~10 part of hollow powder, 0.01~1 part of alkynol class inhibitor, containing hydrogen silicone oil
10~40 parts, 0~3 part of black slurry.Embedding silica gel prepared by the invention is closed cell foamed material, while also having excellent anti-impact
Hitting property, least, flexibility, sound-proofing, water proofing property and vapour proof, volume is not influenced by ambient temperature, coefficient of thermal expansion pole
It is small, but the aesthetics after its rheological property and embedding needs to be further increased.
Invention content
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of embedding silica gel, the coefficient of expansion is low, and
The good leveling property in solidification, surfacing when sizing material embedding, aesthetics is good, and significantly more efficient protection component reaches good
Performance.
For this purpose, the present invention uses following technical scheme：
The present invention provides a kind of embedding silica gel, and the casting glue is add-on type two-component casting glue, by component A and B component
Composition；
Wherein, the component A, by weight, including following component：
The B component, by weight, including following component：
20~45 parts of vinyl silicone oil
30~70 parts of surface modifying stuffing
0.05~0.2 part of catalyst.
Wherein, the component A, by weight, including following component：
20~45 parts of vinyl silicone oil, for example, vinyl silicone oil parts by weight be 20 parts, 21 parts, 22 parts, 23 parts, 24 parts,
25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40
Part, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts.
2~7 parts of containing hydrogen silicone oil, such as the parts by weight of containing hydrogen silicone oil are 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts.
40~80 parts of surface modifying stuffing, for example, surface modifying stuffing parts by weight be 40 parts, 45 parts, 50 parts, 55 parts, 60
Part, 65 parts, 70 parts, 75 parts, 80 parts.
0.01~0.1 part of inhibitor, for example, inhibitor parts by weight be 0.01 part, 0.02 part, 0.03 part, 0.04 part,
0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, 0.1 part.
The B component, by weight, including following component：
20~45 parts of vinyl silicone oil, for example, vinyl silicone oil parts by weight be 20 parts, 21 parts, 22 parts, 23 parts, 24 parts,
25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40
Part, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts.
30~70 parts of surface modifying stuffing, for example, face modified filler parts by weight be 30 parts, 35 parts, 40 parts, 45 parts, 50
Part, 55 parts, 60 parts, 65 parts, 70 parts.
0.05~0.2 part of catalyst, for example, catalyst parts by weight be 0.05 part, 0.06 part, 0.07 part, 0.08 part,
0.09 part, 0.1 part, 0.11 part, 0.12 part, 0.13 part, 0.14 part, 0.15 part, 0.16 part, 0.17 part, 0.18 part, 0.19 part,
0.2 part.
In view of the deficienciess of the prior art, low bulk high-leveling embedding silica gel of the present invention, can overcome existing
The defects such as easy cracked and protrusion in technology, good appearance difference be low with reliability, product viscosity is low, good leveling property, is heated
Expand small, not cracked, good appearance is good, but also the requirement for taking into account machinability, mechanical property etc..
It varies with temperature and causes in one direction it should be noted that low thermal expansion of the present invention refers to colloid
Length variation be expansion rate be less than 15ppm/K, in use will not because temperature increase and obviously expand.
High-leveling refers to sizing material good fluidity when being poured into component after being uniformly mixed, and is rapidly filled with each gap
Place, formed it is smooth and without the plane of apparent concave-convex sense, it is related to the factors such as colloid viscosity, surface tension.
Preferably, the contents of ethylene of the vinyl silicone oil is 0.2~1.0wt%, such as the ethylene of vinyl silicone oil
Base content be 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%,
1wt%, preferably 0.3~0.6wt%.
Preferably, the vinyl silicone oil is vinyl-terminated silicone fluid or ethenyl of side chain silicone oil, preferably end-vinyl silicon
Oil；The activity of end-vinyl is more than ethenyl of side chain, and the promotion of the mechanical strength of crosslinking rate and sizing material is made to become apparent from.
Preferably, the viscosity of the vinyl silicone oil be 100~2000cp, such as vinyl silicone oil viscosity be 100cp,
200cp、300cp、400cp、500cp、600cp、700cp、800cp、900cp、1100cp、1200cp、1300cp、1400cp、
1500cp, 1600cp, 1700cp, 1800cp, 1900cp, 2000cp, preferably 300~1000cp.Contents of ethylene in system
It must be cooperateed with mutually with hydrogeneous content, ensure the mechanical performance after suitable viscosity and solidification, further increase the steady of performance
It is qualitative.
The surface modifying stuffing includes surface treatment auxiliary agent and powder, the matter of the surface treatment auxiliary agent and the powder
Amount is than being (0.1~1):100, such as the mass ratio of the surface treatment auxiliary agent and the powder is 0.1:100、0.2:100、
0.3:100、0.4:100、0.5:100、0.6:100、0.7:100、0.8:100、0.9:100、1:100.If surface treatment helps
The mass ratio of agent and powder is less than 0.1:100, then the effect unobvious of powder are handled, low bulk and high-leveling cannot be reached
Effect；If the mass ratio for being surface-treated auxiliary agent and powder is higher than 1:100, then the increase of component viscosity is apparent, and levelability is deteriorated.
The powder is at least two in graphite, silica flour, silicon powder, titanium dioxide, calcium carbonate, carbon black and alumina powder
The mixture of kind.Such as the mixture of powder is combined as：The mixture of graphite, silicon powder, graphite, titanium dioxide mixture,
The mixture of graphite, calcium carbonate, graphite, carbon black mixture, graphite, alumina powder mixture；The mixing of silica flour, silicon powder
Object, silica flour, titanium dioxide mixture, silica flour, calcium carbonate mixture, silica flour, carbon black mixture, silica flour, alumina powder
Mixture；The mixture of silicon powder, titanium dioxide, silicon powder, calcium carbonate mixture, silicon powder, carbon black mixture, silicon is micro-
The mixture of powder, alumina powder, titanium dioxide, calcium carbonate mixture, titanium dioxide, titanium dioxide mixture, titanium dioxide, aluminium oxide
The mixture of powder, the mixture of calcium carbonate, carbon black, calcium carbonate, alumina powder mixture, the mixing of carbon black and alumina powder
Object, graphite, silicon powder, titanium dioxide mixture, graphite, silicon powder, calcium carbonate mixture, graphite, silicon powder, carbon black it is mixed
Close object, graphite, silicon powder, alumina powder mixture, graphite, calcium carbonate, carbon black, graphite, carbon black and alumina powder it is mixed
Object is closed, equally, the mixture of the powder may be four kinds, five kinds, six kinds, seven kinds of mixture, herein not due to length
It enumerates.
The powder listed all has low-expansion coefficient performance, and wherein graphite and silica flour is aobvious to the reducing effect of the coefficient of expansion
It writes.Simultaneously by being surface-treated the powder of additive modification, surface treatment auxiliary agent is as using silane, silazane, having low polymerization degree
Siloxanes, when be surface-treated auxiliary agent mixed with powder high temperature when, surface treatment active group and polarity of the auxiliary agent by itself
The silicone hydroxyl of key and powder surface acts on, and so that the latter is lost amount of activated, and the hydrophobicity of powder surface increases, and polarity reduces, from
And powder intermiscibility similar to silicone oil component and binding force is made to improve.During preparing A, B component, powder can be effectively improved
The dispersion degree of body and silicone oil reduces viscosity, improves levelability.Such surface modifying stuffing to reduce sizing material the coefficient of expansion,
Improving it has positive effect using craftsmanship simultaneously.
Preferably, at least containing one kind in graphite and silica flour at least two mixture in the powder.Such as
At least two mixture in powder contains only the graphite in graphite and silica flour, at least two mixture in powder containing only
There is the silica flour in graphite and silica flour, at least two mixture in powder contains graphite and silica flour simultaneously.
Preferably, the grain size of the powder is 1~20 μm, preferably 5~15 μm.Packing material size and the ratio in system are mutual
It matches, ensures to avoid settling while suitable viscosity.The mass fraction of graphite and silica flour in the composite can pass through
Its mass ratio is adjusted to regulate and control.
The surface conditioning agent include methacryloxypropyl trimethoxy silane, dimethyldimethoxysil,ne,
One kind in hydroxy-end capped dimethyl silicone polymer and hexamethyldisilazane or at least two mixture.Such as at surface
Manage the mixing for being combined as methacryloxypropyl trimethoxy silane, dimethyldimethoxysil,ne of the mixture of agent
Object, methacryloxypropyl trimethoxy silane, hydroxy-end capped dimethyl silicone polymer mixture, methacryl
The mixture of oxygroup propyl trimethoxy silicane, hexamethyldisilazane, dimethyldimethoxysil,ne, hydroxy-end capped poly- two
The mixture of methylsiloxane, dimethyldimethoxysil,ne, hexamethyldisilazane mixture, hydroxy-end capped poly- diformazan
The mixture of radical siloxane and hexamethyldisilazane, methacryloxypropyl trimethoxy silane, dimethylformamide dimethyl oxygen
The mixture of base silane, hydroxy-end capped dimethyl silicone polymer, methacryloxypropyl trimethoxy silane, dimethyl
The mixture of dimethoxysilane, hexamethyldisilazane, dimethyldimethoxysil,ne, hydroxy-end capped polydimethylsiloxanes
The mixture of alkane and hexamethyldisilazane, methacryloxypropyl trimethoxy silane, dimethyldimethoxysil,ne,
The mixture of hydroxy-end capped dimethyl silicone polymer and hexamethyldisilazane.
Preferably, the hydrogen content of the containing hydrogen silicone oil is 0.3~0.6wt%, such as the hydrogen content of containing hydrogen silicone oil is
0.3wt%, 0.35wt%, 0.4wt%, 0.45wt%, 0.5wt%, 0.55wt%, 0.6wt%, preferably 0.35~
0.45wt%.
Preferably, the inhibitor is ethynylcyclohexanol, methyl butynol and t etram-ethyltetravinylcyclotetrasiloxane
In any one or at least two combination.Such as the mixture of the inhibitor is combined as ethynylcyclohexanol, methyl
The mixture of butynol, ethynylcyclohexanol, t etram-ethyltetravinylcyclotetrasiloxane mixture, methyl butynol and tetramethyl
The mixture of base tetravinyl cyclotetrasiloxane, four silica of ethynylcyclohexanol, methyl butynol and tetramethyl tetravinyl ring
The mixture of alkane.
Preferably, the catalyst is platinum catalyst.
Preferably, the platinum catalyst is the complex and/or the chelate of platinum and the mixture of organosiloxane of platinum,
Such as one kind or extremely in chloroplatinic acid, chloroplatinic acid-isopropanol complex, chloroplatinic acid-divinyl tetramethyl disiloxane complex compound
Few two kinds of mixture.It is preferred that chloroplatinic acid-divinyl tetramethyl disiloxane complex compound, the content of active ingredient are
3000-5000ppm。
The second object of the present invention is to provide a kind of preparation method of embedding silica gel, and the preparation method includes following step
Suddenly：
1) it is (0.1~1) in mass ratio that will be surface-treated auxiliary agent with powder:100 are uniformly mixed, and table is obtained after heating stirring
Face modified filler；
2) by weight, 20~45 parts of vinyl silicone oil, 40~70 parts of surface modifying stuffing, 2~7 parts are contained
Blender heating stirring is added in hydrogen silicone oil, and 0.05~0.1 part of inhibitor is added, continues to stir, obtains component A；
By weight, 20~45 parts of vinyl silicone oil, 30~70 parts of surface modifying stuffing are added in blender
Heating stirring is added 0.01~0.2 part of catalyst and continues to stir, obtains B component.
Preferably, the detailed process of step 1) is, by be surface-treated auxiliary agent with methyl-silicone oil be diluted to 5% it is molten
Then liquid is (0.1~1) in mass ratio with powder:100 are uniformly mixed in kneader high speed, and the blade of the kneader turns
Speed is 30~60rpm, is heated to 60~90 DEG C, stirs 20~40min, then stops stirring and heating, is placed at room temperature for 8~12h,
It vacuumizes again, the vacuum degree≤- 0.095MPa vacuumized, is heated to 60~90 DEG C of 0.5~2h of drying process, obtains surface
Modified filler.
In the present invention, mixing for each material component needs larger shearing force, common stirring to be difficult to realize in step 1),
Therefore it needs to carry out in kneader；And during vacuum kneading, needs to raise the temperature to 60~90 DEG C, processing is made to help
Agent reacts with filler.
Preferably, in step 1), the blade rotating speed of the kneader is 30~60rpm, for example, blade rotating speed be 30rpm,
35rpm, 40rpm, 45rpm, 50rpm, 55rpm, 60rpm, vacuum degree≤- 0.095MPa of the vacuum.It should be noted that
Vacuum degree is indicated by negative pressure (the strong numerical value of system pressure subatmospheric) in the present invention, and the numerical value of negative pressure is smaller, then it represents that true
Reciprocal of duty cycle is higher.
Preferably, the detailed process of step 2) is, by weight, by 20~45 parts of vinyl silicone oil, 40
~70 parts of surface is modified compounded mix, 2~7 parts of containing hydrogen silicone oil is warming up to 60~90 DEG C in planetary mixer, and stirring 1~
After 2h, 0.5~2h is vacuumized, 0.05~0.1 part of inhibitor is added, 5~20min is stirred, obtains component A；
By weight, by 20~45 parts of vinyl silicone oil, 30~70 parts of surface modifying stuffing in planetary mixer
In be warming up to 60~90 DEG C, after stirring 1~2h, vacuumize 0.5~2h, be added 0.01~0.2 part catalyst stirring 5~
20min obtains B component.
Preferably, the mixing described in step 2) is carried out in planetary mixer, the stirring speed of the planetary mixer
Degree be 40~100rpm, such as planetary mixer mixing speed be 40rpm, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm,
100rpm；Vacuum degree≤- 0.095MPa of the vacuum.
The third object of the present invention is to provide a kind of application method of embedding silica gel, by the component A and the B component
It is in mass ratio (0.95~1.05):1 mixing, uses after being placed at room temperature for solidification.Such as component A presses quality with the B component
Than being 0.95:1、0.96:1、0.97:1、0.98:1、0.99:1、1:1、1.01:1、1.02:1、1.03:1、1.04:1、1.05:
1。
The fourth object of the present invention is to provide a kind of application of embedding silica gel, by the embedding silica gel for LED power
Or the embedding of dry-type transformer.
Compared with prior art, beneficial effects of the present invention are：
(1) embedding silica gel of the invention selects surface modifying stuffing as raw material, system is combined with silicone oil system and inhibitor
Standby component A, is combined with silicone oil and catalyst and prepares B component, and A, B component are used cooperatively, and can effectively realize the coefficient of expansion of sizing material
With the balance of levelability, reduce the coefficient of thermal expansion of composite material, and embedding surfacing is beautiful, coefficient of thermal expansion 6~
Between 15ppm/K, good leveling property, can significantly more efficient protection component, reached good performance.
(2) preparation method of embedding silica gel of the invention, the coefficient of expansion of embedding silica gel obtained is low, and is flowed in solidification
Levelling is good, and surfacing is beautiful, can keep good embedding effect under severe cold and heat climatic environment, prevent component
Cracking or damage.
(3) embedding silica gel of the invention can be widely applied to the electronic component such as LED more demanding to temperature stability
The embedding of power supply, dry-type transformer.
Specific implementation mode
The technical solution further illustrated the present invention below by specific implementation mode.
Unless specific instructions, various raw materials of the invention are commercially available buys, or is prepared according to the conventional method of this field
It obtains.
Unless otherwise specified, the viscosity value in the present invention measures at 25 DEG C.
Embodiment 1
1) methacryloxypropyl trimethoxy silane is diluted to 5% solution with methyl-silicone oil, then with powder
Body is uniformly mixed in kneader high speed, 80 DEG C, mixing speed 50rpm of temperature, stirs 30min, then stops stirring and heating,
10 hours are placed at room temperature for, then vacuumize 80 DEG C of drying process 1h, surface is obtained and is modified compounded mix.It is surface-treated auxiliary agent and powder
The mass ratio of body is 0.3:100.Powder is the composition of graphite powder, silica flour and silicon powder, mass ratio 1:1:8, grain
Diameter is 10 μm.
2) surface of the vinyl-terminated silicone fluid of 20 parts by weight, 75 parts by weight is modified compounded mix, the Silicon Containing Hydrogen of 5 parts by weight
Oil is warming up to 80 DEG C in planetary mixer, after stirring 1.5h, vacuumizes 1h, and the inhibitor of 0.05 parts by weight, stirring is added
10min obtains component A；
The surface modifying stuffing of the vinyl-terminated silicone fluid of 25 parts by weight, 75 parts by weight is warming up to 80 in planetary mixer
DEG C, after stirring 1.5h, 1h is vacuumized, the catalyst that 0.01 parts by weight are added stirs 10min, obtains B component.
Wherein, the contents of ethylene of vinyl-terminated silicone fluid is 1.0wt%, viscosity 100cp.The hydrogen content of containing hydrogen silicone oil is
0.3wt%, viscosity 100cp；Inhibitor is ethynylcyclohexanol；Catalyst is chloroplatinic acid-divinyl tetramethyl of 3000ppm
Base disiloxane complex compound catalyst.
Embodiment 2
1) methacryloxypropyl trimethoxy silane is diluted to 5% solution with methyl-silicone oil, then with powder
Body is uniformly mixed in kneader high speed, temperature 60 C, mixing speed 60rpm, stirs 25min, then stops stirring and heating,
11 hours are placed at room temperature for, then vacuumize 60 DEG C of drying process 2h, surface is obtained and is modified compounded mix.It is surface-treated auxiliary agent and powder
The mass ratio of body is 0.5:100.Powder is the composition of graphite powder, silica flour and silicon powder, mass ratio 1:1:8, grain
Diameter is 12 μm.
2) surface of the vinyl-terminated silicone fluid of 30 parts by weight, 65 parts by weight is modified compounded mix, the Silicon Containing Hydrogen of 5 parts by weight
Oil is warming up to 70 DEG C in planetary mixer, after stirring 2h, vacuumizes 1.5h, and the inhibitor of 0.08 parts by weight, stirring is added
10min obtains component A；
The surface modifying stuffing of the vinyl-terminated silicone fluid of 30 parts by weight, 70 parts by weight is warming up to 80 in planetary mixer
DEG C, after stirring 1.5h, 1h is vacuumized, the catalyst that 0.1 parts by weight are added stirs 10min, obtains B component.
Wherein, the contents of ethylene of vinyl-terminated silicone fluid is 1.0wt%, viscosity 100cp.The hydrogen content of containing hydrogen silicone oil is
0.3wt%, viscosity 100cp；Inhibitor is methyl butynol；Catalyst is chloroplatinic acid-divinyl tetramethyl of 3000ppm
Disiloxane complex compound catalyst.
Embodiment 3
1) methacryloxypropyl trimethoxy silane and hydroxyl endblocked polydimethylsiloxane are used into methyl respectively
Silicone oil is diluted to 5% solution, is then uniformly mixed in kneader high speed with powder, 80 DEG C, mixing speed 50rpm of temperature,
30min is stirred, then stops stirring and heating, is placed at room temperature for 10 hours, then vacuumizes 80 DEG C of drying process 1h, obtains surface
Modified compounded mix.It is surface-treated auxiliary agent methacryloxypropyl trimethoxy silane and hydroxy-end capped polydimethylsiloxanes
The mass ratio of alkane and powder is 0.2:0.2:100.Powder is the composition of graphite powder, silica flour and silicon powder, mass ratio
It is 1:1:8, grain size is 10 μm.Hydroxyl endblocked polydimethylsiloxane viscosity 100cp.
2) 30 parts of vinyl-terminated silicone fluid, 63 parts of surface are modified compounded mix, the containing hydrogen silicone oil of 7 amount parts is stirred in planet
It mixes and is warming up to 80 DEG C in machine, after stirring 1.5h, vacuumize 1h, the inhibitor of 0.05 parts by weight is added, stir 10min, obtain A groups
Part；
30 parts of vinyl-terminated silicone fluid, 70 parts of surface modifying stuffing are warming up to 80 DEG C in planetary mixer, stirring
After 1.5h, 1h is vacuumized, the catalyst that 0.01 parts by weight are added stirs 10min, obtains B component.
Wherein, the contents of ethylene of vinyl-terminated silicone fluid is 1.0wt%, viscosity 100cp.The hydrogen content of containing hydrogen silicone oil is
0.3wt%, viscosity 100cp；Inhibitor is the mixture of methyl butynol and t etram-ethyltetravinylcyclotetrasiloxane；Catalysis
Agent is chloroplatinic acid-divinyl tetramethyl disiloxane complex compound catalyst of 3000ppm.
Embodiment 4
1) methacryloxypropyl trimethoxy silane and hydroxyl endblocked polydimethylsiloxane are used into methyl respectively
Silicone oil is diluted to 5% solution, is then uniformly mixed in kneader high speed with powder, 90 DEG C, mixing speed 30rpm of temperature,
40min is stirred, then stops stirring and heating, is placed at room temperature for 8 hours, then vacuumizes 90 DEG C of drying process 0.5h, obtains table
Face is modified compounded mix.It is surface-treated auxiliary agent methacryloxypropyl trimethoxy silane and hydroxy-end capped poly dimethyl silicon
The mass ratio of oxygen alkane and powder is 0.2:0.2:100.Powder is the composition of graphite powder, silica flour, silicon powder and alumina powder,
Its mass ratio is 1:1:4:4, grain size is 10 μm.Hydroxyl endblocked polydimethylsiloxane viscosity 100cp.
2) 30 parts of ethenyl of side chain silicone oil, 63 parts of surface are modified compounded mix, the containing hydrogen silicone oil of 7 amount parts is in planet
It is warming up to 90 DEG C in blender, after stirring 1h, vacuumizes 1h, the inhibitor of 0.05 parts by weight is added, stir 10min, obtain A groups
Part；
30 parts of ethenyl of side chain silicone oil, 70 parts of surface modifying stuffing are warming up to 80 DEG C in planetary mixer, stirred
After mixing 1.5h, 1h is vacuumized, the catalyst that 0.01 parts by weight are added stirs 10min, obtains B component.
Wherein, the contents of ethylene of ethenyl of side chain silicone oil is 0.5wt%, viscosity 200cp.The hydrogen content of containing hydrogen silicone oil
For 0.3wt%, viscosity 100cp；Inhibitor is the mixture of methyl butynol and t etram-ethyltetravinylcyclotetrasiloxane；It urges
Agent is chloroplatinic acid-divinyl tetramethyl disiloxane complex compound catalyst of 3000ppm.
Embodiment 5
1) methacryloxypropyl trimethoxy silane and dimethyldimethoxysil,ne are used into methyl-silicone oil respectively
It is diluted to 5% solution, is then uniformly mixed in kneader high speed with powder, 80 DEG C, mixing speed 50rpm of temperature, stirring
Then 30min stops stirring and heating, is placed at room temperature for 10 hours, then vacuumize 80 DEG C of drying process 1h, obtains surface modification
Compounded mix.It is surface-treated auxiliary agent methacryloxypropyl trimethoxy silane and dimethyldimethoxysil,ne and powder
Mass ratio be 0.2:0.2:100.Powder is the composition of graphite powder, silica flour, silicon powder and alumina powder, mass ratio
It is 1:1:4:4, grain size is 10 μm.Hydroxyl endblocked polydimethylsiloxane viscosity 100cp.
2) 30 parts of vinyl-terminated silicone fluid, 63 parts of surface are modified compounded mix, the containing hydrogen silicone oil of 7 amount parts is stirred in planet
It mixes and is warming up to 80 DEG C in machine, after stirring 1.5h, vacuumize 1h, the inhibitor of 0.05 parts by weight is added, stir 10min, obtain A groups
Part；
30 parts of vinyl-terminated silicone fluid, 70 parts of surface modifying stuffing are warming up to 80 DEG C in planetary mixer, stirring
After 1.5h, 1h is vacuumized, the catalyst that 0.01 parts by weight are added stirs 10min, obtains B component.
Wherein, the contents of ethylene of vinyl-terminated silicone fluid is 1.0wt%, viscosity 100cp.The hydrogen content of containing hydrogen silicone oil is
0.3wt%, viscosity 100cp；Inhibitor is t etram-ethyltetravinylcyclotetrasiloxane；Catalyst is the chloroplatinic acid-of 3000ppm
Divinyl tetramethyl disiloxane complex compound catalyst.
Comparative example 1
Difference lies in inorganic agent dosage is 0, i.e., handles powder without surface treatment auxiliary agent with embodiment 5.
Comparative example 2
Difference lies in graphite levels 0, i.e. powder ratio are silica flour with embodiment 5：Silicon powder：Aluminium oxide is 1:4:
4。
Comparative example 3
Difference lies in silica flour dosage is 0, i.e., powder ratio is graphite with embodiment 5：Silicon powder：Aluminium oxide is 1:4:
4。
Comparative example 4
Difference lies in surface treatment auxiliary agent is methacryloxypropyl trimethoxy silane and six with embodiment 5
Methyl disilazane, i.e., be changed to hexamethyldisilazane by hydroxyl endblocked polydimethylsiloxane, other are constant.
Comparative example 5
Difference lies in the dosage for being surface-treated auxiliary agent increases, that is, is surface-treated auxiliary agent methacryloxypropyl with embodiment 5
The mass ratio of base propyl trimethoxy silicane and dimethyldimethoxysil,ne and powder is 0.6:0.6:100, other are constant.
Comparative example 6
With embodiment 5 ethenyl of side chain silicone oil is selected difference lies in, vinyl silicone oil, contents of ethylene 1.0wt%,
Viscosity is 100cp.
Comparative example 7
Difference lies in surface treatment auxiliary agent is vinyltrimethoxysilane and methyl trimethoxy oxygroup silicon with embodiment 5
The ratio of alkane, the two and powder is 0.2:0.2:100, other are constant.
Comparative example 8
Difference lies in powder is white carbon, and aluminium hydroxide, silica flour, its ratio be 1 with embodiment 5：1:8, remaining is not
Become.
After the sizing material A of above-described embodiment 1-5 and comparative example 1-8, B component are respectively completed, according to mass ratio be 0.95~
1.05:Room temperature curing uses after 1 mixing.
Comparative example 9
Difference lies in A, B component are according to mass ratio 2 with embodiment 5:Room temperature curing uses after 1 mixing.
In the present invention, the test method of casting glue performance is as follows：
The coefficient of expansion：Sizing material is solidified into the print that size is 5 × 25mm of Φ, then uses NETZSCH DIL 402C heat swollen
Swollen instrument measures.Range of measuring temp is RT~150 DEG C, and heating rate is 5 DEG C/min.By the size with temperature for analyzing sample
Change rate obtains its coefficient of expansion.
Viscosity test：It is tested using rotational viscometer, 25 DEG C of test temperature；
Mechanics Performance Testing：According to standard《GBT 528-2009 vulcanized rubbers or thermoplastic elastomer tensile stress-strain
The measurement of energy》, the tensile property of sample is tested.
The performance data for the embedding silica gel that above-described embodiment 1-5 and comparative example 1-9 are provided is as shown in table 1 below.
Table 1
By embodiment 1 to the comparison of embodiment 5, when handling small auxiliary agent usage amount or single use, compound viscosity is high, production
Product poor fluidity.The collocation of powder is more apparent using the viscosity of sizing material can also reduced in example 5, and the coefficient of expansion is decreased obviously.
Therefore selection processing auxiliary agent collocation uses, and the formula comprehensive performance that powder collocation uses is more preferable.
The performance data provided by embodiment 5 and comparative example 1-3 is not it is found that when containing processing auxiliary agent in filler group composition
When, adhesiveness obtained can be caused high, levelability is poor, and the coefficient of expansion is higher；When graphite or small silica flour dosage, the coefficient of expansion
Reduce unobvious.Only just there is low bulk to be flowed with high for the specific processing auxiliary agent of selection, the silica gel prepared under given conditions
The characteristic of levelling.
By the data of embodiment 5 and comparative example 4 it is found that cured strength can be caused to decline using hexamethyldisilazane,
Viscosity increases, and levelability is poor.
By the data of embodiment 5 and comparative example 5 it is found that more using surface treatment auxiliary agent, then colloid viscosity increases, levelling
Property be deteriorated.The dosage of filler surface treatment auxiliary agent treatment effect in a suitable range is more preferable.
By the data of embodiment 5 and comparative example 6 it is found that using ethenyl of side chain silicone oil, relative to vinyl-terminated silicone fluid,
Coefficient of thermal expansion can be improved, it can be seen that when vinyl silicone oil selects vinyl-terminated silicone fluid, the coefficient of thermal expansion and stream of sizing material
The comprehensive performance balance of levelling is more preferable.
By the data of embodiment 5 and comparative example 7 it is found that using vinyltrimethoxysilane and methyltrimethoxysilane
Viscosity as inorganic agent then sizing material rises apparent, and levelability is deteriorated.
By the data of embodiment 5 and comparative example 8 it is found that using white carbon, aluminium hydroxide, silica flour is as filler, then glue
It is apparent to expect that viscosity increases, intensity declines expansion rate and increases.
By embodiment 5 to the data of comparative example 9 it is found that when not mixed according to corresponding proportioning using A, B component, sizing material is consolidated
Changing the time can shorten or extend, and rubber strength declines, and hardness deviates critical field, and expansion rate increases.
The present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment, but the present invention is not
It is confined to above-mentioned detailed process equipment and technological process, that is, does not mean that the present invention has to rely on above-mentioned detailed process equipment and work
Skill flow could be implemented.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to product of the present invention
The equivalence replacement of each raw material and the addition of auxiliary element, the selection of concrete mode etc., all fall within protection scope of the present invention and public affairs
Within the scope of opening.
Claims (10)
1. a kind of embedding silica gel, which is characterized in that the embedding silica gel is made of component A and B component, wherein the component A,
By weight, including following component：
The B component, by weight, including following component：
20~45 parts of vinyl silicone oil
30~70 parts of surface modifying stuffing
0.05~0.2 part of catalyst.
2. embedding silica gel according to claim 1, which is characterized in that vinyl silicone oil in the component A and B component
Contents of ethylene is 0.2~1.0wt%, preferably 0.3~0.6wt%；
Preferably, the vinyl silicone oil is vinyl-terminated silicone fluid or ethenyl of side chain silicone oil, preferably vinyl-terminated silicone fluid；
Preferably, the viscosity of the vinyl silicone oil is 100~2000cp, preferably 300~1000cp.
3. embedding silica gel according to claim 1 or 2, which is characterized in that the surface modifying stuffing includes surface treatment
The mass ratio of auxiliary agent and powder, the surface treatment auxiliary agent and the powder is (0.1~1):100.
4. embedding silica gel according to claim 3, which is characterized in that the powder is graphite, silica flour, silicon powder, titanium white
At least two mixture in powder, calcium carbonate, carbon black and alumina powder；
Preferably, at least containing one kind in graphite and silica flour at least two mixture in the powder；
Preferably, the grain size of the powder is 1~20 μm, preferably 5~15 μm.
5. embedding silica gel according to claim 3 or 4, which is characterized in that the surface treatment auxiliary agent is methacryl
Oxygroup propyl trimethoxy silicane, two silicon of dimethyldimethoxysil,ne, hydroxy-end capped dimethyl silicone polymer and hexamethyl
One kind in azane or at least two mixture.
6. the embedding silica gel according to one of claim 1-5, which is characterized in that the hydrogen content of the containing hydrogen silicone oil is 0.3
~0.6wt%, preferably 0.35~0.45wt%；
Preferably, the inhibitor is in ethynylcyclohexanol, methyl butynol and t etram-ethyltetravinylcyclotetrasiloxane
It is a kind of or at least two mixture；
Preferably, the catalyst is platinum catalyst；
Preferably, the platinum catalyst is the complex and/or the chelate of platinum and the mixture of organosiloxane of platinum；
Preferably, the platinum catalyst is chloroplatinic acid, chloroplatinic acid-isopropanol complex, chloroplatinic acid-divinyl tetramethyl two
One kind in silicone complex or at least two mixture.
7. a kind of preparation method of embedding silica gel as claimed in any one of claims 1 to 6, which is characterized in that the preparation method
Include the following steps：
1) it is (0.1~1) in mass ratio that will be surface-treated auxiliary agent with powder:100 are uniformly mixed, and obtain after heating stirring and change to surface
Property filler；
2) by weight, by 20~45 parts of vinyl silicone oil, 40~70 parts of surface modifying stuffing, 2~7 parts of Silicon Containing Hydrogen
Blender heating stirring is added in oil, and 0.05~0.1 part of inhibitor is added, continues to stir, obtains component A；
By weight, 20~45 parts of vinyl silicone oil, 30~70 parts of surface modifying stuffing are added in blender and are heated
Stirring is added 0.01~0.2 part of catalyst and continues to stir, obtains B component.
8. preparation method according to claim 7, which is characterized in that the detailed process of step 1) is to help surface treatment
Agent is diluted to 5% solution with methyl-silicone oil, is then (0.1~1) in mass ratio with powder:100 is mixed in kneader high speed
It closes uniformly, the blade rotating speed of the kneader is 30~60rpm, is heated to 60~90 DEG C, stirs 20~40min, then stops
Stirring and heating, are placed at room temperature for 8~12h, then vacuumize, the vacuum degree≤- 0.095MPa vacuumized is heated to 60~90
DEG C be dried 0.5~2h, obtain surface modifying stuffing；
Preferably, the detailed process of step 2) is, by weight, by 20~45 parts of vinyl silicone oil, 40~70 parts of table
Face is modified compounded mix, 2~7 parts of containing hydrogen silicone oil is warming up to 60~90 DEG C in planetary mixer, after stirring 1~2h, takes out true
0.05~0.1 part of inhibitor is added in 0.5~2h of sky, stirs 5~20min, obtains component A；
By weight, 20~45 parts of vinyl silicone oil, 30~70 parts of surface modifying stuffing are risen in planetary mixer
Temperature is to 60~90 DEG C, after stirring 1~2h, vacuumizes 0.5~2h, and 0.01~0.2 part of catalyst is added and stirs 5~20min, obtains
To B component；
Preferably, in step 2), the mixing speed of the planetary mixer is 40~100rpm；The vacuum degree vacuumized
≤-0.095MPa。
9. a kind of application method of such as claim 4-6 any one of them embedding silica gel, which is characterized in that by the component A
It is in mass ratio with the B component (0.95~1.05):1 mixing, uses after being placed at room temperature for solidification.
10. a kind of application of such as claim 4-6 any one of them embedding silica gel, which is characterized in that by the embedding silica gel
Embedding for LED power or dry-type transformer.
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| CN109762515A (en) * | 2019-01-28 | 2019-05-17 | 东莞兆舜有机硅科技股份有限公司 | A kind of bonding Embedding Material and preparation method thereof and the application in dry-type transformer |
| CN110964327A (en) * | 2019-12-16 | 2020-04-07 | 杭州之江新材料有限公司 | High-refractive-index transparent silica gel and preparation method and application thereof |
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| CN116063854A (en) * | 2023-03-09 | 2023-05-05 | 深圳天鼎新材料有限公司 | Double-component flame-retardant ceramic silica gel and preparation method and application thereof |
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| CN110964327A (en) * | 2019-12-16 | 2020-04-07 | 杭州之江新材料有限公司 | High-refractive-index transparent silica gel and preparation method and application thereof |
| CN110964327B (en) * | 2019-12-16 | 2021-09-17 | 杭州之江新材料有限公司 | High-refractive-index transparent silica gel and preparation method and application thereof |
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