CN108034257A - A kind of underwater encapsulating material of organosilicon and preparation method thereof - Google Patents
A kind of underwater encapsulating material of organosilicon and preparation method thereof Download PDFInfo
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- CN108034257A CN108034257A CN201711292495.XA CN201711292495A CN108034257A CN 108034257 A CN108034257 A CN 108034257A CN 201711292495 A CN201711292495 A CN 201711292495A CN 108034257 A CN108034257 A CN 108034257A
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- underwater
- encapsulating material
- organosilicon
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- fluorine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Wrappers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses underwater encapsulating material of a kind of organosilicon and preparation method thereof, by polysiloxanes and/or acrylate containing fluorine containing at least two vinyl, with the poly-hydrogen siloxane containing at least two reactive hydrogen under the action of organic platinum catalyst, encapsulating material is obtained by heat cure；Device encapsulation of the underwater encapsulating material of organosilicon of the present invention suitable for underwater, wet environment or containing water phase, is also used as underwater adhesive.
Description
Technical field
The invention belongs to encapsulating material technical field, more particularly to a kind of underwater encapsulating material of organosilicon and its preparation side
Method.
Background technology
With the fast development of microelectronics integrated technology and package technique, the volume of electronic device is less and less.Electronics device
In part process, it is often necessary to encapsulated using suitable mode.Encapsulation is to be connected arrangement using specific encapsulating material
Each element of electronic product connected cures the safeguard measure being environmentally isolated with wherein.Playing prevents moisture, dust and harmful gas
Intrusion of the body to electronic component, slows down vibrations, prevents external force damage and the effect of stable element parameter
Since electronic package material has important influence to the reliability and service life of electronic device, electronic seal in recent years
The research of package material is of increased attention.Electronic package material is to be used to carry electronic component and its mutually interconnect
Line, plays the basis material of mechanical support, sealed environment protection, signal special delivery etc..
Current common electronic package material includes epoxy resin, makrolon, glass, polymethacrylate and has
The high transparency material such as machine silicon.Since makrolon, glass and polymethacrylate encapsulating material hardness are difficult to greatly
Shaping, therefore three kinds of materials are often used as shape lens material, and epoxy resin and organosilicon be due to easily molded processing,
As main encapsulating material.However, under water, under seabed or the particular surroundings such as hot and humid, package material on the market at present
Material can spontaneously form water membrane with device surface.Hydrone in this layer of moisture film and the adhesive material of routine are not phases
Hold, even repel, cause the bonding of device, sealing, encapsulation, repairing etc. in particular circumstances very unfavorable.It would therefore be highly desirable to
The high-touch feature encapsulating material that solution and development can be packaged under water, under seabed or the environment such as hot and humid.
Although there is the so-called underwater encapsulating material of 4 to 5 moneys currently on the market, its using epoxy resin as matrix,
In actual application, it is highly prone to the influence of water or humid air and causes cure package effect poor.
In addition, technical staff has carried out the correlative study on improving underwater packaging effect, but these researchs are most of
From bionical angle, using the component containing hydroxyl, such as the enhancing such as dopamine, catechol is with pasting the mutual of surface
Effect, so as to fulfill underwater encapsulation.But these components are expensive, remain in laboratory stage so far, method there is no to meet real
Border demand.
In encapsulating material, the thermo oxidative stability and electrical insulation capability of organosilicon are very prominent, and hardening time is short, and
With excellent moisture resistance, waterproof, antirust, cold-resistant, resistance to ozone and weather resistance, and after organosilicon is fully cured, adhesion strength
Greatly, good airproof performance, steam and oxygen are difficult to pass through.These excellent properties cause organosilicon to be particularly suited for water compared to other materials
Lower encapsulation, but there has been no correlative study and product.
The content of the invention
In view of the problems of the existing technology, the object of the present invention is to provide a kind of underwater encapsulating material of organosilicon and its system
Preparation Method.
To achieve these goals, the present invention uses following technical scheme：
A kind of underwater encapsulating material of organosilicon, including following raw material：Vinyl polysiloxane and/or fluorinated acrylate
Class, poly-hydrogen siloxane, catalyst, wherein vinyl polysiloxane and/or acrylate containing fluorine：The mass ratio of poly-hydrogen siloxane
For 1-2:1-4.
Preferably, the catalyst is the organometallic complexes such as platinum, rhodium, ruthenium, palladium, gold, rare earth or iron system, it is used
Measure the 50-100ppm for organosilicon encapsulating material.
It is further preferred that the catalyst is platinum (0) -1,3- divinyls -1,1,3,3- tetramethyl disiloxanes, chlorine platinum
Sour complex.
Preferably, the vinyl polysiloxane is the polysiloxanes containing at least two vinyl.
It is further preferred that dimethyl silicone polymer, double ethene of the vinyl polysiloxane for bi-vinyl end-blocking
The methyl phenyl silicone of end-blocking, 3- (methacryloxypropyl) oxypropyl trimethyl silane etc..
Preferably, the vinyl polysiloxane substitutes polysiloxanes for the fluorine containing at least two vinyl.
It is further preferred that the vinyl polysiloxane is poly- difluoromethyl/dimethyl silica of bi-vinyl end-blocking
Alkane, trifluoro propyl methylvinyl-polysiloxane.
Preferably, the acrylate containing fluorine contains the fluorinated acrylate of vinyl or fluorine-containing polyacrylic acid for end
Ester.
It is further preferred that the acrylate containing fluorine is trifluoroethyl methacrylate, methacrylic acid hexafluoro fourth
Ester.
Preferably, the poly-hydrogen siloxane is the poly-hydrogen siloxane containing at least two reactive hydrogen.
It is further preferred that the poly-hydrogen siloxane is poly dimethyl/methyl hydrogen siloxane, polymethyl hydrogen siloxane.
Preferably, the poly-hydrogen siloxane substitutes poly-hydrogen siloxane for the fluorine containing at least two reactive hydrogen.
It is further preferred that the poly-hydrogen siloxane is poly- difluoromethyl/methyl hydrogen siloxane, diisopropyl
(nine fluorine hexyls of 3.3.4.4.5.5.6.6.6-) silane etc..
When containing fluorine in the encapsulating material of the present invention, the hydrophobicity of encapsulating material can be increased.It is therefore preferable that vinyl
At least one of polysiloxanes and poly-hydrogen siloxane contain fluorine；Alternatively, acrylate containing fluorine replacement or part can also be used
Vinyl polysiloxane is replaced, to improve the hydrophobicity of encapsulating material, promotes it to carry out cure package under water.
Preferably, the raw material of the underwater encapsulating material of organosilicon of the invention further includes initiator, its dosage is double bond monomer
One thousandth.
It is further preferred that the initiator is AIBN.
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：
S1：Vinyl polysiloxane and/or acrylate containing fluorine, poly-hydrogen siloxane and catalyst are uniformly mixed, obtained
To performed polymer；
S2：It is heating and curing, obtains the underwater encapsulating material of organosilicon.
Preferably, in S1, the method for mixing includes convention stir mixing and/or ice-bath ultrasonic is disperseed.Wherein, routinely stir
It is with 1000 revs/min of speed to mix mixing, is stirred 15-120 minutes；Ice-bath ultrasonic disperses to be on ice bath, with 40-
60Hz frequency ultrasounds disperse 15-120 minutes.
Preferably, in S2, it is heating and curing to cure 2~90 minutes under 50~150 ° of С.
Term " poly-hydrogen siloxane containing at least two reactive hydrogen " in the present invention, wherein reactive hydrogen refer to poly- hydrogen silica
Hydrogen atom in alkane on si-h bond, silicon hydrogen-based can both be formed a film with crosslinked at low temperature, form surface waterproofing layer, can also be with containing insatiable hunger
Hydrosilylation is carried out with the compound of key, so as to introduce different groups.
Term " fluorine substitution polysiloxanes " and " fluorine substitution poly-hydrogen siloxane " in the present invention are to refer to fluorine-containing poly- silicon respectively
Oxygen alkane and fluorine-containing poly-hydrogen siloxane.
Beneficial effects of the present invention：
The present invention provides underwater encapsulating material of a kind of organosilicon and preparation method thereof, under catalyst action, two kinds of silicon
Crosslinking curing realizes underwater encapsulation to alkane monomer under water.Organosilicon secondary curing material is prepared with following excellent using aforesaid way
Point：
(1) polysiloxanes containing at least two vinyl and the poly-hydrogen siloxane containing at least two reactive hydrogen can pass through silicon
Addition reaction of hydrogen forms cross-linked network, regulates and controls the curing of the controllable material of number of the ratio and reactive group of 2 kinds of monomers
Time and cross-link intensity etc.；
(2) hydrosilylation in the present invention, with polymerizing condition is gentle, the crosslinking curing time is short, is given birth to without small molecule
Into the features such as, gained curing materials water white transparency simultaneously possesses very high refractive index, is very suitable for commercial Application.
(3) high hydrophobicity of polysiloxanes make it that the water vapor transmittance of encapsulating material is extremely low, from the interference of steam, and
The hydrophobicity of material can be further improved by the introducing of fluorine component, so as to optimize underwater encapsulation performance；
(4) present invention, which is preferably prepared in the raw material of organosilicon encapsulating material, contains fluorine atom, can dramatically increase material
Hydrophobicity；
(5) organosilicon encapsulating material of the invention is suitable for underwater, wet environment or the device containing water phase encapsulates,
It can be used as underwater adhesive etc., there is great industrial value and meaning.
Brief description of the drawings
Fig. 1 is before curing, the state diagram of the organosilicon encapsulating material of embodiment 1 in copper sulfate solution；
Fig. 2 is after hardening, the state diagram of the organosilicon encapsulating material of embodiment 1 in copper sulfate solution；
Fig. 3 is the surface contact angle figure of the organosilicon encapsulating material of embodiment 1 after hardening；
Fig. 4 is the DSC curve figure of the organosilicon encapsulating material of embodiment 1 after hardening；
Fig. 5 is the TGA curve maps of the organosilicon encapsulating material of embodiment 1 after hardening.
Embodiment
The present invention is described in more detail below in conjunction with examples below, but the example is not formed to the present invention's
Limitation.
Embodiment 1
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：The poly- diformazan that bi-vinyl is blocked
Radical siloxane (molecular weight 10000) and dimethyl methyl hydrogen (siloxanes and polysiloxanes) (molecular weight 13000) weigh in
In reagent bottle, mass ratio 1:2, and add the platinum catalyst of 80ppm, when ice-water bath ultrasound 1 is small, when stirring 1 is small after, obtain pre-
Aggressiveness, is then heating and curing 30 minutes in 50 ° of С, obtains the underwater encapsulating material of organosilicon.
Fig. 1 is that two kinds of organosilicon silane monomers are close due to silane monomer before curing reaction is crosslinked in embodiment 1
Degree is smaller than copper sulfate solution and immiscible, so there is obvious layering in oil-water interfaces；
Fig. 2 is that two kinds of organosilicon silane monomers are after curing is crosslinked in embodiment 1, and the material after curing is sulphur
Sour copper liquor seals, and does not have drop to flow down in bottle wall；
Fig. 3 is that two kinds of organosilicon silane monomers are crosslinking the contact angle of curing rear surface in embodiment 1.Contact angle is
120 ° of С, show that material surface is hydrophobic structure after curing；
Fig. 4 is the DSC of the organosilicon encapsulating material produced in embodiment 1 after the crosslinking curing of two kinds of organosilicon silane monomers
Curve, exothermic peak of not absorbing heat significantly between 30 ° of С to 230 ° of С of temperature range, shows the crosslinking degree of organosilicon material
Height, curing degree are strong.
Fig. 5 is that the TGA of the organosilicon encapsulating material produced in embodiment 1 after two kinds of organosilicon silane monomer crosslinking curings is bent
Line, encapsulating material weightlessness 5% when temperature be 385 ° of С, show material excellent heat stability, in the temperature range of 30-385 ° of С
It is interior to possess stable performance.
Embodiment 2
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：The poly- difluoro that bi-vinyl is blocked
Methyl/dimethyl siloxane (molecular weight 10000g/mol) and dimethyl methyl hydrogen (siloxanes and polysiloxanes) (molecular weight
13000) to weigh in reagent bottle, mass ratio 1:2, and the platinum catalyst of 80ppm is added, when ice-water bath ultrasound 1 is small, stirring
1 it is small when after, obtain performed polymer, be then heating and curing 30 minutes in 50 ° of С, obtain the underwater encapsulating material of organosilicon.
Embodiment 3
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：By the poly dimethyl of ethenyl blocking
Siloxanes (molecular weight 10000), dimethyl methyl hydrogen (siloxanes and polysiloxanes) (molecular weight 13000) and 3- (methyl
Acryloyl-oxy) weighing of oxypropyl trimethyl silane is in reagent bottle, mass ratio 1:4:1.Add 80ppm platinum catalysts and AIBN
(dosage is the one thousandth containing double bond monomer), when ice-water bath ultrasound 1 is small, when stirring 1 is small, after obtaining performed polymer, then at 50 °
С is heating and curing 30 minutes, obtains the underwater encapsulating material of organosilicon.
Embodiment 4
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：By the poly dimethyl of ethenyl blocking
Siloxanes (molecular weight 10000), dimethyl methyl hydrogen (siloxanes and polysiloxanes) (molecular weight 13000) and diisopropyl
(nine fluorine hexyls of 3.3.4.4.5.5.6.6.6-) silane is weighed in reagent bottle, mass ratio 1:1:1, add 80ppm platinum catalysis
Agent and AIBN (dosage is the one thousandth containing double bond monomer), when ice-water bath ultrasound 1 is small, when stirring 1 is small, after obtaining performed polymer,
Then it is heating and curing 30 minutes in 50 ° of С, obtains the underwater encapsulating material of organosilicon.
Embodiment 5
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：By trifluoroethyl methacrylate and
Dimethyl methyl hydrogen (siloxanes and polysiloxanes) (molecular weight 13000) is weighed in reagent bottle, mass ratio 1：3, and add
Enter the platinum catalyst of 80ppm, when ice-water bath ultrasound 1 is small, when stirring 1 is small after, obtain performed polymer, be then heating and curing in 50 ° of С
30 minutes, obtain the underwater encapsulating material of organosilicon.
Embodiment 6
A kind of preparation method of the underwater encapsulating material of organosilicon, comprises the following steps：The poly- difluoro that bi-vinyl is blocked
(siloxanes is with gathering for methyl/dimethyl siloxane (molecular weight 10000), trifluoroethyl methacrylate and dimethyl methyl hydrogen
Siloxanes) (molecular weight 13000) weighing is in reagent bottle, mass ratio 1:1:1, and add the platinum catalyst of 80ppm, frozen water
Bath ultrasound 1 it is small when, stirring 1 it is small when after, obtain performed polymer, be then heating and curing 30 minutes in 50 ° of С, obtain organosilicon and seal under water
Package material.
The above description is merely a specific embodiment, but protection scope of the present invention is not limited thereto, any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be subject to scope of the claims.
Claims (10)
1. a kind of underwater encapsulating material of organosilicon, it is characterised in that including following raw material：Vinyl polysiloxane and/or fluorine-containing
Esters of acrylic acid, poly-hydrogen siloxane, catalyst, wherein vinyl polysiloxane and/or acrylate containing fluorine：Poly-hydrogen siloxane
Mass ratio be 1-2:1-4.
2. the underwater encapsulating material of organosilicon according to claim 1, it is characterised in that the catalyst for platinum, rhodium, ruthenium,
Palladium, gold, rare earth or Ferrious material organic coordination compounds.
3. the underwater encapsulating material of organosilicon according to claim 1, it is characterised in that the vinyl polysiloxane be containing
There is the polysiloxanes of at least two vinyl.
4. the underwater encapsulating material of organosilicon according to claim 1, it is characterised in that the vinyl polysiloxane be containing
There is the fluorine substitution polysiloxanes of at least two vinyl.
5. the underwater encapsulating material of organosilicon according to claim 1, it is characterised in that the poly-hydrogen siloxane is containing extremely
The poly-hydrogen siloxane of few 2 reactive hydrogens.
6. the underwater encapsulating material of organosilicon according to claim 1, it is characterised in that the poly-hydrogen siloxane is containing extremely
The fluorine substitution poly-hydrogen siloxane of few 2 reactive hydrogens.
7. the underwater encapsulating material of organosilicon according to claim 1, it is characterised in that the acrylate containing fluorine is end
Hold fluorinated acrylate or fluorine-contaninig polyacrylate containing vinyl.
8. a kind of preparation method of the underwater encapsulating material of organosilicon, it is characterised in that comprise the following steps：
S1：Vinyl polysiloxane and/or acrylate containing fluorine, poly-hydrogen siloxane and catalyst are uniformly mixed, obtained pre-
Aggressiveness；
S2：It is heating and curing, obtains the underwater encapsulating material of organosilicon.
9. the preparation method of the underwater encapsulating material of organosilicon according to claim 8, it is characterised in that in S1, mixing
Method include stirring at normal temperature mix and/or ice-bath ultrasonic disperse.
10. the preparation method of the underwater encapsulating material of organosilicon according to claim 8, it is characterised in that in S2, heating
It is cured as curing 2~90 minutes at 50~150 DEG C.
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| CN201711292495.XA CN108034257B (en) | 2017-12-08 | 2017-12-08 | Organic silicon underwater packaging material and preparation method thereof |
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| CN201711292495.XA CN108034257B (en) | 2017-12-08 | 2017-12-08 | Organic silicon underwater packaging material and preparation method thereof |
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| CN108034257A true CN108034257A (en) | 2018-05-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111228572A (en) * | 2020-01-09 | 2020-06-05 | 天新福（北京）医疗器材股份有限公司 | Artificial skin and preparation method and application thereof |
| CN116376420A (en) * | 2023-04-19 | 2023-07-04 | 湖南中能新材料技术有限公司 | Fluorine-containing coating and preparation method and application thereof |
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| US20170101566A1 (en) * | 2014-03-26 | 2017-04-13 | Dong Shi | Transparent organosilicon gel adhesive |
| CN106751346A (en) * | 2016-11-24 | 2017-05-31 | 陕西聚洁瀚化工有限公司 | The synthetic method of fluorochemical monomer modified organosilicon encapsulating material |
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| CN102807757A (en) * | 2012-07-31 | 2012-12-05 | 烟台德邦先进硅材料有限公司 | Organic silica gel used for packaging IGBT (insulated gate bipolar translator) module, and preparation method of organic silica gel |
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| CN116376420A (en) * | 2023-04-19 | 2023-07-04 | 湖南中能新材料技术有限公司 | Fluorine-containing coating and preparation method and application thereof |
| CN116376420B (en) * | 2023-04-19 | 2024-05-24 | 湖南中能新材料技术有限公司 | Fluorine-containing coating and preparation method and application thereof |
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